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User Manual IndentAnalyser Version 3_E

1. Results summary babas No Save Selection 1 RUE RMU E Quarz 1 1 3 004 0 118 5 946910 15620 0 170 or 4 136 7 141 mr 33 52 43 27 0 065 Save All 2 Quarz_B3_5 0mN AVR Quarz 1 i 1 5 000 0 164 9 713380 71 64620 0 170 899 8 0 60 0 319 0 253 79 57 56 11 0 095 3 Quarz_B3_10mN AVR Quarz 1 10 1 10 002 0 249 10 076400 70 83780 0 170 933 4 0 65 0 958 0 717 74 78 77 10 0 147 4 Quarz_B3_30mN AVR Quarz 1 10 1 29 996 0 470 9 180830 68 93700 0 170 850 4 0 67 5 236 3 693 70 53 136 34 0 299 ul o 5 Quarz_B3_50mN AVR Quarz 1 9 1 50 001 0 625 8 996560 68 52740 0 170 833 4 0 75 11 434 7 923 69 30 176 83 0 404 IEE 6 Quarz_B3_100mN AVF Quarz 1 10 1 99 998 0 913 8 801140 67 81440 0 170 815 3 0 68 32 922 22359 67 92 250 35 0 601 E None 7 Quarz_B3_300mN AVF Quarz 1 10 1 300 451 1 636 8 888790 68 40560 0 170 823 4 0 54 174 304 116 517 66 85 435 34 1 098 C Eror 8 Quarz_B3_500mN AVF Quarz 1 4 1 500 717 2 147 8 908580 68 36750 0 170 825 2 0 59 367 858 253 159 65 27 561 09 1 458 C Standard deviat 5 3141 587 76 647 5 7 05 inne fet Oo 3 181 16 0 74047 0 51659 1 6893 o 47 951 0 12094 138 9 30 842 B 4948 189 34 0 50844 P Copy to DB 0 145 05 93 701 5 5463 24276 0 5 5461 20 032 181 23 17956 989934 97 231 97 612 1 3 004 0 118 8 9011 67 814 017 815 3 0 35 0 141 0 118 65 27 43 27 0 065 Hh Clear 1 500 72 2147 10 076 72156 O17 933 4 0 75 387 86 25316 983 52 561 09 1 458 a Fig 30 Results Summary window Save Selection saves the values from a portion of the table selected
2. ioe Stiffness mN um E 400 200 na ae stiffness 0 10 20 30 40 50 60 70 80 90 100 Force mN Fig 107 Stiffness function for a Berkovich indenter with virtually ideal curve Fit function No 5 has proved to be best for describing curves of this type It is necessary to experiment a little with both the fit function and the point number at the start of the fit with low forces in order to find the optimum fit function which results in a horizontal curve line The following graphs show further examples of stiffness curves at maximum forces of 2000mN and 500mN 2 5004 N o Q Oo 2 0004 E E Ss Z E 1 5004 i 14 500 l gy a ab oO 1 000 1 000 g 500 500 Instrument stiffness l Instrument stiffness Fit l Fit 0 500 1 000 1 500 2 000 0 50 100 150 200 250 300 350 400 450 500 Force mN Force mN Fig 108 Examples for stiffness functions with maximum forces of 2000MN left and 500mN right The Average stiffness field shows the average stiffness over all points of the stiffness range following the calculation Presentation this selection field only appears when the stiffness function has been calculated Here it is possible to switch from the stiffness function view default to the compliance function Fit type this selection field only appears when the stiffness function has been calculated Instead of
3. The square root of contact area is IA vr fie u gt 2 E 1 8 1 8 r 2 2 The reduced modulus Er is given by 1 ixi i s E E E The radial displacement correction u is given by u Lan F cos arctar a v gt Measured values F maximum force S unloading depth hmax maximum depth ho depth after unloading m unloading exponent Important note The measurement data except m are obtained from the force displacement curve without stiffness correction uncorrected data This is carried out in the program even if a stiffness function is used in configuration Known values e E Young s modulus of the indenter Index i and the sample Index s e vy Poisson s ratio of the indenter Index i and the sample Index s Calculated values e hc contact depth e sqrt A square root of contact area e Sf instrument stiffness This is varied in the calculation starting with infinite stiffness After calculation of two area functions for the two reference materials instrument stiffness can be calculated by a comparison of the two area functions The area function must not depend on the reference material If there is a difference especially with larger indentation depths or loads this is usually caused by inaccurate stiffness values for the instrument For the calculation infinite stiffness is initially assumed and then reduced gradually until an optimum match of the two area functions is obta
4. ASMEC ONAT Data File DAT Inspectors reference data file AEF Muli data file 044 Average data file AYR Surface scan data file SCN The following types of file can be opened DAT Default data format for ASMEC devices Pure uncorrected test data are stored in this format REF Contains the reference measurements for the lateral force measurements for determining the current spring constants of the retaining springs see chapter 5 8 DAA Multi data Files contain multiple measurement curves of the same application and same force 11 asmec ADVANCED SURFACE MECHANICS after zero point and thermal drift correction When these measurement curves are averaged the result is an AVR file AVR Average Data Files contain an averaged measured curve after all necessary corrections have been performed SCN Surface Scan data files contain data from surface scans All files referred to here contain beside the actual test data also metadata on the settings carried out application used position and valid correction functions which can be shown via the Information button Select the folder and file name by clicking on the icons in the File Selection dialog The folder will remain as default path for reading until you select a different path or close the program fi Save Save Save data in the special IndentAnalyser file format as ASCII or Excel file The IndentAnalyser file format depends on the activ
5. ADVANCED SURFACE MECHANICS 6 3 Calibrating the effective indenter radius There are various applications for which the radius function of a spherical indenter is of importance rather than the area function It describes the effective radius as a function of the effective indentation depth The effective indentation depth he is the deformation of the sample Index s without the deformation of the indenter Index i The deformation portions correspond to the ratios of the Young s moduli The effective radius is the radius Reg of a sohere which produces the same indentation depth h at the same force F as the non ideal indenter E is the reduced Young s modulus h 9 F he s mIa Ret a o OE T16 Eh v f E The effective radius is for example required to calculate the stresses in the surface of a sample in contact with a spherical tip This relates to the evaluation of purely elastic measurements with the Elastic modulus measurements with spheres application Section 5 5 and to the evaluation of scratch tests The window for calibrating the radius function is opened via Calibration gt Effective sphere radius The first step measurement of the reference material and the second step evaluation of raw data are the same as for plastic deformation except that only one AVR file for one maximum force must be generated The third step creating an AREA file is not necessary Effective Sphere Radius olaj Read data E mod
6. If very high lateral resolution is required or only a small sample are is available measurement with the LFU is to be preferred After completion of a measurement or after reading of a data file containing scratch data the Scratch page opens automatically in the Measurement data window Measurement data from Scratch_500mN_Silicium_D_S10 6_0001 DAT mS Surface slope 0 06841 Correct Depth limit 1 0 1 Depth limit 2 0 1 0 50 i z Q o c 075 gt A i Show on bottom axis Show on left axis OQ D Distance Depth v Scratch_500mN_Silicium_D a 1 00 Scratch_500mN_Silicium_D Lateral force i Scratch_500mN_Silicium_D Pre scan depth Scratch_500mN_Silicium_D Post scan depth E 1 25 V Scratch depth 7 Marks j Pre Scan Marks f Subtract V Post Scan Marks Normal force Marks V Lateral force Marks K Marks 1 50 0 50 100 150 200 250 300 V Show legend V Show cursor Risener LUR lt lt more He el Normal F h Curve Lateral F h Curve Normal data over time Lateral data over time Scratch results Approach Image Fig 90 The Scratch page in the Measurement data window before surface slope correction 88 asmec ADVANCED SURFACE MECHANICS The sample slope is calculated in scratch direction and shown at top right under Surface slope provided a pre scan of the surface or a scratch tests with constant force was carried out The sample slop
7. Validity range from jel 05 2008 Range start Range end 1 Correction type One area function Description by fe One fit fu Coefficients From 0 001 pm To 1 499 urm TEZE Fiat fiai 4 533200217 0S5 25262 0 000425556 1 4 01693319 a2 0424754 x 4 5332 a2 0 5533725 Fig 17 Fit coefficients of the area function and window for changing them All data entered in the Indenter tab can be saved in a database for easier access Save in DB button and retrieved with Open DB H Area function database JE lol x Found 1 record s 1 Berkovich 1 B3 Diamond 12 ASMEC UNAT Details found 3 record s Area_No FromDate 1 3 17 01 2007 09 03 2007 8 2 1 1 4 08 03 2007 17 03 2012 g 5 07 05 2007 05 05 2012 8 0 368 Instrument f Indenter no E 3 Angle fi 97 je Indenter type Berkovich Damar E Modul 5 ae E oo es O ae Onn 44 9 or jamoni 40 0 07 14 95 109 05 2007 11 25 20 Material Diamond GPa 114 Poisson Inclination 4 Stored at 11 Description S apphire Fused Silica quick measurement 8 2 5s Details Fit function 1 Fit coefficients C11 C16 j Area no Corr type fi BO Fit function no a rey ele j Validity date From 17 01 2007 cians C18 i To 109 03 2007 From ym C14 14 5779 j Spline File To pm C15 j Export to e
8. 1 832 SH Results for unloading curve O re lt i ey fe 72 sacerr rue weer 5 const 4 744221141 rn x 2938554543 E7 From 0430163 a rom 0 To 0 290063 Linear fit range Load Unload From 50 toca fioo FitLoad n i Hi Polynom 1 order Fit Unload Show V Load V Load fit 6 0 5 0 4 0 3 0 2 0 1 0 0 0 W Unload M Unload fit In Displacement um Equal scale top bottom Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 59 The Special page of the Average results window In the example chosen 2 fit lines for a linear fit over the last 50 of the loading and unloading curves are shown in logarithmic representation This allows calculation of the exponents of the loading curve shown in the Results field as m 1 832 This is in contrast to the ideal exponent for a pyramidal indenter of two 5 1 7 Results over depth page The dependence of various parameters on the indentation depth can be shown on the Results over Depth page For a normal hardness measurement with only one unloading cycle the only choices available are e Martens hardness e estimated indentation hardness e differential Martens hardness For the estimated indentation hardness a depth independent Young s modulus is assumed and the elastic part of the deformation is subtracted This corresponds to the earlier definition of plastic hardnes
9. 1980 574 Friction between indenter and sample Contact stiffness of the sample as average of the both values S1 und S2 The stiffness value S is used for the calculation of the area function Contact stiffness of the sample at maximum force It is calculated as first derivative of the fit of the unloading curve with a polynomial of second or third order fit function 2 or 3 Contact stiffness of the sample at maximum force obtained from another method It is calculated as first derivative of the fit of the unloading curve with a power function F C h h Instrument stiffness frame stiffness in normal direction as inverse value of the compliance Cf Sfl Instrument stiffness frame stiffness in lateral direction Exponent of the unloading curve from the equation F h h yn F Epsilon factor m It describes the ratio between elastic deformation above the contact area hs and below the contact area h hO without consideration pf plastic contributions There exists a connection between Epsilon und the exponent of the unloading curve m that can be used for a more accurate calculation of the Epsilon value Itis eps 1 for m 1 flat punch 125 asmec ADVANCED SURFACE MECHANICS eps 0 75 for m 1 5 sphere eps 0 727 for m 2 cone For real materials eps can vary between 0 8 and 0 7 according to a complicated function The derivation of the eps value was only done for purely elastic deforma
10. 8 3 14 3 Calculation of errors Unless otherwise stated the statistical error is always shown Systematic errors are not considered Statistical errors are calculated from the standard deviation according to a Student distribution t o t n Student factor AX Fa Standard deviation n Number of measurements Error contributions due to inaccuracies in force or displacement calibration instrument stiffness or compliance or area function are not considered These systematic error contributions compensate each 128 asmec ADVANCED SURFACE MECHANICS other to some extent and it is difficult to give an upper limit for a systematic error The relative error for contact stiffness AS S is given by AS Ah max AF nax AS sys Ah U Ta pa 4 MH S h F S h max max max ASsys is calculated for normal hardness measurements no dynamic QCSM or CSM tests from the two different fit methods for the unloading curve Half of the difference for S between the two fit methods is used as a measure for the error of the fit method AS S1 S2 2 AFmax is the statistical error of the force measurement at maximum force Ahmax is the statistical error of the displacement measurement at maximum force Ahy is the average value of the statistical errors for displacement measurement over all values in the fit range of the unloading curve usually between 40 and 98 It is generally very similar to AN Ah the statistic
11. Average rate nms 0 0894 Use average rate Reset Drift rate nms UBERS Hold period number 1 Fit accuracy nm 0 1158 loj Use Marks Displacement change nm All All 0 None t None W Period 1 lw E Iw Fit curves A W Legend Time s Cancel i Fig 48 The Thermal drift correction window Fit start and Fit end as percentages of the hold period can be changed using the fields in the top right hand corner of the window The arrow buttons nay can also be used to increase or reduce the Fit start value in 5 steps The Drift rate field gives the result of the linear fits in nanometers per second It is assumed that any change in thermal drift due to warming or cooling of the instrument is small If several measurements are analysed one after the other a change in the drift rate from one measurement to the next can generally be disregarded Once the program has started it notes the average drift rate of all measurements analysed The accuracy of the drift correction can often be improved by using the average rate from several measurements This is shown in the Average rate field If you wish to use the average rate for the correction click the Use average rate box below the field Use the Reset button to return the average drift rate to zero A benchmark for the quality of the fit is provided by the Fit accuracy nm value which should be minimal It represents the average difference in depth bet
12. C Giypadrati m Aig File up correction factor i Zero point correction nm 4 83 ero point error nm 0 636 Depth range for back extrapolation nm ao Thermal drift correction done y Correction method 4 Instrument stiffness correction done y see stifness function on Instrument page Fit range for thermal drift correction oftmax Start 25 l Thermal drift correction nm s 0 013 End 100 3 Fig 25 The Applied corrections page of the Configuration window 34 3 Wat cwe The Comparison window asmec ADVANCED SURFACE MECHANICS The window is used for comparing curves Clicking on the Compare button initially opens an empty window Data can be imported via Add Graph Comparison Normal Force mN 80 20mN Test 70 30mN Test 40mN Test 60mN Test 90 40 30 20 10 0 0 00 0 10 0 20 Normal Displacement um 0 30 fa Show With marks All C All C None None jw Graph 1 W Graph 2 W Graph 3 iw Graph 4 iw Graph amp PLE LIL Scale to 1 f None C y asis f saws Both ut Curve no I Add Graph Iw Showy tithe Show footer We Legend M Start at 0 0 Iw Inside Fig 26 Comparison window with comparison of 5 measured curves of different maximum force on the same sample The following types of data can be selected e Data files from IndentAnalyser DAT e Average files from IndentAnalyser AVR
13. Indentation Method Oliver amp Pharr Main results 138 HIT 4629 3 MPa EIT 80 335 GPa HV 428 73 Vickers CIT 6 18 RIT 1 29 Hypothesis Poisson s ratio nu 0 17 Additional results Fmax 0 11 mN hmax 30 29 nm S 0 0137 mN nm hc 23 94 nm hr 22 49 nm hp 21 33 nm m 1 14 Epsilon 0 81 Ap 23022 79 nm Welast 0 44 pJ Wplast 0 91 pJ Wtotal 1 36 pJ nIT 32 55 Measured values Q Time s Pd nm Fn mN Q Q 0 2416 5 032 0 0049 0 4832 7 5558 0 0112 0 7247 9 0165 0 0181 asmec ADVANCED SURFACE MECHANICS 9 10 Data from a Zwick hardness measurement head Data from a Zwick universal hardness measurement head must be in ASCII format Data export should therefore be performed in the Zwick testXpert software The program can work with various output formats Since 2014 an export format has been available in which the start of the individual segments Loading and Unloading Creep is marked The format always has the same column structure The file extension is TXT and should be used in preference if available For older testXpert software versions the file extension is TRA Here the column structure and also the titles of the columns may vary in different languages Data in languages other than English or German cannot be read Example of the file structure of the TXT format Sample name Stahlplatte xyz Sample number 1 Customer undefined Comment 1 Comment 2 Indenter type
14. Load On Sample Stiffness Modulus Hardness m sy nam mN N m GPa GPa Q 48 200 1860 143 0 004990 FEE KKH Q 48 400 1855 408 0 004958 FEE KKH Time DisplacementIntoSurface LoadOnSample Stiffness Modulus Examples of data files are supplied with the program The units of columns are given in the last header row Only SI units are permitted nm um um mm LN MN N s Please adjust your XP nanoindenter routine Export sample to fit to these requirements The procedure is described below 132 asmec ADVANCED SURFACE MECHANICS To export ASCII data proceed as follows in the TestWorks software Go to main menu Define The Sample Export routine must be installed on the Configuration page If this is not the case left mouse click and use Insert Configuration Item Insert the expression Sample Export The Test Export module will appear note the difference in the name compared to Sample Export Set the following properties on this page Export Template press Browse Use the MTS Nano Test Export file File Mode use Auto Increment Each exported file receives an increasing number at the end Destination file Export Filename use a characteristic file name for the measurement You should change the file name at each data export for a different sample Next go to the Channels page Press the Export order button Use the arrow keys to arrange the columns as in the
15. Selecting this option means this data will be used for correction Statistics Acceptance range for measurement average times standard deviation if multiple force displacement curves are evaluated the results will include an average maximum indentation depth plus associated standard deviation The program indicates if the difference between the average indentation depth and the indentation depth of an individual curve is greater than the acceptance range In this case it is recommended that a measurement be scrapped and excluded from averaging It is recommended that only values between 2 3 should be used Statistics Acceptance range for measurement average times standard deviation 2 Black white output in results window during printout Black white output in results window during printout with some printers problems occur when individual results in the Average results window are shown in color This option allows the results display to be switched briefly to black and white during printing 3 2 6 Analysis Lateral page Configuration esl Main Hardware Instrument Indenter Analysis normal Analysis lateral Results Other Spring constant for Lateral Force Unit mN ym 18 87 V Automatic reference measurement can only be deactivated during one session not permanent Depth limit 1 for scratch test um 0 1 Depth under load Depth limit 2 for scratch test um 0 1 Remaining plastic deformation Fig 20 Th
16. 13 asmec ADVANCED SURFACE MECHANICS Report Re po rt Show a window with a preview of the results report The report page shows the document exactly as it will be printed Use the buttons at the top of the window to change the presentation save the report or print it More details can be found in Section 3 8 Stress strain Stress strain This button is only available when the Average results window is open and the Neural networks module has been purchased with the program Click on the Stress strain button to open the evaluation window calculation of elastic and plastic material parameters using neural networks Compare Compare Open the Comparison window Allows a large number of curves to be compared in one window See Section 3 5 Ny Graph Graph Open the Graph Commander window This allows most properties of any diagrams to be changed and additional functions to be used The Graph Commander always uses the current graph in the current window If necessary the mouse must be clicked on the correct window to activate the window The active diagram window is shown in the right hand segment of the Graph Commander status bar See Section 3 6 Open Template opens a previously produced graphic template TEE file Click on the icons in the file selection dialog to select the directory and file name A template is a mask for presentation of the diagrams Background side walls in three dimensional views frame legend axes
17. Fourth step calculation of area function and instrument stiffness To determine the indenter area function for pointed indenters the menu item Calibration gt Area function and instrument stiffness from plastic deformations is called up The window Indenter rea function will appear A blue curve for an ideal indenter of the type entered in the configuration will already be visible A Data input Located top right in the Read data section of the window is the Open icon Click on this button to import one of the available AREA files for Specimen 1 fused silica in the example and Specimen 2 sapphire in the example 98 asmec ADVANCED SURFACE MECHANICS Read data E modulus Poisson r gt Sample 1 72 0 17 410 0 234 indenter lo o7 lt lt more Fit function 8 B EB Points from f ja to l10 fal Indenter area function Tip radius upper limit um lo Average stiffness mN um fo Square root A um Data from sample 1 ideal Tip lv Fit V Ideal 0 00 0 25 0 50 0 75 1 00 nE um fl HH Close Fig 102 Window for calculation of the indenter area function from plastic indentations The correct data for Young s modulus E modulus and Poisson s ratio Poisson r for these reference materials and for the indenter diamond in this example should then be entered The values for fused silica Sapphire and diamond are already in the fields and only need to be changed if other materials are b
18. Marks 40 30 20 10 0 10 20 30 40 Lateral reference curve Marks Lateral Displacement um Collect Analyse y bi Fig 94 The Lateral F h Curve page in the Measurement data window after reading of a wear test file Before the lateral data are evaluated zero point correction and thermal drift correction must be carried out using the normal normal direction force displacement data To do so go to the Normal F h Curve page and press the Analyse button or use the Analysis button in the main menu After correction the curves in the Measurement data window will change After drift correction the curve in Fig 94 will appear as shown in Fig 95 92 asmec ADVANCED SURFACE MECHANICS 500 450 D O oO Oo oi oO 350 5 _ gt Z D 300 075 D O oO O O 250 3 7T D 1 00 A E w 5 200 i z 5 1 25 Z 150 100 1 50 50 1 75 0 0 00 0 25 0 50 0 75 1 00 1 25 1 50 1 75 40 30 20 10 0 10 20 30 40 Normal Displacement um Lateral Displacement um Fig 95 Normal left and lateral right force displacement curves after correction of thermal drift The left hand figure shows the normal force displacement curve The large change in depth at maximum force is caused by the surface slope of the sample In the lateral curve red in the right hand figure it can clearly be seen that the surface was not completely horizontal A further evaluation can now be carried o
19. Use OK Cancel Save Fig 13 Instrument stiffness database window All data input in the Instrument tab can be saved in a database for later access Save in DB button and later recovered via Open DB The Instrument Stiffness Database window contains all saved parameters see Fig 13 The Fit Data window is an effective tool for analysis and data fitting It is also used to represent the fit function graphically when the J button is pressed 21 sasmec ADVANCED SURFACE MECHANICS a fil Fit Data AHA Function number Number of terms 3 1931 561014 0 340951 7576 0 0001308300218 Show Data m Wwith marks IV Show Fit With marks J Showresidusl IV With marks Points for fit curve 100 From ai To point Xi point Fit function 2 Read PAR column f v No action Y column 2 No action x factor 1 Y factor fi Z E wn wn D ep 400 600 1 000 k k Force mN Calculation Close Fig 14 The Fit data window with display showing a stiffness function 3 2 4 Indenter page The Indenter page contains the following parameters Configuration esl Main Hardware Instrument Indenter Analysis normal Analysis lateral Results Other Indenter type Berkovich x Indenter no BI Area function no it Indenter material Diamond Young s modulus GPa fhi Poisson s ratio 0 07 eel ae 0 154 Effective opening angle w haz o To Comment
20. axis scaling and designation headings and other graphics elements have properties which can be saved in a template It does not contain the properties of curves or test data You can use a template to specify your own presentation style for instance for publications A template has file extension TEE You can only import a template file if a window with a diagram chart window is open The template only affects the active diagram If several windows are open you should click on the required diagram before opening the file saveT Save Template This can be used to store the properties of the current diagram as a template see 0 A window opens in which you can select the directory and enter the file name The file extension is added automatically Note that the axis scaling will also be specified in the template In this case loading a new template may result in incorrect axis scaling and data may disappear because they lie outside the scaling To avoid this effect put the axis scaling properties in the Chart Editor on the Axis Scales page on Automatic This must be done for every relevant axis 14 asmec ADVANCED SURFACE MECHANICS 3 2 Open a configuration file For every instrument every indenter tip and every new area function a separate CFG file should be stored The CFG files will be saved in the folder CFG Files one level below the program path per default Any number of CFG files can be saved with any possible name foll
21. e Text files with TXT header ASCII data with header if these files are also saved with IndentAnalyser the header contains information on the assignment of axes axis designations and curve titles e Text files without header ASC ASCII data without header e Line diagram files GRA from earlier ASMEC software e Any text files with multiple columns without headers The program automatically identifies the number of data columns in a TXT or ASC file and suggests the number of curves for import The first file defines the title and axis designations in the diagram Show With marks f All C All 0 None f None if Grphi D Ww Graphe Ww Graphs Ww Grphd w Graph Mi Grap Remove Graph 5 Imported curves can be deleted by a right mouse click on the field containing the graph number then confirming with a left mouse click All curves displayed in the Show subwindow can be hidden by selecting None and revealed again by selecting All In the With marks subwindow all curves can be shown with m All or without None markers at the measuring points 35 asmec ADVANCED SURFACE MECHANICS Fig 27 Deleting curves in the Comparison window Scale to enables scaling of the X axis Y axis or both axes to the value 1 as maximum Curves measured with different loads are then the same size and their shapes can be compared better The titles of the axes can be changed by right mouse clicking on th
22. if available with a symbol The points are linked by a continuous line Va margin when the application Elastic modulus measurements with spheres has been selected for the measurement Clicking the button opens the Elastic fit of load displacement curve window This window opens automatically when an AVR file of this application is opened The button Young s modulus calculation using purely elastic deformations is visible on the right 5 1 1 Load displacement page The Average results window opens when an AVR files average data files are imported or the Analyse button in the Measurement data window is pressed and the application selected is suitable for hardness tests On the Load Displacement page the complete loading and unloading curve a fit curve red and the tangent to the unloading curve at maximum force are shown The results for the parameters selected 57 asmec ADVANCED SURFACE MECHANICS during configuration are shown at the right hand side of the window The results can be selected with the mouse and copied to the clipboard from where they can be pasted into other documents E Average results a S QuarzfrB2_B2 0009 DAT 100 ge of a N x F 90 h 0 956 um Smoothing H 8 93 GPa E 12 3 GPa 0 ns 0 170 80 HV 826 9 kp mm2 Cir 0 44 Wtot 32 565 ng Reset 70 We 20 906 nJ NIT 64 20 S 265 56 mN um WV Marks 60 he 0 667 um Fit marks 50 Force mN 40 D H l 30 Sample P
23. is used for the calculation of stiffness Show tangent shows the tangent to the unloading curve at maximum force The gradient represents the contact stiffness S Tangent start at hmax the tangent for calculation of contact stiffness usually begins at the point of maximum load at the end of the creep segment If the material is still creeping significantly at the start of unloading however it may be more accurate if the tangent is applied to the point of maximum depth hmax at a somewhat lower force In this case this field must be checked This has no influence on the result for the stiffness the gradient of the tangent only on the calculation of the contact depth and 58 asmec ADVANCED SURFACE MECHANICS therefore the area An example is shown below 100 98 96 94 92 Force mN Force mN 90 88 86 84 82 1 600 1 650 1 700 1 600 1 650 1 700 Displacement um Displacement um Fig 53 Position of the tangent on the unloading curve left with automatic fit between 98 and 40 right using tangent start at hmax Show error band the error band shows the error of the indentation depth for each data point as 1x standard deviation Show plastic depth shows the force displacement depth curve after deduction of the elastic part of the deformation so that only the plastic deformation remains Sample Poisson s ratio The Poisson s ratio is necessary for the calculation of the indentation modulus of
24. mN upper force limit for instrument stiffness Above this force ces value constant stiffness is assumed The upper limit is determined during Soret ia calibration but can be changed here Range end 2038 1 Coefficients contains the coefficients of the function with which the stiffness is described To define your own function a window can be opened via the Edit a button to enable fit function and parameters to be entered see Fig 12 Neen Each function number is linked to a fit function this can be found in 8 4 The ie 03929867404 individual coefficients which depend on the fit functions can be entered here X 1 8 means x Fig 12 Fit function input window Caution the stiffness function has a substantial influence on the test results Changes to the stiffness function should therefore be made only with great care ioj xi Found 1 record s with Instrument N N Corr a N Start N End N N Stiffness N Fit fu NCI NC2 NC3 gt Yes ASMEC UNAT 2739 2 5 780 29853544205 312 82602963635 20 5167515 e gt Edit With LFU 4 For instrument ASMEC UNAT Normal Lateral Description A Edit Fit coefficients normal Stored at 09 05 2007 11 27 19 Correction type Stiffness mN m 2735 2 Start mN End mN Obtained 15apphire Fused Silica quick measurement 8 2 5 Spline datafile none NC5 fo NC10 Ic Export to EXCEL
25. seseeseseeeesrreserreres 76 5 6 Evaluation of cyclic measurements for determination of yield point ssssseseeseseeesseeee 79 5 7 Evaluation with neural networks optional ssssssseseseesesresessrrrressrrrreesrrreressrrrreesrrrrressn 83 5 8 Lateral reference measurements ccccccccssesssseeecccccsaeeeseccecccssaeuuseeeeceeeessuauseeeecesessauaaeeeeseees 87 5 9 Analysis orl Scratch TES S ncseh tncesneces ccasueceassnc anmiiesdenanteass senesapanneceat wratsedeeencaasmaaneesnente 88 ae 5 10 Es Analysis of friction and wear tests ccccccsssccccessececeesececeeesecessueceeeeneceeeaneeeetes 91 5 11 ES Analysis ol tensile COS CS renren nn E ene necemuacsieae 95 Determination of Area Function and Instrument Stiffness cceeccccccccccsesessseeeeceeeseeuseeeeeeesssnaensees 97 6 1 Calculation from plastic indentations pointed indenterS ssssessseesessreressrerrseserrresrrrrressrreres 97 6 1 1 First step measuring reference MaAtETIAIS cccccccessecccessececeeseceeceecceseesecetsuseceeseneceesenes 97 6 1 2 Second step processing the raw data ssssssssessssersssrrresrrererrrressreresrrressreresrrressreresrrreene 98 asmec ADVANCED SURFACE MECHANICS 6 1 3 Third step creating an AREA file scsescossseccnssscucnssscsecusvsctenssscneusssestoussscueussscneousrense 98 6 1 4 Fourth step calculation of area function and instrument stiffness eseese 98 6 2 Calculatio
26. the header The program has a copy protection based on the number of the hard drive or partition Disk ID No on which it is installed The program can be tested as a time limited full version This requires registration and requesting of an Access code When the trial version is started the Welcome window appears Fig 1 The Disk ID No of the computer is shown at bottom right in this window To obtain the access code for a time limited full version or to request a quotation for licensing the software e mail this number to the supplier or to ASMEC The easiest way to do this is by clicking on the e mail address info asmec de in the Welcome window This will open the e mail program provided it is installed then all you need to do is complete and send the ready to use e mail form If the hard drive is re formatted or the software installed on a new computer a new release code will similarly be required asmec ADVANCED SURFACE MECHANICS Welcome sasmec LOVARGED SUREACE UEEHAMICE Copyright 2004 2014 byASMEC GmbH This is a unregistered version of indentAnalyser Version 3 1 0 It can not be used for the analysis of raw data You are allowed to use the software for test purposes only You need an access code to test the software 30 days as full version To getthe code do the following send your Disk ID no given below together with your contact details to the distributor and ask for atime limited access code You can us
27. umas j Namal Fih Curve Normal data over time Appioach Image Fig 43 Status window with information on measurements and Measurement data window with measured curve After completion of the measurement all data points are listed in the table Unchecking the Show graph box hides the measured curve Check the Marks box to display the measuring points with a symbol Collect copies the measured curve to the Data overview window Multiple measured curves can be collected here before being evaluated together and averaged beforehand if necessary Analyse starts the evaluation of the measurement displayed in the window Whether zero point correction and thermal drift correction are carried out manually or automatically depends on the settings in the Configuration window on the Analysis normal page If correction is performed manually the appropriate window will be displayed and OK must be pressed With automatic evaluation the corresponding evaluation window will be shown With hardness measurements this is the Average results window Click on Print button to print out the graph not the data table on the default printer Click on Add Graph gE button to copy all curves from the graph to the Comparison window If the window does not exist yet it will automatically be opened The Save button opens the Save File Dialog To save the data from the displayed load displacement curve select one of the four file formats ASCII mat
28. 200 6 150 T e Isotropic data 150 E Fit Data E c 100 e Kinematic data 100 x Fit Data Stress Strain Curve Upper Stress Strain 50 50 Lower Stress Strain Rp 0 2 0 0 0 5 10 15 20 25 30 0 5 10 15 20 25 30 True strain Plastic strain Fig 88 Two display variants in the neural network module Left calculation with error limits via Markov chain Right portion with kinematic hardening 5 8 Lateral reference measurements In order to generate lateral displacements a force is required to cause deformation of the leaf springs of the lateral force unit lateral spring stiffness This force acts in addition to the frictional force between sample and indenter and must be known precisely so that it can be subtracted from the total measured force Due to the design and the heavy demands placed on the normal stiffness of the spring system the spring characteristic may be slightly non linear To determine the spring characteristic a reference measurement with no contact between sample and indenter is carried out before the lateral force measurements and saved with the extension REF see Fig 89 Lateral force mN oO 4 2 0 2 4 Lateral Displacement um Fig 89 Lateral reference measurement for a scratch test with stage movement The spring constant is 12 15 mN um 87 asmec ADVANCED SURFACE MECHANICS Since IndentAnalyser Version 3 this data has been stored in the normal data file as well
29. 3 2 6 Ana iowa Beco el Ofc 21 2 ae ene A eee ee ee 29 3 23 FR SUNS 0 asec cc stagnate ues nce aieane E ease aaueenieb anneceeanatcesecaraeoensscteaentasueeuenast 30 3 2 8 AGr DIEE se arsao tise bac psoas E NAR 31 3 4 ES The Information WINKOW ssssscscccccsssssssssecccecsscnsssseeccceccsensnsesessccessaaasseaecsecesseaanseseseeee 32 3 5 S The Comparison WINdOW siecnaiicewsssnwossasivcchowesdodesartnseasnsaaveawieasmanneieasiunassmeeteiaobedeismeaseees 35 3 6 S The Graph Commander c ssscccccsseccecesscccceesececseseccccesececseececsegecesseesecessunecessuneceeseneeeetas 36 3 7 tre TRE SUES AIC aen sane teite ccueasnunsei tenets t induc E EE E 38 3 7 1 Working with the table ccccccccsssccccessececeenecceceescceeeeececseeceeeeesecessenecessuaeceeseeneeesseneees 38 3 7 2 ii Creating a graph from the Results table sessssossesessesssenserrrresrrrnssrerererrrssrereserreseeees 40 3 7 3 Pal Displaying results as a 3D graphic or a contour plOt ssssssssssseesssrrresrrressreresrrrseseeress 41 3 8 3 Creating a rePOMt sccccsccccsscocessercsoroncaccseseroesercnononensarenosssessonevenecensersuoneescuorensaeesesersnssreroues 43 4 asmec ADVANCED SURFACE MECHANICS 3 8 1 F rmatting the report ireren p AOE E aiis 43 3 8 2 REDOC OFE VIEN erae E E E A N 45 importing and Correcting Data souseran a 46 aL PENDO e EE R 46 4 2 Importing and displaying measurement data ccecccccssecccc
30. 500 216 1 155 22 24 Click on the Edit button to change the contents of cells in the table The wording on the button will change to Stop edit After the changes have been made click on the button again to finish editing All results are shown without errors by default Errors can only be shown if averaged curves are being evaluated The column Average of should show a number greater than 1 In this case the statistical errors Error or the standard deviation Sigma SD Standard Deviation for force and depth only for these two parameters can be shown by selecting Error or Sigma SD in the Show error box Select the None field to hide this data Show eror f Mone C Error f Sigma SD The easiest way to change the column width is to place the mouse on the line between two columns at the head of the table and drag the line to the desired position Calculation of average and standard deviation clicking on this button causes a second table to be created below the Results table The new table contains the following values e Mean mean value for each column e Sigma standard deviation for each column e V variations coefficient standard deviation divided by the mean value as a percentage e Min minimum value for each column e Max maximum value for each column Nothing is shown for columns without numbers 39 asmec ADVANCED SURFACE MECHANICS The layout and size of the columns are the same as in the ta
31. Creep Absolute creep depth c CIT Relative creep RIT Relaxation x Add results to table 5 V Show parameter graph 0 00 0 10 0 20 0 30 0 40 Contact depth um Load Displacement Creep T Drift Time dependence Approach Special Results over Depth 0 50 0 60 V Show error bars Fig 73 Young s modulus results for the cyclic measurements in Fig 148 via depth E Average results fo Marks Fit marks IV Marks Fit marks dd Fi Multiple creep curves are visible on the Creep page of the Average Results window if more than one creep segment hold period at maximum force is used during the measurement This enables comparison of creep behavior against maximum force In the example 10 creep segments of 10 seconds each were used Overall fused silica shows very low creep Compared to QCSM measurements cyclic measurements have the disadvantage that fewer measuring points over depth are available and the measurement time is greater This in turn results in thermal drift having a greater influence lt 0 5mN with QCSM measurements In addition more accurate results can be achieved for very low forces 72 asmec ADVANCED SURFACE MECHANICS Creep curves Wis 4 A Sys RIN Oe A N e fi y X oo Y p 7 0 g 6 0 O1 O Depth Change nm oo 2 0 0 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 10 0 Time s Fig 74 Comparison of creep curves for 10
32. So 26 24 h 9 249 um 22 Crit force 13 608 mN Unload ratio 35 749 Reset 20 Cycles 40 Peset M Marks 13 Fit marks 16 14 Ee nia ample Poisson s ratio 0 2 5 12 A 4 Drift rate nm s B 5 10 Unloading curve shift nm fo Find o imum 8 pt 6 t i 9 Calculation 0 R Show fit 1 0 000 0 020 0 040 0 060 0 080 0 100 0 120 0 140 Se clean Displacement um F Show error band Load Displacement T Drift Time dependence Special Fig 84 Evaluation window for cyclic measurements after Calculation has been pressed Load mN 0 035 0 040 0 045 0 050 0 055 0 060 Displacement um Fig 85 Defined point for the elastic plastic transition at a critical force of 13 6mN at cycle maximum and a force after unloading of 4 8mN 82 asmec ADVANCED SURFACE MECHANICS 5 7 Evaluation with neural networks optional The Stress strain module Stress strain gt 4IN button can be used to determine material parameters of metallic materials from indentation experiments if a prescribed loading sequence with a spherical indenter is used in the experiments The measurement sequence requires during loading at equal force intervals three creep phases each of 100 seconds and a creep phase of 600 seconds at the end Additionally the indentation depth must be approximately 10 2 of the indenter radius The basis of the identification process is the adoption of a material model of viscoplasticity which
33. a function a horizontal straight line can also be drawn through the stiffness points by selecting Constant value see Fig 109 This is recommended when there is a larger scatter of the points or when the curve is not ending horizontally The Points from value should be increased to consider mostly the 106 asmec ADVANCED SURFACE MECHANICS stiffness results for larger forces Instrument stiffness function o ne Read data E modulus Poisson r sampie1 72 0 17 Sample 2 410 0 234 indenter 1140 0 07 Instrument stiffness lt lt more 6 000 Fit function 5 1 KJ Points from e ij B24 z 7 000 sin A ee C Fundion Constant value Presentation 4 000 Stifness C Compliance 3 000 Tip radius upperlimit um 0 386 Average stiffness mN um 2258 4 Stiffness mN Lum 2 000 1 000 IV Stiffness V Fit Area calculation Stiffness calcul 10 20 30 40 50 60 70 80 90 100 Save in CFG file Force mN Dy Fak Fig 109 Example of describing instrument stiffness with a constant value To save the result of the stiffness calculation in a CFG file click on Save CFG file D Repeated calculation of area function after calculation of instrument stiffness With the stiffness function now saved correctly the area function must be calculated again by clicking on Area calculation The new area function result is saved in the same CFG file The question about overwriting can be answered wi
34. become very long in this case Close closes the window This can only be done when a calculation is not running 78 asmec ADVANCED SURFACE MECHANICS Elastic fit of load displacerent curve fs fos Young s Modulus GPa Poisson s R ieee Fit parameter i sh Nominal tip radius um rf A No layer Substrate 74 434 0 17 Thickness um 6167 Youngs modulus D 4 layer eo E Eo C Sphere radius C 9 layers W Use radius function Fit of Ca avers C Loading curve a D C Unloading cure f Average of both Elastic fit of load displacement curve Points for calculation Measurement Firstl1 BS Last 63 4 ie Period 2 al Results Modulus 72 049 GPa Mean D 0 8705 nm Force mN Show With marks M Measurement D iw Fit f W Show title 000 010 020 0 30 Displacement um Fig 80 Fit result for fused silica without layers including the radius function 5 6 Evaluation of cyclic measurements for determination of yield point The critical load for the elastic plastic transition yield strength of a material can be determined using cyclic loading unloading measurements with a spherical indenter The von Mises stress as a measure of the yield strength can be obtained from the following calculation with ASMEC s external program ELASTICA This program is not part of the IndentAnalyser software The measurement is performed with the pre defined application Yield strength by
35. consequently the REF files are no longer required for the evaluation Nevertheless it is worth keeping them to enable easy comparison of these reference measurements at a later stage The measurement parameters and the displacement range for the reference measurement are selected automatically The data file name selected for the first normal measurement is used as the file name for the REF file The REF files can be read via the Open button in exactly the same way as normal data files A lateral reference measurement includes at least one to and fro movement usually two The maximum deflection is determined by the deflection programmed for the subsequent measurements The deflection during a reference measurement is always slightly greater than the biggest deflection of the programmed applications In scratch tests with stage movement deflection is only around 5um as only the stage moves and the position of the LFU is maintained close to zero 5 9 Analysis of scratch tests Scratch tests can also be performed without a lateral force unit However no lateral forces and therefore no friction values can then be measured Programming scratch tests was described in Section Fehler Verweisquelle konnte nicht gefunden werden The preferred scratch test method is measurement with stage movement as this enables longer scratch tests to be carried out distributing damage over a greater area of the sample and allowing it to be better identified
36. cyclic measurements with spheres After a measurement or after reading a DAT file containing such a measurement the measured curve is shown in the Measurement data window After pressing the Analyse button in this window or the Analysis button in the main menu a zero point correction and a thermal drift correction is done The chronological progress of the measurement can be seen on the Normal signals over time page Fig 82 After all corrections or after reading an AVR file containing such a measurement the Average results window automatically opens in a different view from that for normal hardness measurements For improved accuracy in such measurements it is a good idea first to average a number of equal measurements and to evaluate the averaged curve only 79 asmec ADVANCED SURFACE MECHANICS E Measurement data from DP21_S10 2_0005 DAT ee 70 Points 152 N F mN h pm t s i 0 049 0 9001 0 67 a 2 0 129 0 903 1534 3 0 197 0 905 2 02 4 0 289 0 906 2 67 5 0 361 0 008 334 6 0 440 0 909 4 02 7 0 521 0 010 4 67 a 8 0 602 0 911 3 384 9 0 681 0 011 6 02 10 0 762 0 012 6 67 yi 11 0 842 0 013 7 34 O 12 0 920 0 013 8 02 LL 13 1 685 0 920 9 52 T 14 0 749 0 913 11 902 15 1 828 0 921 12 52 O 16 0 642 0 912 14 02 a 17 1 997 0 022 15 52 18 0 705 0 013 17 92 19 2 192 0 924 18 52 29 0 775 0 9014 20 02 21 2 410 90 025 21 52 22 0 850 0 015 23 02 23 2 648 0 9027 24 52 0 000 0 050 0 100 0 150 0 2
37. data over time Approach Image Fig 46 The Image page in the Measurement data window 50 asmec ADVANCED SURFACE MECHANICS Image page It is possible to attach up to 4 images created with the IndentAnalyser software to the data file This simplifies assignment of images and test data The images must be available in BMP format and a text file containing the image parameters must exist in the same directory that was automatically saved by IndentAnalyser see Fehler Verweisquelle konnte nicht gefunden werden Video Control The image sizes which are possible are shown at bottom right They correspond to the size of the cameras which have been used so far with UNAT instruments The number of images available is shown under Available images and the current image can be selected via the Show image selection field Release image allows the images to be removed from the file Some image information is shown in the Information field When a measurement has been performed with the lateral force unit additional Lateral F h Curve and Lateral signals over time pages are present They have the same functions as the pages for the normal force unit When a scratch test has been performed the Scratch results page appears additionally Its function is explained in connection with the evaluation of scratch tests in section 5 9 4 3 Zero point correction The force and displacement data are recorded during surface detection if the
38. deformation purely elastic deformation at the corresponding pressure distribution e Elastic deformation above Ac the portion of purely elastic deformation above the contact surface This corresponds to value hs in the results list e Plastic deformation the purely plastic portion of the deformation product of hardness and area function e Elastic plastic deformation total deformation With spherical indenters this can also be purely elastic if the yield point is not exceeded Theoretical curve F mok Exa Pressure distribution Load Points Theoretical curve C Sphere paren C Cone 200 ial 100 C Flat punch Constant lt lt Results Power function 90 Load mN 100 Hardness GPa 9 5 an Young s modulus GPa 72 Poisson s ratio 0 1 7 70 Creep length nm 2 Creep time s f 0 we O0 Unloading exponent 1 25 Radius ym 6 5579 Contact area ur 10 626 5 50 rea ur Inst stiffness mN um 1E0008 ka Thermal drift nm s lo 40 Loading rate mNs ft 30 C Elastic deformation 20 Elastic deformation above Ac C Plastic deformation Elastic plastic deformation 10 V Use current area function V Radial displacement correction 0 Calculation Save as DAT 0 00 0 10 0 20 0 30 0 40 0 50 0 60 0 70 0 80 0 90 V Show point marks Displacement um He fe Close Fig 123 Window for modelling force displacement curves 118 asmec ADVANCED SURFACE MECHANICS Not every combination makes sen
39. difference between fit and test data reaches a minimum method of least squares The calculated zero shift in nm is shown in the Zero shift field The purple curve shows the fit result for the depth range used for the fit The default range is defined during configuration in the Default depth range for back extrapolation field of the Analysis normal page This normally lies between 20nm and 50nm The green curve shows the extrapolation of the fitted curve to zero force Usually a purely visual examination of the plotted green curve for zero point correction is sufficient to judge whether the fit selected is adequate or not A numerical value for the quality of the fits is given in the Fit accuracy uN field The value expresses the mean force difference between the fit curve and the data points and should be a minimum value 51 asmec ADVANCED SURFACE MECHANICS I Zero point correction for Quarzglas_B5_0042 DAT Secs First point for fit 46 0 35 Last point for fit 60 Move nm 0 0 3 Zero shift nm 10 47 Fit method 0 25 f Hertz C Quadratic Linear 02 Fit accuracy uM 2 34 oO m Upper end Lower end 0 15 0 1 Upper end Lower end 0 05 Show With marks W Load data j Iv Fit E Se 0 0 01 0 02 0 03 0 04 Depth um Skip ax Fig 47 The Zero point correction window Manual corrections can now be made by clicking on the blue and green arrow buttons The horizontal arrow buttons aw or the arrow keys o
40. enabled enables analysis of scratch tests with oscillating lateral force 18 asmec ADVANCED SURFACE MECHANICS unit Requires the scratch test module data from a lateral force unit only UNAT Materials Database enabled activates the materials database A separate purchase of the database is required 3 2 3 Instrument page Instrument IndentAnalyser can not only evaluate data from ASMEC instruments but it can also be used with other nanoindenters or hardness testers provided the data is in ASCII format The instrument from which data are to be evaluated can be selected from the drop down menu Instrument No Defines an instrument number to enable clear assignment of the instrument in use This is especially important if more than one instrument is in operation or if data are to be exchanged between different users If test data from a different instrument are to be evaluated the file extensions used by the instrument per default must be entered in the Data file extension field When a UNAT is in use the DAT extension is entered here and cannot be altered If necessary a Second extension can be entered in the belonging field Configuration cox Main Hardware Instrument Indenter Analysis normal Analysis lateral Results Other Instrument ASMEC UHAT Instrument no jos 2001 The instrument and software version i connected with the raw data format Only data files belonging to the chosen in
41. example above You can also use the MSM file of the TestWorks method in the Examples Nanoindenter XP directory of the InspectorX IndentAnalyser installation path 9 3 UMIS 2000 data DOS software version The original DAT file can be imported in binary form If a file containing creep data CRP and a second hold period at the end of the measurement in QMW format exist with the same file number they will be imported together with the DAT file Additional information will be obtained from the NAM file which must be located in the same path Examples of data files are supplied with the software Note If your software uses different file extensions please contact your software supplier CRP and QMW files exist in ASCII format with the following structure 19 34 55 01 18 2002 Depth Force 0 02 616 79 50 00296 0 07 617 10 50 00254 The measurement date is obtained from the date of the NAM file not from the first row of the ASCII file Cyclic measurements developed for spherical indenters possess file extension ALT WinUMIS software version The original data files with a file extension consisting of three digits can be imported A PAR file with the same name and containing additional measurement information is also imported It must be located in the same path Normally only files with the same initial digit in the file extension e g O for the first 100 files 000 099 are shown in the file selection dialog in order
42. file can be copied to another computer and used there for analysis of test data Configuration files with the extension CFU from older versions of the separate program IndentAnalyser can also be imported Configuration lS Main Hardware Instrument Indenter Analsis normal Analysis lateral Results Other Selected configuration file B1_201 3 11 29 2000mN CFG Instrument Program owner ASMEC Software access code A303 832 553 363 214 655 12 Get Disk ID No lo unlimited Run with log file Standard path for configuration tiles CFG HAE Laufwerk DelphiinspectoX CFG Files UNAT Kunden Continental Standard path for parameter tiles PAA H E Laufwerk Delphiiinspectors Version SPARFiles 000 Standard path far position files POS H E Laufwerk DelphitInspector Version 3 POSFiles 8 Standard data path DAT H Messdaten UNAT Dater Gerate Besitzer Continentah2013 11 28 00000 5 Cancel Save CF Fig 8 Main page of the Configuration window Instrument Program owner The name of the owner or user of the measuring instrument or software program can be entered here This is purely for information IndentAnalyser software is copy protected Without an access code the program will start as a trial version Only the importing of raw data is prevented most of the other functions can be used without restriction The software access code which is received from the supplier after purchase of the software is e
43. hung Nr Kraft Tiefe korr H rte Zeit 1 0 386 0 010 7215 0 5 2 0 508 0 015 6072 1 0 WINDOWS software version Only ASCII data can be imported Use the instrument software export program It is recommended that all files in a series with the same load are saved in an ASCII file using the file extension TXT A different file extension can be set on the Instrument page in the configuration To use data in the load range below 0 4mN the Output Protocol must be changed A number of data files are supplied in the Example directory If you have problems importing data check the structure of the data file with an ASCII editor and try to reproduce the same file structure with your report Two examples follow Example 1 This example contains data below 0 4mN for zero point determination They do not exist in the default output format At least two empty lines must be left between this data and data above 0 4mN An empty line must be left between data from a complete measurement and the next measurement Quarz 500 mN hap 20 11 02 09 30 03 HM k 499971 30 0 300 3753 80 x 35 610 y 39 864 Kraft mN Tiefe um Zeit sec Comment this are data below 4mN 0419999 Q 0043421 0 1 for zero point detection 060948 Q 00681055 0 2 They are not in the standard 0800863 O 00906338 0 3 format 0 0990505 Q 0108627 0 4 0 118009 Q 0129148 0 5 0 136975 0146397 0 6 0 155938 0164985 Q 7 0 175091 0181639 0 8 0 194059 019799
44. is able to describe the key phenomena of metallic materials under mechanical loading With monotonic loading and small strains the conditional equations represent a Chaboche model The following formulae apply E E FE Variable Symbol Unit E Total strain E OTE E Elastic strain E e B Inelastic strain E i n Inelastic strain rate i S 1 j j F o k n in Accumulated inel strain S Stress o MPa Overstress F MPa k k i e 0 B s Isotropic hardening k MPa Young s modulus E GPa S t dt Viscosity exponent m Viscosity parameter n MPams Initial overstress F MPa y 3c 0 AL limo k R Ob Yield stress k MPa S oo p Initial slope of hardening y MPa do 3 Hardening parameter B o lim y Cc s gt 0 ds 2 For the purely plastic stress strain relation the following formula is valid The first term is the yield stress the second the isotropic hardening and the third the kinematic hardening ZeroNet Geschwindigkeitsabh Anteil E Modul ENet Viskositatsparameter ViscNet K Geschwindigkeitsunabh Anteil a oe Kraft Kraft Eindringtiefe Daten Eindringtiefe Dehnung On basis of this material model a large number of finite element simulations for the calculation of the deformation behavior during an indentation experiment load displacement curves have been done 83 asmec ADVANCED SURFACE MECHANICS With these data a neural network has be
45. left or right hand axis e g for scratch test curves 3 6 MY The Graph Commander Graph Commander Rw mae Fs hicA a Normal Active Measurement data Fig 28 The Graph Commander window for editing graphs The Graph Commander buttons have the following functions E4 Chart Editor opens the highly powerful Chart Editor with which all graphic parameters can be changed It possesses its own Help function however this does not work on all platforms Click on the question mark then click on the item for which information is required 36 asmec ADVANCED SURFACE MECHANICS le Chart Editor m r 2 Seres General Axis Titles Legend Panel Paging walls 3D i Visible scales Title Labels Ticks Grid Position ie Behind W Automatic W Visible M Inverted Change Desired Increment 2 Bottorn Asis Logarithmic Log Base Ho lke Depth Right A Depth Top Minimum Maximum W Auto 0 Change Offset B Fig 29 Chart Editor window df Standard presentation this button undoes all changes to the diagram and restores it to the state which existed when the window was first opened Measure screen position with this button the cursor becomes a crosshair as soon as it is positioned in the area of the diagram The crosshair is extended up to the relevant co ordinate axes The exact position is shown in the left and middle segments of the Graph Commander status bar see Fig 28 The X
46. may be different from the order of Vickers or indentation hardness which consider only plastic deformation The Martens hardness can also be calculated for purely elastic deformation Martens hardness determined from the slope of the increasing force displacement curve For homogeneous materials dimension of the inhomogenities in the region of surface is small in relation to the indentation depth the following equation is at least partly valid preferring pairs between 50 F and 90 Fmax for the force displacement curve h mM VF The slope m can be determined by a linear regression In this case it is possible to determine the hardness by the following modified method from the force indentation For Vickers and modified Berkovich indenters it is h m A 0 depth curve HM As h 26 43 with A as contact area of the indenter surface Equivalent Vickers hardness Hi may be correlated to HV for a wide range of materials by using a suitable correction function H are related to the Vickers Hardness number HV by a scaling factor For a Vickers indenter it is HV H r 0 927184 given by the ratio of the projected contact area to the real contact area The unit for the Vickers hardness is ko mm although the unit is normally not gibe together with a Vickers hardness number Converting the different units of GPa and kp mm by using the fall acceleration one gets HV 0 094546 H r For a modified Berkovich indenter the fact
47. method the area function is described Correction type One area function AE 4 9038 Ideal 4 95 One area function description of the area function with a fit function over the entire depth range This field is only used to clarify the Description by selection option below Indenter slope above fit range in diagram VA f hc i e root of area function function of indentation depth the curve above the fit range has a constant gradient to be entered here For Berkovich or Vickers indenters the ideal value is 4 95 Deviations from this value give an indication to either an inaccuracy in area function determination or to actual deviations If it is not clear whether the deviation is real the ideal value should be used Description by This bar specifies which method was used to describe the area function The options shown here are specified in the Calibration gt Area function and instrument stiffness menu during calibration and automatically transferred from here Description by f One fit function f Teo fit functions f Data table f Radius function One fit function the area function is described by a function with up to 10 coefficients for the entire indentation depth area Two fit functions use of two fit functions for increased accuracy one function in the lowest indentation depth range the other in the succeeding indentation depth range up to the end of the determination range of the area function Data table the a
48. normal test force Click on the arrow keys Ar up or SH down down to move the selected row in the table up or down In this way the order of results in the Results window and the results table can be defined If a uniform display of digits color or bold presentation is required click on the All equal buttons below the relevant fields 3 2 8 Other page Special parameters for instrument Hyson SSS Additional configuration settings are carried out on the Other page If the software is started Contact force surface detection WN 05 without hardware only the top part of the window will be visible This part relates to Force tolerance for hold period uN 5 settings for data import from other devices 31 asmec ADVANCED SURFACE MECHANICS Tolerances for contact force and force during hold periods are set here These values are required for automatic recognition of the individual segments of a measurement If there is an error when importing test data from other instruments this often due to incorrect setting of these values The values should be at least twice as great as the peak to peak force signal noise Data import use these fields to define when data compression is used Data can be compressed for evaluation in the Results window in order to reduce the number of data points Too high a number of data points slows down the data processing Configuration Main Modules Instrument Indenter Analysis nor
49. requirements of the current standard ISO 14577 considers the radial elastic deformation ur parallel to the surface within the contact area and increases the accuracy of the area function This is why the Radial displacement correction field is selected as default For most materials this correction is below 2 however for fused silica frequently used as a reference material it is more than 4 5 Calibration using fused silica would consequently affect the results of all other materials with a certain amount of radial displacement see also chapter 3 2 5 Variable epsilon factor This correction also goes beyond current standard ISO 14577 and considers a variable epsilon factor which unlike the fixed value of 0 75 in the standard can fluctuate between 0 7 and 0 8 depending on the exponent of the unloading curve It increases the area function accuracy and is therefore used as default see chapter 3 2 5 Beta factor Beta factor h Checking Beta factor allows a value to be entered for the beta factor B which deviates from default value 1 Default value 1 should only be changed if really necessary see chapter 3 2 5 Instrument stiffness f Stifness function from configuration C Const stifness mN um 3744 3 Use this field to select whether the stiffness function from Configuration default recommended is used for calculating the stiffness function or a load independent constant instrument stiffness in mN um Allow negative in
50. s 0 5mm Step 0 001nm s 0 inm Calc Pressing the left or right key will increase or reduce the drift rate in steps of 0 005nm s The step size can also be selected in the pop up menu After the optimum match between the two curves has been found the critical load for the elastic plastic transition must be defined This is the point at which the loading and unloading curves begin to diverge Click on the Calculation button to obtain an estimate of the location of this point The yield point is indicated by a blue cross Fig 84 The position of the blue cross can be adjusted by hand afterwards Enlarge the area of the diagram around the cross as in the image below and use the blue arrow keys to move the cross to the point at which the elastic plastic transition can clearly be seen The critical force for the yield point is shown in the Results field in the right hand part of the window This is the force value for the Y axis divided by the unloading ratio quotient from force after unloading and maximum force of the selected cycle In the example a critical force of 13 408mN was attained with an unloading ratio of 35 75 The ELASTICA software is required to determine the von Mises stress as a measure of the yield stress The input parameters for the calculation indenter radius critical force can be taken from the 81 asmec ADVANCED SURFACE MECHANICS IndentAnalyser results E nisi
51. sasmec ADVANCED SURFACE MECHANICS IndentAnalyser Version 3 User Manual Last revision 12 August 2014 asmec ADVANCED SURFACE MECHANICS Disclaimer All trademarks in this user manual are the property of their respective owners and are recognized as such Although every care has been taken in compiling the information contained in this User Manual no guarantee regarding the completeness or correctness of this information is offered or implied ASMEC GmbH accepts no liability for damage resulting from disregarding or non observance of the instructions in this manual In the event of difficulties not covered by this manual or where the instructions appear to be unclear please contact our Service Department at service asmec de ASMEC Advanced Surface Mechanics GmbH Bautzner Landstra e 45 01099 Radeberg OT Rossendorf Chief Executive Officer Dr Jan Stefan Roell Prokuristen Dr Thomas Chudoba Ronald Schliefer Handelsregister Dresden HRB 22387 USt IdNr DE 813898987 Tel 49 0 351 2695 345 Fax 49 0 351 2695 346 E mail info asmec de Website www asmec de asmec ADVANCED SURFACE MECHANICS Table of Contents hss AIR aC eee a E A 6 2 Program Startup and first stepS eeeesseseesesrensssrerssrrersrrrresrrerssreresererssreresererssrereserressreresrteessrereserressee 6 2 1 Starting the program as a trial version cccccccssseccccseccccescceceusececeuneceeeeueceeeeeecessunecee
52. shown as contour plot left or 3D grid right 24 75 24 50 24 25 HjGPa 4 00 23 75 23 50 23 25 0 20 0 30 0 40 0 50 0 60 Fig 35 Results shown as line graph 42 asmec ADVANCED SURFACE MECHANICS 3 8 Creating a report 3 8 1 Formatting the report A report can be produced if at least on entry is present in the Results table Click on the Report button and two windows will appear Report Preparation small and Measurement Report Preview preview window in background The settings for the content shown in the report are performed in the Report Preparation window which contains several pages Results page check the values to be shown in the report By default these are the values which are also shown in the Results table However all available values are accessible Report Preparation _ n D ammm mS W Include Load Displacement Chart into Report W Add Errors to Results Printer Setup Print Fig 36 Results page of the Report Preparation window In the top part of the page check to select whether e A graphic with the measured load displacement curves is shown in the report nclude Load Displacement Chart in Report e Error descriptions are included in the report Add Errors to Results All changes immediately become effective in the preview window where you can check that the formatting is suitable Sample page this page already contains all the information available for
53. stability and the noise of the force or displacement signal It should be noted that the noise shown will be reduced when multiple data files are averaged This window is therefore not suitable for determining the Contact force for Piezo see chapter 4 2 62 asmec ADVANCED SURFACE MECHANICS Average results Quar2fB2_B2_0009 DAT Approach Force mN Displacement um Force Displacement 16 14 12 10 6 4 2 0 lV Force over time Necscsssccssssescnseeesssssscsseeeen Time s WV Displacement over time Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 58 The Approach page of the Average results window It is possible to zoom in to the graph and view details shortly before detection of surface contact 5 1 6 Special page Many different variations of loading and unloading curves can be shown on the Special page to allow different models and fit procedures to be tried The parameters for the X axis and Y axis can be selected to the right of the graph e Time e Displacement e Force e n Displacement natural logarithm of displacement e n Force natural logarithm of force e Root Displacement square root of the displacement e Displacement 3 2 displacement to the power of 3 2 e Displacement 2 displacement squared e Root Force square root of the force e Force42 3 force to the power of 3 2 e Force 2 forc
54. the data rows can be recognized by the words Raw data CSV File Version 1001 indenter type Other Tip radius 000 um Hardness unit Dynamic hardness Read times 1 Objective lens 40 Folder for test data C DUH Data Folder for ASCII data C DUH Data Test condition Test mode Load unload Sample name S S Sample No Test force 10 000 mN Loading speed 3 4740mN sec Hold time 5 sec Test count 5 Parameter name Temp Parameter 180 Comment Shimadzu Corporation Test result J96 BM 14 10mN 1 Force Depth1 Depth2 Depth3 Depth4 1 2 Elasticity Length mN um um um um Pa um 9 000000 0 148926 0 042114 0 103791 0 045135 0 000000 0 000000 0 0000080 Raw data 74 Data no Depth Force Time UmM mMN sec 53 1 929 0 008 3 650 53 1 904 0 006 3 600 5 1 878 0 007 3 550 9 8 Nanotest data Only ASCII data can be read The file extension should be LDD or TXT A different file extension can be set on the Instrument page in the configuration The file header of the LDD files must consist of 10 rows The first digit gives the number of 137 asmec ADVANCED SURFACE MECHANICS measurements in the file With this file type the time is not exported too If time data are not available a time interval of 0 1 seconds between two points is assumed With TXT files no identifier for the columns and no hea
55. the configuration Reading is done via the Open amp button or the menu item File gt Open Data File In the Open dialog the file type is selected under Object type and the corresponding file is opened Offnen suchen in baa CF Ee yFischerscope DOs ne Fischerscope WIN Zuletzt High Load Stress Strain verwendete D C Manoindenter XP DCM Fra UNAT Desktop Eigene Dateien Arbeitsplatz a Objekthame Netzwerkumgeb Objekttyp ASM EC UNAT Data File DAT x Abbrechen ung ASMEC ONAT Data File DAT Indent nalyser reference data file AEF Multi data file DAA Average data file AVA Fig 42 Dialog window for selecting data files After a measurement has started or after reading a file the Status window appears on the left hand side of the screen giving the application the point number and the point co ordinates The Measurement data window on the right contains the load displacement curve and all the individual datasets in a table The file name is shown in the window header The table shows N measuring point number F mN force F h um displacement t s time 47 asmec ADVANCED SURFACE MECHANICS The units depend on what was selected during configuration If a dynamic mode was used for the measurement the curves for force and displacement amplitude will also be shown You can switch between the Amplitudes and Phases displays i S I
56. the sample This is the information which was specified in the Sample window before the measurement Check Include in Report to specify that the sample data will be included in the report 43 asmec ADVANCED SURFACE MECHANICS Report Preparation Results Sample Customer Print Options W Include into Report Sample Hame TiN Sample Ho Co Comment 1 Standard deposition process Comment 2 J Maternal Mew Material Substrate Steel Thickness nm Layer 1 TiN 2000 Layer 2 none E Layer 3 Printer Setup Print Fig 37 Sample page of the Report Preparation window The report header then appears as shown below zasmec ADVANCED SBURFACE MECHANICS Measurement Report Report Date 04 12 2073 17 57 31 Indentation Sam ple Sample Name TiN Substrate Steel Sample Mo 11 Coating 1 2000 nm TiN Standard deposition process Fig 38 Report header with sample data Customer page customer data can be entered on this page The data will automatically be stored in the program and will be available again when next called up Only one customer can be defined at a time Check Include in Report to specify that the customer data will be included in the report 5 r bepa Bieparalog _ _ lt eS FirstName Hen SSS Ll LZ Organisation ASMEC GmbH Department Street Ho City Phone Fax E Mail Printer Setup Print Fig 39 Customer page of Repor
57. the sample from the reduced modulus including indenter deformation which can only be measured Often only an estimate can be used The following values can be used if the actual Poisson s ratio is not known steel nickel iron 0 3 most metals 0 35 gold lead palladium platinum 0 4 glasses 0 2 ceramics and hard coatings 0 25 DLC diamond like carbon 0 2 polymers 0 4 wood 0 3 Changing the Poisson s ratio causes an immediate recalculation of the results The Poisson s ratio which was used in the analysis is saved in the AVR file so is restored when the file is opened again Pile up correction factor correction for consideration of the pile up effect i e the occurrence of plastic deformation of the material upward bulging around the edges of the indentation which result in shift of the surface position A value greater than 1 means that the contact surface is greater than the result of the first calculation pile up while a value less than 1 indicates sinking in at the edges The size of the pile up effect cannot be obtained from the indentation curve alone It requires an additional measurement of the profile using AFM or another type of profilometer 59 sasmec ADVANCED SURFACE MECHANICS Fig 54 Example for the pile up effect in copper 5 1 2 Creep page This page shows one or more creep curves during a hold period of the force at a local force maximum after correction of therma
58. this case smoothing can be carried out by increasing the number of adjacent points for calculation of the rate using the Smoothing range field All signals are shown on the left axis of the diagram Depending on the unit they may have very different maximum values e g 1um for depth and 500mN for force and the shape of the curve cannot be identified clearly For this reason curves can be scaled automatically by pressing Auto scale or by hand using a factor in the Factor fields All curves are then scaled so as to have the same maximum The resulting scaling factor can be read in the Factor fields and in the diagram legend Scaling can be prevented by unchecking the Scale box er hverage feos QuarzfB2_B2_0009 DAT Show Force mN x2 6657 C Loading rate a Displ um x278 39 Stiffness mN um x1 Show Displacement over time C Displacement rate Strain rate Smoothing range for rate calculation points left right 1 S Show Scale Factor lv v Force 2 6657 iV IW Displace 278 39 Wo Stiffness 1 0 20 40 60 80 100 120 140 160 180 200 Time s Auto scale Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 57 The Time dependence page of the Average results window 5 1 5 Approach page The Approach page shows data from the approach of the indenter to the surface before contact occurs It allows checking the
59. to limit the number of file names on view You must change the file type in the selection bar in order to see the next 100 file names 100 199 etc WinUMIS2 data files exist in ASCII format with the following structure First row Fused Silica LP2 5 MB2 100mN 000 0 0 0 0 0 0 0 0 21 01 02 15 18 57 False 0 LP2 133 asmec ADVANCED SURFACE MECHANICS 55335335 1ime P mN ht um Stiffness dP dh Lateral Force mN Lateral Position um P ht unused hp a R dP dh E H unused unused unused unused unused Second row IC 0 4 35655855910443E 3 2 85595325398774E 04 0 3333339333993 Third and following rows Loading 2 25 2 95093053589148E 3 1 2225058137157E 03 0 0 0 55555 Loading 4 51000000000204 4 24044269080789E 02 3 89028786499682E 03 0 0 0 The segment type is indicated by the first word in each row The arrangement of the columns must be as follows Time Force P depth ht Additional columns are not imported 9 4 Fischerscope data DOS software version Only ASCII data can be imported Use the instrument software export program It is recommended that all files in a series are saved in an ASCII file using the file extension DAT A different file extension can be set on the Instrument page in configuration Use of the Profi output protocol is strongly recommended To use data in the load range below 0 4mN the Output Protocol must be changed using the Supervisor Change Protocol m
60. value is in the left segment and the Y value is in the middle segment The values must each be noted manually or transferred for further use Pressing the button again disables the function i Copy to clipboard copies the current diagram to the clipboard It can then be pasted into other programs such as Word or Excel Print graph starts the print preview for the diagram The printer on page layout margin settings and other parameters can be selected here and the diagram printed Fi Save graph as picture opens the file explorer to save the diagram in these formats WMF Windows Meta File BMP Bitmap JPG JPG format PDF portable document format Marks larger enlarges the data point markers for curves if present by one pixel in both X and Y directions Maximum size is 12 Marks smaller reduces the size of the data point markers for curves if present by one pixel in both X and Y directions Minimum size is 1 j gt Lines thicker increases the line thickness of the curves by one pixel Maximum size is 15 ka Lines thinner reduces the line thickness of the curves by one pixel Minimum size is 1 37 asmec ADVANCED SURFACE MECHANICS A Letters larger increases the font size for all headings and captions by one step A Letters smaller reduces the font size for all headings and captions by one step AE Background grid on off turns the background grid on the diagram on and off The other button
61. via Tools gt Modulus Converter When the Average results window is open the results are automatically transferred to the modulus converter An isotropic body is fully defined by two elastic constants If Young s modulus E and Poisson s ratio v are known the bulk modulus K and the shear modulus G can also be calculated via the formulae K E und G E 3 6v 2 1 v By transposing the formulae Young s modulus and Poisson s ratio can also be calculated from the bulk and shear moduli If one of the values is changed all the others are automatically re calculated in the window It is then necessary to stipulate via the E const and n const buttons whether Young s modulus or Poisson s ratio is to remain constant The reduced Young s modulus is an average modulus composed of the elastic properties of the indenter Index i and the sample Index s Isotropy of the indenter is also a requirement It is calculated according to E E Only the reduced Young s modulus can be determined directly from indentation experiments The Young s modulus of the sample can only be calculated if the elastic constants of the indenter are known and an assumption is made for the Poisson s ratio of the sample Modulus Converter Youngs Modulus E GPa Poisson s Ratio n indenter fa 0 07 Sample 220 03 199 63 faa Reduced Modulus GPa Econst Bulk Modulus GPa 183 33 f neconst Shear Modulus GPa 84 615 Close Fig 126 T
62. 0 Hardness modulus sae l p measurement with QCSM method onma Force closed loop f Displacement closed loon ite Farce onen la iO Ay nlacement oneri loan Absolute position of reference seat Ante ct See a X mm M6326 Y mm B6482 Z mm 3 9511 Tncrease per cycle Decrease to Time s Patel Cycle Force mN Points i Type Dwell 3 Progress Mode sa Approach 0 0 000 undefined Eve undefined 0 00 Linear SEBE pase TE TEDES Find Surface 0 0 300 2 04 no 0 10 Quadratic X um 225 Load 1 220 000 103 87 no 30 3 00 Quadratic Creep 1 220 000 15 44 na E 3 00 Linear Y um 250 Unload 1 22 000 6 00 na 20 0 10 Quadratic Hold 1 22 000 60 00 n FO 0 50 Linear Final Unload 0 0 264 1 60 no E 0 10 Linear Z um 0 034903 Goto position below indenter Goto position below camera Restore application parameter cn i Fig 24 The Position and Segments page of the Information window Applied Corrections page This page shows corrections applied to the test data It is possible at any time subsequently to trace the parameters and results for surface detection zero point correction and thermal drift correction Information for TIN_Bi_QCSM_3 220mN AVR Mairi Position and segments Instrument Indenter Appled corrections Hardware Sample Poisson s ratio 0 25 Used contact force pM 20 Zero point correction done y Piei Correction method Ta Hertz Ty hl arial
63. 0 0 40 0 50 0 60 0 70 Contact depth um Fig 69 Comparison of ratios of Martens hardness and indentation hardness for the same samples ea 5 2 Evaluation of variable load displacement measurements This application allows fully flexible programming of measurements with force or displacement control in open or closed loop mode with no restriction on the parameters of the individual segments This also includes measurements without surface detection only for displacement control or measurements with unloading up to negative indentation depth for analysis of adhesion effects An evaluation using the Average results window will only deliver reasonable results for hardness and modulus if the application is programmed for a normal hardness test In any other case evaluation must be performed by the operator using the Measurement data window which opens when a DAT file is imported or by exporting the data to external software Normal Force mN 0 020 0 000 0 020 0 040 Normal Displacement um Fig 70 Measured curve for adhesion measurement between a silicon sphere and a flat silicon sample The example in Fig 71 shows the force displacement curve from a measurement where a smooth silicon sphere of 3mm diameter was pressed against a flat silicon piece The measurement was 70 asmec ADVANCED SURFACE MECHANICS done under displacement control and it can be seen that due to adhesion effects a negative force is required to remove t
64. 00 vee LOR Normal Displacement um Collect Analyse B deN Fig 81 A cyclic measured curve for determination of yield point in the Measurement data window Measurement data from DP21_S10 2_0005 DAT Po ey i p Measurement points Signals over time Giaphe Marks V Force Iv V Displacement IV Piezo voltage V 70 60 50 5 40 s z 30 a Scale Factor WV F Scale f 20 M D Scale 300 02 V Y Scale fi Aut 10 e Av Force mN x1 Displacement um x300_02 Subtract compliance 0 I Show title I Show legend 0 20 40 60 80 100 120 140 160 180 Time s 4 fd Normal F h Curve Normal data over time Image Fig 82 Chronological sequence of a measurement for the determination of the yield point with a hold period at the end to determine the thermal drift In the special Average results window the points from the loading cycles always just 1 point and the points from the unloading cycles are connected by two black lines These two curves are approximated by a red fit curve for the loading values and a green fit curve for the unloading values Fig 83 In the purely elastic range both curves should match at small indentation depths However there may often be a small difference between the two curves from the beginning due to the effects of thermal drift and surface roughness This can be corrected by using the Find optimum button The best match between the red and green curves in the lo
65. 000 V Measurement 1 lv Fit 4 0 Stiffness calcul 10 20 30 40 50 60 70 80 90 100 Save in CFG file Save in Database Displacement um is Cl a Fig 115 The Instrument stiffness function calibration window with the loading curve of a 1 1KN measurement into a hardness reference block After reading the loading curve for the measurement is displayed The local gradient and hence the 113 asmec ADVANCED SURFACE MECHANICS exponent of the power function is determined section by section for each part of the loading curve The following display options are available in the Show field e Load Depth displays the loading curve e n Load Depth logarithmic display of the loading curve The curve should be a straight line otherwise the correction method cannot be applied e Loading exponent local exponent of the loading curve After calculation the following can also be displayed e Instr stiffness function of instrument stiffness or compliance Presentation stiffness e Instr compliance function of instrument compliance Presentation Compliance Press Stiffness calcul to start the calculation The bowing of individual sections of the loading curve is varied point wise by varying the value for instrument stiffness until the desired exponent is achieved If the instrument stiffness in the measurement data has already been over corrected negative values for compliance can also be permitted by clicking on A
66. 04T H SMessdatenS ONAT Datensindenter BSAreatunction BS 22 05 2008 Quare_ BS 0027 DAT H MesedatenSU NAT Datensindenter bS4reatunction BS 22 05 200850uarz BS 0028 04T H MesedatenSUNaAT Datensindenter BS4Areatunction BS 22 05 2008 Quare_BS 0029 DAT H MesedatenSUNaAT Datenslndenter B S4Areafunction BS 22 05 200850uarz B5 O030 0A4T Ho correction done Fig 51 The File selection window with options for averaging curves Order monn nnn nnnP eee RPh PP e ests tS SO A Analyser f Every single file Equal parameters same sample equal load or depth same cycles W Store average data automatically as AYA Sample Poisson s ratio a2 Zer point comection qr Thermal dritt correction Manual Manual f Automatic Automatic f None f None ie Save all files with equal load depth after correction as DAA Allow average of data trom different samples Allow average of data trom different indenters Tolerance limits for averaging Segment point number tolerance 7 20 Force tolerance 22 of Frias 1 Minimum force tol for averaging mH 0 05 Segment time tolerance 4 20 Add files Start comection Close Store average data automatically as AVR specifies that a new data file with the extension AVR average will be stored for each averaged curve default setting This has the advantage that correction and averaging do not need to be repeated if the data are re evaluated at some point This
67. 1 Indenter radius Opening angle Time Force 0003 0 0103 0 0203 0 0349 0 0369 0 0378 um Displacement Segment 0 5192 Q 0 5392 0 5591 139 asmec ADVANCED SURFACE MECHANICS Example of the file structure of the TRA format The type of data column is identified by the file header This only works for English or German designations Version 1 Prufzeit Traversenwegaufnehmer Eindringtiefe Standardkraft sh 5 pum um N 7 81246e 005 1 56683e 006 0 308276 0 031949 00992187 1 56683e 006 0 308276 0 0320273 0299219 0409373 0 348271 0 0327634 0399219 0 040937350 348272 0 0325598 Version 2 Standardkraft Standardweg Prufzeit 3 333215e 002 4 325458e 007 2 148440e 004 7 650584e 002 9 994958e 002 9 785156e 003 1 029973e 001 9 991835e 002 2 978516e 002 Version 3 Fliefkurve Messing ZPV Anzahl Zyklen Stufen 5 Maximale Prufkraft 30 0166 N Geschwindigkeit Belastung 0 5 N s Geschwindigkeit Entlastung 0 5 N s Pr fzeit Eindringtiefe Standardkraft 4 882812e 006 4 893224e 002 4 281736e 002 2 000488e 002 8 885043e 002 5 928558e 002 4 000488e 002 1 087932e 001 7 081333e 002 140
68. 3 Maximum friction 0 182 Minimum friction 0 066 Work per cycle pJ 9 517 Average displacement pm 1 541 Maximum displacement pm 1 567 Friction coefficient Normal Displacement um 0 20 40 60 80 100 Cycle number Show legend A Fig 98 The Lateral Data Analysis window with the average values for friction and wear depth over cycle number 5 11 ES Analysis of tensile tests The evaluation of tensile tests also takes place in the Measurement data window After reading a data file the curves are shown here Normal Force mN 1 0 0 0 1 0 2 0 Normal Displacement um Fig 99 Example of the display on the Normal F h Curve page in the Measurement Data window during measurement In measurements using the Z stage only the displacement signal from the measuring head is visible during measurement and is controlled close to zero The residual deflection is later added to the Z stage 95 asmec ADVANCED SURFACE MECHANICS movement This curve does not provide useful information Only when the measurements are complete can a worthwhile curve which also considers the stage movement of the Z stage on the displacement axis be displayed Force displacement curve 1 000 900 800 700 600 500 Force mN 400 300 200 100 0 50 100 150 200 250 300 350 400 Displacement um Fig 100 Complete force displacement curve after a tensile test with Z stage on thin metal wire In this examp
69. 505 2415189 182 8160719 E 8 609128219 Cancel Fig 129 Showing input data black fit curve red and deviation from fit blue On the right is the window for changing coefficients and fit range After a fit has been performed the result can be saved in a parameter file ending in PAR via the button This is a simple text file in which the function number the number of terms the coefficients and the fit range are stored A file of this type can be re imported via Read PAR Only the fit function without data will then be shown The Modify button opens the Coefficients window Fig 129 in which all data for the fit are shown and can be changed This allows for example a different fit function to be selected or the fit range changed Click OK for the change to be applied and executed immediately 122 asmec ADVANCED SURFACE MECHANICS 8 Explanation of Results and Formulas 8 1 Explanation of results of hardness tests Symbol Description Number of measurement when several measurements are analyzed at once Cycle number for measurements with several load unload cycles for which hardness Cycle data can be obtained for every cycle Relative X coordinate of the measurement Relative Y coordinate of the measurement Y Relative Z coordinate of the measurement Sample number as integer value Maximum test force normal direction of a measurement or a loading cycle Indentation depth under applied tes
70. 7 0 9 0 21303 00 0213239 1 0 232 0229075 1 1 0 251157 0243202 1 2 0 270131 0 0257106 1 3 0 289107 Q 0270712 1 4 O 308083 Q 0283723 T5 0 327059 0296809 1 6 Q 34622 0 030982 1 7 0 365198 0322014 1 8 Q 384176 0334505 1 9 403155 Q 0346178 2 135 Kraft mN Q 422323 0 519255 Tiefe um 0356736 Q 0413614 Zeit sec 0 1 0 2 Example 2 with no data below 0 4mN Untitled hap 18 02 2002 16 21 05 HUkorr 0 100007 30 0 300 3989 4 x 8 00 y 12 94 F h t 4 205046e 001 7 530984e 001 1 085815e 000 1 418530e 000 1 751307e 000 2 084512e 000 2 415367e 002 3 961656e 002 5 067367e 002 6 173077e 00e2 7 057077e 0e2 7 941788e 002 9 5 Hysitron data 1 000000e 001 2 000000e 001 3 000000e 001 4 000000e 001 5 000000e 001 6 000000e 001 asmec ADVANCED SURFACE MECHANICS Only ASCII data can be imported The file extension should be TXT A different file extension can be set on the Instrument page in the configuration The file header should consist of 3 rows The third row contains the description of the data columns Depth nm Load uN Time s 000000 1 023817 000000 099956 1 007790 003000 Additional text lines before the numbers and additional columns are ignored The data columns must be arranged this way with units nm uN and s otherwise an error will occur The file structure with the Loading Creep Unloading and Hold Period segme
71. 9 Test 10 Test 11 Test 12 Test 13 Test 14 Test 15 R Test 16 fa Test 17 fal Test 18 Test 19 R Test 20 ic Test 21 a Test 22 i eccncgunseunsounscong K K A K K I KI 00d 09090 KI KI KI KI KI KI KI KI lt I 4 Fig 50 Data overview window ia File selection for analysis Ho Max Load File jame 00 000 mH 2 S00 000 mH 3 500 000 mH 4 500 000 mH 5 00 000 mH 5 500 000 mH f 500 000 mH a 500 000 mH J 00 000 mH 10 500 000 mH 11 300 000 mH 12 300 000 mH 13 300 000 mH 14 300 000 rit 15 300 000 mH 16 300 000 mH 17 300 000 mH 18 300 000 mH 13 300 000 mH z0 300 000 mH zl 100 000 mH oe 100 000 ret 23 100 000 mH 24 100 000 mH ad 100 000 mH 26 100 000 mH ae 100 000 mH ao 100 000 mH ed 100 000 ret 30 100 000 mH H MessdatenS UNAT Datensindenter BS4reatunction BS 22 05 200850uarz B5 _0001 0AT H SMessdatenS UNAT Datensindenter BS4reafunction BS 22 05 200850uarz B5 0002 DAT H SMessdatenS ONAT D atensindenter B BrAreafuncton BS 22 05 200850uarz B5 O003 04T H MesedatenSU NAT Datensindenter BSAreafunction BS 22 05 200850uarz BS 0004 DAT H MessdatenS UNAT D atensindenter E SAreatunction BS 22 05 200850uarz B5 0005 04T H SMessdatenS UNAT Daten indenter BS4Areatunction BS 22 05 2008 Querz_B5 _0006 DAT H SMessdatent UNAT Datenslndenter B S44reatunction BS 22 05 2008 GQuare B5 0007 DAT H MesedatenSUNaAT Datensindenter BS4reatunction BS 22 05 2008Quaerz BS 0008 DAT H MesedatenSUNaAT Datens
72. Access to the elastic fit method is only possible if the Average results window is open The window can then be opened with the Elastic fit Va button in this window It will open automatically if the Elastic modulus measurements with spheres application was used The Young s modulus which has been determined and the Poisson s ratio from the Average results window are automatically transferred to the substrate properties fields The loading and unloading portions of the force displacement curve are shown separately and an average value is calculated for both parts Normally the average value is the most accurate curve and should be used for the fit The Fit of f Loading curve f Unloading curve f A f Average of both selection is done via the Fit of field 77 asmec ADVANCED SURFACE MECHANICS Please note if a curve with low plastic deformation is selected the loading and unloading portions will not match and the averaged curve may be strangely shaped In this case only the loading curve must be used This type of calculation can be useful if the first part of the loading curve is elastic and only the first few points of the loading curve are to be used for the fit The composition of the sample is specified using the buttons at top left When the window is opened it is assumed that no layer is present Use the radio buttons to select the number of layers The modulus and Poisson s ratio from the Average results window are transf
73. Approach segment is selected as the first segment in the measurement cycle The data obtained before surface contact can then be used for more accurate zero point correction As a contact force greater than zero is always necessary in order to find the surface the zero point correction is also always necessary The only time it may be possible to dispense with zero point correction is in measurements with very great indentation depth as the error is then negligible To start zero point correction for a measurement select the Normal F h Curve tab in the Measurement data window and click on the Analyse button You can also start the analysis by using the Analysis button in the main menu If there are multiple curves the same thing will happen if you press the Start correction button in the File selection for analysis window In this case the zero point correction must be performed successively for each measurement The Zero point correction window opens and the first data points of the measured curve and the last 50 points of the approach segment are displayed together with a green and a purple fit curve The fit method is selected in the configuration and can also be changed in the Zero point correction window itself using the Fit method option buttons Normally a Hertzian contact is assumed where the load displacement curve follows the relationship F C h h0O The curve is shifted to the left or right by a change in the hg value until the
74. Av Displacement um x105 41 the diagram by holding down the left mouse button and draggin Ay Voltage v xd 7333 8 y 8 881N8 It ME Measurement data from Quarz_81 0005 DAT Measurement points Signals over time Graphs Marks V Force V V Displacement V Piezo voltage V V Norm stiffness Y B j Iv Vibration Stiffness C Phase C Amplitude gt 3 5 Zz s E Scale Factor T v V FScale 1 c 2 v M D Scale f1 o E _ a IV Y Scale 1 e Ay Force mN x1 Auto scale Av Displacement um x1 Stiffness M Subtract compliance IV Show title IV Show legend 0 20 40 60 80 100 120 140 160 180 200 Time s He id Fig 44 The Normal data over time page in the Measurement data window Check the Scale fields to select which curves are to be scaled Scale Factor W F Scale fi F force W D Scale 105 61 D displacement Jv Y Scale 2 7333 p V voltage The scaling factor is selected manually by entering it in the Factor fields The scaling becomes effective when you exit the field via the TAB key or mouse click Check the appropriate boxes in the bottom subwindow to decide whether the graph has a title Show title or a legend Show legend Approach page shows the force and displacement data for the approach segment in which the tip is lowered by the actuator to detect the surface 49 sasmec ADVANCED SURFACE MECHANICS The page is not visible if no approach dat
75. Determined with Areafunction_Quarz_neu AREA 00 Indenter area function WV Use area or radius function Use area function for Martens hardness Validity range from 29 1 1 2013 To 30 1 1 2014 Stored at 01 12 2013 Correction type One area function ee 4 9038 Ideal 4 95 above fit range Description by One fit function Two fit functions Data table Radius function 1 Fit function no E 9 2 Fit function no fo F Data table Coefficients Edit Coefficients 0 001 um 3 16371 um 0 002081112 0 001899715 0 4124063 4 737036 0 01733936 amp Open DB fey Save in De Fig 15 The Indenter page of the Configuration window indenter type Berkovich indenter no eo 0 Area function no Ja Indenter type In this bar the indenter type is selected from the pull down menu The following types are available Vickers for hardness and modulus measurements 22 asmec ADVANCED SURFACE MECHANICS Berkovich for hardness and modulus measurements Sphere for modulus measurements scratch tests wear tests and surface scans cube corner for special hardness measurements and fracture toughness investigations Cone for special tests Flat punch for special investigations Rockwell cone with an opening angle of 120 and a spherical cap of 200um radius Knoop for special investigations only not suitable for Young s modulus measurements The message below appears when the type of indente
76. Displacement amplitude x100 Normal Force mN Amplitide mN um 0 00 0 10 0 20 0 30 0 40 0 50 0 60 0 70 0 80 0 90 Normal Displacement um Fig 75 Example for the graph from a QCSM test on fused silica in the Measurement data window In addition to the force displacement curve shown in black the Measurement data window also shows the vibration amplitude of the force signal in blue and the vibration amplitude of the displacement signal in green Both amplitude curves belong to the right hand axis of the diagram Force amplitude is expressed in mN and displacement amplitude in um The final evaluation of the QCSM data then takes place in the Average results window Usually multiple measurements with the same parameters are averaged and only the averaged curve is evaluated The Vibration page shows the amplitudes and the phase shift between the piezo voltage driving voltage and the displacement and force signals This page is only visible for data from ASMEC UNAT instruments In contrast to the CSM method used with other instruments in which the vibration is applied directly to the shaft with the tip and where the phase shift between force and displacement signals can directly be measured in the QCSM method the phase of the two signals can only be measured with regard to the piezo movement The force oscillation further arises only after surface contact at low frequencies where the inertial mass does not play a role The phase shift b
77. Printer Setup button opens the Print setup window Indentation Indentation ADVANCED SURFACE MECHANICS Measurement Report ADVANCED SURFACE MECHANICS Measurement Report Report Date 04 12 2013 12 15 05 Report Date 04 12 2013 12 36 00 Customer Her Mustermann Customer Her Mustermann ASMEC GmbH ASMEC GmbH 49 351 2695 345 49 351 2695 345 Sample Sample Name TiN Substrate Steel Sample Sample Name TiN Substrste Steel Sample No 11 Coating 1 2000 nm TiN Sample No 11 Costing 1 2000 nm TiN Standard deposition process Standard deposition process Results Results H GPa E GPa 516 7 489 0 459 7 488 5 23 3 0 000 File name N F mN h pm H GPa E GPa ns File name TiN_B1_QCSM_3_130mN AVR 1 120 028 0 538 23 61 516 7 0 250 TiN_B1_QCSM_3_120mN AVR TiN_B1_QCSM_2 150mN AVR 1 150 040 0 580 24 40 489 0 0 250 TiN_B1_QCSM_3_150mN AVR 1 TiN_B1_QCSM_3_180mN AVR TiN_B1_QCSM_3_180mN AVR 180 047 0 640 25 62 459 7 0 250 TE _ Average Standard dev 48 0 000 459 7 0 250 180 047 516 7 0 250 File name HV kpimm CIT Wtot nd We nJ NIT S mNipm TiN_B1_QCSM_2_120mMN AVR 2187 4 0 99 24 764 10 790 43 57 985 32 TiN_B1_QCSM_2 150mN AVR 2259 9 0 93 20 865 13 471 43 64 1002 95 TiN_B1_QCSM_3_180mN AVR 2373 1 0 93 41 076 17 940 43 67 1027 15 aa 00 als22 B CIT NIT 9 S mN m TiN_B1_QCSM_3_130mN AVR 0 99 43 57 File name he um TiN_B1_QCSM_3_150mN AVR 0 93 r 43 64 TiN_B1_QCSM_3_180mN AVR 0 93 g 43 67 Average 0 95 43 63
78. RFACE MECHANICS The values in this field can be transferred to other programs by copying and pasting Check tick the individual boxes to enable or disable the curves or set point markers W Scratch depth Marks W Pre Scan Marks Subtract if Post Scan Marks Normal force Marks We Lateral force Marks ia Marks lf Show cursor ee te iw Show legend lt more Read background image Ere i Scratch depth N shift postscan distance it post scan distance um B Peta ey s ay Step Inm s Step 0 5nm s Estimated offset um Step 0 1nm s Drift rate nms Step hehe Step 0 01nm s lols amw Step0 005nm s Step 0 001 nm s The curves and the point marks can be switched on or out by checking the belonging fields Subtract is used to subtract the pre scan curve if present from the other depth curves This can be used to reduce the effect of surface roughness somewhat In this way a peak on the surface becomes a valley in the other curves As thermal drift also occurs during a scratch test and the measurement time is often 100 seconds or more thermal drift should be corrected to obtain an accurate evaluation The More button opens an additional window for this purpose A drift rate can be generated with the lower two arrow keys and applied to the measured curves A criterion which can be used for the best correction is for the pre and post scan curves to lie approxi
79. Results over Depth page Fig 73 The parameters for the X axis and Y axis can be selected with the corresponding pull down menus 71 asmec ADVANCED SURFACE MECHANICS y Average results Quartz B8 100m AVR F 79 990 0 003 mN h 0 854 0 002 um H 8 849 0 134 GPa E 71 78 1 20 GPa Er 69 43 1 16 GPa ns 0 170 HV 819 7 12 4 kp mm2 Git 0 78 Wtot 23 301 ng We 15 241 ng NIT 65 41 Fe 235 55 2 16 mN um m 1 287 e he 0 591 0 004 um ers a 1 696 um Y Ac 9 039 0 137 um2 T t rec 7 0 0 3 Rul Re 41 637 Sample Poisson s ratio 0 1 7 Pile up correction factor Moo Unload z fit range From 98 To 40 2 M Show fit 1 Full range Show fit 2 Full range 0 30 0 40 0 50 0 60 Displacement um 0 70 0 80 0 90 V Show tangent Tangent start at hmax Show plastic depth Show error band Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Fig 72 Cyclic measurement of fused silica with 10 cycles Quartz_B8_100mN AVR Parameter for axis Contact depth v 70 ppa 474TH 65 Parameter for Y axis ion modulus Yourra s modulus ikd 60 E Indentation modulus rouna R Er Reduced modulus 55 E Plain strain modulus withou ns Sample Poisson s ratio 50 Ei Indenter Young s modulus ni Indenter Poisson s ratio HM Martens hardness 45 HMs Martens hardness from sh H Equivalent Vickers hardne
80. The Fit Data window with displacement signal during a hold period of 120s and a linear fit The X axis is in microns The average deviation is 0 24nm The first and last points of the curve are marked with a green point when imported They identify the fit asmec ADVANCED SURFACE MECHANICS range The numbers of the points are also shown in the From point To point fields By changing the values in these fields the fit range can be restricted It can also be defined by double clicking on a point on the curve It should previously be specified in the Define by double click field whether the lower limit Left end or the upper limit Right end is to be defined by double clicking The fit function is specified via the Fit function field 24 functions are available in the current version see Chapter 8 4 The current fit function type can be displayed by clicking on the question mark d Click on Calculation to start the calculation The fit curve can then be seen as a red line and the fit results are shown at top right in the window see Fig 128 In addition the deviation from the fit can be seen as a blue curve via Show residuals The full curve is visible even if the fit range was limited This can be prevented via Show range only so that only the points in the fit range are shown see Fig 129 Data Fit Residuals Coefficients Fit function 5 Range start 5 0762 Range end 101 5 2412 761476
81. This can be used to improve the accuracy of the calculation of the area function from the indentation depth Epsilon factor C Constant f Variable In international standard ISO 14577 a constant value of 0 75 is recommended However recent results show that epsilon can vary between around 0 7 0 8 We therefore recommend using a variable epsilon factor Beta factor the beta factor B takes into account differences in elastic deformation between a rotationally symmetrical indenter cone or sphere and an indenter with sharp edges pyramid In the literature on the subject differences between 1 and 6 have been found for purely elastic calculations Additional plastic deformation reduces these differences significantly however As it is not clear how strongly plastic deformation reduces the difference a value of 1 0 for the beta factor is recommended This value is also used in ISO 14577 Beta factor 1 0 recommended fi Default sample Poisson s ratio this value is displayed in the Results Window and can be modified there later It is used to calculate the Young s modulus of the sample from the reduced Young s modulus which can only be obtained directly from indentation tests If no value is known for the sample material a value of 0 3 for metals and 0 25 for other materials is recommended Default sample Poisson s ratio 0 2 With radial displacement correction recommended checking this field will cause the lateral elasti
82. TiN_B1_QCSM_3_150mMN AVR 0 467 Standard dev 0 03 j 0 04 TiN_B1_QCSM_3_180mN AVR 0 503 Variance i 2 65 0 10 Minimum 0 93 7 43 57 Maximum 0 99 43 67 1027 15 TiN_B1_QCSM_3_120mN AVR 0 440 Load Displacement Curve File name TiN_B1_QCSM_3_130mN AVR 0 TiN_B1_QCSM_3_150mN AVR 0 TiN_B1_QCSM_3_180mN AVR_0 Average Standard dev n o So o Msximum Normal Force mN n Qo 0 2 0 4 Normal Displacement um Fig 41 Print preview in Report window On left without statistical values but with graph on right vice versa 4 Importing and Correcting Data 4 1 File types DAT standard data format for an individual measurement by IndentAnalyser The data format and file name extension for the raw data depend on the type of instrument selected With other instruments the extension will often be DAT or TXT AVR average data file This file contains the averaged and corrected force displacement and time data from multiple measurements with the same maximum force and the same number of cycles the standard deviations for each data point including measurement description sample name area function instrument stiffness and other parameters The file format is generated by IndentAnalyser or IndentAnalyser software DAA multi measurement data file DAA files contain the force displacement and time data corrected with regard to zero point and thermal drift for any required number of individual measurements incl
83. With some instruments the end of a segment is shown in the data file however the start and end of a hold period must usually be identified by searching for data with approximately constant force This depends on the noise of the force signal It is therefore important to use the correct parameters for Force tolerance for hold period and Contact force for surface detection on the Other page of the Configuration window Appropriate values are set during selection of an instrument An optimization of these parameters may nevertheless be necessary Configuration Main Hardware Instrument Indenter Analpets normal Results Uther Special parameter for instrument Hysitron Contact force surface detection WH 2 Force tolerance for hold period pM 0 5 9 2 Nanoindenter XP G200 data Only ASCII data files can be read from the nanoindenter XP G200 with or without DCM head They may also contain continuous stiffness CSM data The file extension should be TXT or CSV A different file extension can be set on the Instrument page during configuration The meaning of the data columns must be explained in the file header The columns can be arranged in any desired order but their meaning must be stated in the key words DisplacementintoSurface LoadOnSample Time or TimeOnSample Stiffness An example of a file header is Channel Data SegmentIndex Hardness Segment Number Time Displacement Into Surface
84. a exist The red curve with the displacement data shows the distance from the surface before contact 7 3 43 p Measurement points Approach data over time Graghs Marks IV Force Iv IV Displacement W I Piezo voltage M IV Show title I Show footer IV Show legend Estimation for last 10 6 s Force maximum 6 7 pN Standard deviation 2 4 pN Recommended contact force 12 yN Signal a u Force Displacement 16 14 12 10 8 6 4 2 0 Time s fe bH Normal Flh Curve Normal data overtime Approach Image Fig 45 The Approach page in the Measurement data window The display of the approach data is very helpful for checking measurement conditions The noise of the force signal during the approach of the tip is a criterion for environmental conditions and the noise performance of the electronics The contact force which should be used for the approach can be derived directly from it This is displayed in the field to the right of the graph The last 10 seconds approximately before contact with the surface are analyzed The maximum force value and standard deviation of all values during this time are given From this the Recommended contact force is obtained shown with 12uN in Fig 45 216 0 um 162 0 um 0 339 um Pixel 921654 byte Possible image size only BMP format 640 x 480 pixel 1024 768 pixel 1280 x 1024 pixel Normal Fih Curve Normal
85. a in this file 5 1 10 5 1 8 Vibration page For more information see Chapter This page belongs to the analysis of CSM QCSM measurements UNAT only The amplitudes and phases of the oscillations which allow the calculation of contact stiffness and phase shift are shown here See chapter 5 4 Evaluation of QCSM measurements El Average results 260 240 Stiffness Phase difference 220 N o oO Oo oo k Normal stiffness mN um P al ah O 0 10 0 20 0 30 Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 61 The Vibration page of the Average results window 0 40 0 50 0 60 Normal Displacement um Normal phase difference Quar2ffB2_B2_0002 DAT Normal vibration Segment 3 Load Frequency 8 49 Hz Amplitude 0 160 V Segment 4 Creep Frequency 8 49 Hz Amplitude 0 180 V AA 1 beka H O o 4 gt e2 Reset MV Marks I Fit marks Show C Amplitude Phase Stitfness Phase difference V Phase difference h F 65 asmec ADVANCED SURFACE MECHANICS 5 1 9 Extrapolation of the indentation modulus to zero indentation depth This method is used for thin coatings when it is not possible to measure the coating properties without substrate influence It is recommended in ISO 14577 Part 4 1 Hardness measurements must be performed with at least 3 differe
86. age results window with the result of a QCSM measurement on fused silica 5 5 Elastic Young s modulus measurements with spherical indenters Evaluation requires a separately purchasable software module The determination of the Young s modulus of thin layers using fully elastic measurements with a spherical indenter represents a new method which requires an analytical model for the calculation of elastic deformations of coated systems This model has only been available since 1999 T Chudoba N Schwarzer F Richter New possibilities of mechanical surface characterization with spherical indenters by comparison of experimental and theoretical results Thin Solid Films 355 356 1999 284 289 The underlying theory was developed by N Schwarzer N Schwarzer Arbitrary load distribution on a layered half space ASME Journal of Tribology 122 No 4 2000 672 681 The advantage of this model is that the influence of the substrate on the result can be fully determined and corrected Therefore the Young s modulus of very thin layers lt 100nm can be determined although average forces gt 10mN can be used for the measurements 76 asmec ADVANCED SURFACE MECHANICS The method can only be used if coating and substrate are hard enough and the surface roughness is low It cannot be used on polymers or soft metals The loading and unloading curves should agree better than 1 to2 nm An important model assumption with the new method
87. al error for the contact depth is given by e F Ah Ahna AF nay s AS S C max S m Ah the relative error for the elastic surface deformation h is given by h S S Finak Ahs _ AS AFmax AH the relative error for indentation hardness is given by AH _ AFmax 49 Aho H F max C It is assumed that the relative error for the equivalent Vickers hardness is the same as that for the indentation hardness AHM the relative error for Martens hardness is given by AHM _ AFmax 5 ANmax HM F h max max AE the relative error for the absolute and reduced indentation modulus is given by AE AS Ah E S h AA the relative error for the contact area amounts to AA _ Ang A he Aa the relative error for the equivalent contact radius corresponds to the relative error for the contact depth if the systematic error for the contact area calculation is not considered No error statements will be made for the other values in the current program version 129 asmec ADVANCED SURFACE MECHANICS 8 4 Fit functions In the program there are a number of fixed functions which are used to describe the area function or the stiffness function and with which any data in the Tools gt Fit data window can be fitted The functions are identified by consecutive numbers The table lists all the functions available in this version Where the 2 symbol appears in the program the terms of the functi
88. alog appears allowing various parameters to be selected The Print button is best suited to printing out all results and parameters plus the associated curve The maximum width or height of a page is used according to the aspect ratio of the window The dimensions of the elements font size line width etc depend on the size of the window 12 asmec ADVANCED SURFACE MECHANICS If you only wish to print the diagram use the Print buttons in the relevant window or the print button of the Graph commander The latter enables a print preview and adjustment of the various print parameters Information nfo rmation Opens an information window when a test exists or a data file has been read The window contains all relevant information including sample designation measuring position application instrument used indenter and correction functions The information window is automatically updated if a new file is read See also section 3 4 Analysis An a lysis This button is only visible if a data file has been imported and not yet evaluated i e the test data have not yet been corrected and no result is shown in the Average results window It has the same function as the Analyse buttons in the Measurement data window However this button allows easier access and ensures that no correction is overlooked 3 Configu Co nfigu ration Open the Configuration window Once the program has started the data from the most recently read CFG
89. alue in this situation 114 asmec ADVANCED SURFACE MECHANICS In this case a set value of 1 97 was anticipated for the exponent Negative values in the range of 300N arise At high loads the value for instrument stiffness compliance has a very strong influence on the result As described before Section 6 1 4 the bowing of the unloading curve may change when a stiffness function is used Whenever possible therefore only a constant value for instrument stiffness compliance should be used This is achieved via Fit type constant value The first point for determination of stiffness can be varied via Points from In the example the first two points have been disregarded The result is shown in the Mean stiffness Mean compliance field The compliance in this example is with 0 5 nm N very low This is because the data have already been corrected for stiffness All other functions of this window are as described in Section 6 To save the result of the stiffness calculation as a CFG file click on Save CFG file 6 5 Determining the instrument stiffness in tensile direction The micro grippers for clamping tensile test samples have only a finite stiffness The instrument stiffness therefore does not agree to that of an indentation test Instrument stiffness in the tensile direction can be determined by clamping a solid sample in the grips A piece of steel sheet is suitable for example Fig 118 Configuration for determining the
90. asmec ADVANCED SURFACE MECHANICS Function type Instrument stiffness can also be displayed as compliance inverse stiffness This is defined via Function Type The way how the instrument stiffness is described is usually set during the calibration routine and automatically overtaken The use of compliance instead of stiffness has the advantage that even negative compliance can be used for example if data which have already been corrected have been saved and the stiffness in the data file has been over corrected Stiffness function type the stiffness function can be defined in three different ways Constant value constant value of instrument stiffness for the entire force range of the instrument This is the typical version for instruments other than UNAT Function with up to 10 parameters instrument stiffness is defined via a function with up to 10 parameters Data table instrument stiffness is defined in the form of an ASCII table with force and stiffness values in two columns This option is not available in Version3 at present Stiffness function type O Constant value f Function with up to 10 parameters Data table Obtained from Sapphire Fused Silica quick measurement 8 2 53 Comment Average instrument stiffness When using as stiffness function the average value is displayed here for the calibrated force range When using a constant stiffness the value must be entered in this field 07 05 2007 e T ey Stor
91. asuring reference materials The determination of the area function of the indenter is carried out via measurements on a reference material with a high degree of homogeneity and precisely known elastic properties If the instrument stiffness shall be determined at the same time measurements on a second material with a significantly different Young s modulus are required Reference materials should satisfy the following requirements Homogeneity of the mechanical properties Elastic plastic isotropy Stable mechanical properties over working life No formation of surface layers especially oxides Smooth clean surface very low roughness No work hardening pile up or sink in effects No or reduced crack development during indentation Suitable hardness and Young s modulus values Fused silica or another glass is recommended for the determination of area function and sapphire or another material with a large Young s modulus is recommended for the determination of the instrument stiffness The determination of the area function should be as accurate as possible and take place over the entire load range of the instrument At least 10 measurements per load should therefore be performed For loads over 100mN 5 measurements will be sufficient For the calculation of the area function the contact stiffness is required in addition to maximum force and indentation depth The measurements must consist of loading creep and unloading segments Cyclic meas
92. ation with error a C Markoyv Chain Monte Carlo with error Q Show Z 200 True stress strain a Technical stress strain 2 150 C Plastic stress strain wn C Kinematic stress strain B C Original and corected measurement 100 C Input data over time Save results in files Iv Show RAp0 2 50 Stress Strain Curve Identified properties for Rp 0 2 Messing2 TRA 0 With kinematic hardening E Modulus GPa 111 9 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 Yield strength MPa 210 7 True strain Elast limit 3 0 188 Rpd 2 MPa 222 2 Rm MPa 301 2 S te Net Hardening exp 0 063 oaquius We Ea Viscosity Net Stress at infinite strain a sued gem ah t 6 Sigma Net Sigma MPa 328 5 og Kinematic Net Initial slope work hardening t Sigma MPa 5492 E Oo Gamma MPa 3566 7 D Beta gt 41 102 C MPa 1283 5 w B 62 079 lt Load sel Apply stiffness correction desl tH IV Show legend Close Fig 86 The Stress strain curve calculation window for determination of the stress strain curves of metals form indentations with spherical indenters 5 10 15 20 25 30 35 neuron number The following must be noted for the programming of the application as in the examples provided brass 0001 tra and brass 0002 tra 1 There are 4 isochronous phases for the linear increase of loading so that the indentation depth of the spherical indenter amounts to 0 08 0 12 x the indenter radius after the 4th l
93. ation and the fit Data from a depth range below 20nm are not very reliable in this example and should be ignored To save the result of the radius calculation as a CFG file click on Save in Configuration To distinguish it from an area function the word Radius should appear in the name 112 asmec ADVANCED SURFACE MECHANICS 6 4 Determining instrument stiffness from high load indentations with pyramidal indenters This calibration procedure for instrument stiffness is based upon the fact that a quadratic dependence F h exists between force and displacement when pyramidal indenters are used If a loading curve for an indentation made by a Vickers or Berkovich indenter in a homogeneous sample is fitted with a power function F C gt h an exponent m of approximately 2 must result This is only possible however if the tip rounding is of no relevance which can be assumed for indentation depths of 6um and more Therefore this the procedure is not suitable for nanoindenters beside very soft metal samples such as unalloyed aluminum must be used Smaller deviations from the ideal value of 2 0 also occur due to creep effects during the indentation process and to a reduction in hardness with increasing depth even with ideally homogeneous samples causing the value of the exponent generally to be slightly smaller between 1 96 and 1 99 Loading ata constant strain rate would be ideal for which const applies This causes an exponentia
94. ble above If the size or layout of the columns has been changed press the button again to reproduce the same table layout in the Statistics table 3 7 2 iik Creating a graph from the Results table It is possible to create graphs in the Comparison window directly from the Results table This can be used to produce a graph for hardness or Young s modulus over indentation depth zi To do this click on the button ii Add column data to comparison graph window The window Data selection for Graph will appear Data selction for Graph AXIS he Reset Y AXIS F With error bars if available Use the focus rectangle in the summar table to choose the column for e asis Then press OK Then use the rectange to choose the column for asis and press OF again Finally press OF a third time Fig 31 Data selection for Graph window Select a column from the Results table as the X axis by clicking on any field in the column highlighted blue then press the OK button in the Data Selection for Graph window The Y axis is selected in the same Way Comparison Show With marks All All C None C None a a e a V Graphl W h Curve no Add Graph lv Show title Show footer M Legend Iv In V Show error bars WV Start at 0 0 4 H Fig 32 Curve in Comparison window generated from Results table Please note If only one field in the column is selected all the fields in that column will be used f
95. c displacement of the sample surface to be considered in the calculation of the area function This correction takes account of the latest results from contact mechanics and improves accuracy This correction is foreseen in the latest revision of international standard ISO 14577 W With radial displacement correction recommended 27 asmec ADVANCED SURFACE MECHANICS Corrections Zero point correction Zero point correction select the type of zero point correction by clicking Manual in the appropriate field Automatic Corrections Manual manual correction the first measuring points of the loading curve are shown in the Zero point correction window and a shift of the curve around the zero point can be performed manually This is normally the most accurate method None Automatic The zero point correction is performed automatically The Zero point correction window is not shown and there is no opportunity to intervene None no zero point correction is carried out Standard fit method there are 3 options for describing the measuring points close to zero with a fit function Standard fit method Hertz for normal indentation tests a nearly elastic contact with a spherical indenter Hertz Hertz contact is assumed for the first few nanometers of the indentation With this Linear type of contact the force displacement curve follows the relationship F h In this Quadratic case however only the
96. curve are shown on the right hand side of the window Only parameters selected during configuration and associated with the creep analysis are shown Smoothing range for rate calculation allows you to specify how many adjacent points are used in calculating the gradient at one point A greater number of points means greater smoothing The creep rate is always determined if a hold period of at least 1 second is used with force control and at least 4 measuring points are present However creep time should not be less than 5 seconds and must be adjusted to the creep behavior of the materials A ratio Rul Rc is calculated from the creep rate Rc at the end of the creep period and from the unloading rate Rul in the first 20 of unloading The ratio Rul Rc should be greater than 20 otherwise the remaining creep during unloading may result in distortion of the gradient of the unloading curve and therefore lead to an inaccurate Young s modulus result The Rul Rc ratio is checked during evaluation If the value is greater than 20 seconds a warning is displayed in the Status window In this case the result should be critically reviewed However it may not be necessary to discard the result The creep period should be extended in any further measurements 5 1 3 T drift page This page shows the displacement change during the hold period for determination of thermal drift after correction of thermal drift In an ideal case this should be a horizontal line a
97. dent factor as standard deviation and n as the number of averaged measurements Error contributions due to inaccuracies in force or displacement calibration instrument stiffness or area function are not considered The display of the error bars can be deactivated via the Show error bars checkbox at the bottom of the window A reference measurement can be imported on the same page and a hardness ratio or hardness difference in relation to this measurement can be calculated and displayed This is particularly useful for very thin coatings where hardness is influenced by the rounding of the indenter tip lA Average results es fo QuarzffB2_B2_100mN 1 4 R Cycle SELESELE EEE EE peste tees se ME Pasnalor Xari as 70 Contact depth x Smoothing Parameter for Y axis bo 0 60 HM Martens hardness Reset HMd Differential Martens hardt Reset 50 HY Equivalent Vickers hardne S Contact stiffness of sample wo a Equivalent contact radius M Daks cL Ac Projected contact area with l Fit marks HE measure for yield strain a 40 H E GPa measure for resista 5 E H GPa measure for capac sear ao D di uy 30 20 10 Add results to table V Show parameter graph 0 0 00 0 10 0 20 0 30 0 40 0 50 0 60 Contact depth um V Show error bars Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 78 The Results over depth page of the Aver
98. ders are exported The sequence of force displacement and time data cannot therefore be identified There is a choice between two variants in the file selection menu 1 Time Force Depth 2 Depth Force Time It may be necessary to find the correct type by trial and error In the case of Nanotest data no data have so far been exported during the hold period Only values for Loading and Unloading are therefore available even if hold periods were used Example of an LDD file 11 Number of measurements in the file 296 Total number of points of this here the first measurement 152 Number of loading points of this measrement 6 130464e 008 Maximum depth Q 1 079208e 003 Maximum force Q O Q Q 5 838400e 005 1 1098e 009 first data line Example of a TXT file 0 586156 030000 000000 0 470559 0 032653 0 027471 0 003750 0 035896 0 061239 0 858181 0 038695 0 087904 2 383851 0 041162 0 111376 9 9 CSM NHT data Only ASCII data can be imported The file extension should be TXT A different file extension can be set on the Instrument page in the configuration The file header can be arbitrarily constructed The start of the data block is identified by the line which describes the meaning of the columns Time s Pd nm Fn mN The units must be s nm and mN or the values will not be stated correctly Any desired number of measurements in one file is possible Example of the start of a data file Indentation 1
99. e the unloading curve or the average of the two Average B Initial calculation of radius function To start the calculation of the radius function press Calculation In the Average radius field the average effective radius is given for the range in which data from all in this case from both reference materials are present The calculated radius functions are displayed as blue for Material 1 and green for Material 2 curves on the graph The average value for the two is shown as a red curve It is described with a fit function which is represented by a thicker black line on the graph The Use fit function and Use points from to fields have the same meaning as described in 6 1 4 The fit function and the points should be varied until an optimum match between the test data and the fit curve is achieved Function 5 is used as default E Effective Sphere Radius emt Read data Emodulus Poissonr CI auarz 510650 AR V Use EO 017 Sephir_S10 6 om AVR V Use 410 0 234 2 hes 0 223 Indenter 1140 0 07 Average radius um 7 5344 Use of re Use fit function 5 3 d Use points from 3 S to 53 Smoothing o Effective radius um Radius 1 Radius 2 Marks at data V Show fit Average Marks ataverage V Show legend Te 0 00 0 1 0 0 20 0 30 Save in Configuration Save in Database Effective depth um so a Bq o Fig 114 The Effective Sphere Radius window with the results of the calcul
100. e Analysis Lateral page of the Configuration window 29 asmec ADVANCED SURFACE MECHANICS The Analysis lateral page is only shown if a lateral force unit LFU is installed and use of it has been authorized on the Hardware page Spring constant for Lateral Force Unit mN um the average spring constant of the perpendicular holding springs for the LFU sample holder is automatically entered in this field The spring constant is determined by means of reference measurements No change is required Automatic reference measurement When this box is checked the lateral force unit performs an automatic reference measurement in air to determine the spring constant of the retaining springs default This setting can only be disabled during a work session The automatic reference measurement is always enabled when the software is started Depth limit for scratch test Two indentation depth limits can be set for automatic evaluations of scratch tests The force and friction values at which the limits are reached are given as results Limit 1 applies to depth under load i e including elastic deformation Limit 2 applies to the residual depth after unloading i e without elastic deformation 3 2 7 Results page On the Results page you can specify how results will be displayed in the Results window and in the Results summary table Configuration p Main Hardware Instrument Indenter Analysis normal Analysis lateral Results Othe
101. e axis The changes are confirmed with Enter Legend turns the legend on and off Click the left mouse button and drag it to move the legend within the graphic Inside By default the legend is on the right side of the graphic Use nside to position it within the graphic and save space Start at 0 0 the axes are automatically scaled to a range which enables curves to be displayed to the maximum To allow better comparisons of a number of graphs it is often preferable to start all axes at zero Show error bars this field is only active if error descriptions are available for at least one of the curves If this is the case the relevant error bars can be enabled and disabled here be store all series pressing this button enables all visible curves to be stored at the same time in TXT ASC XLS or WMF format If the TXT format is used the curves can then be re imported and all axis designations plus the assignment of the axes will be recovered This is especially useful for the comparisons of hardness or Young s modulus profiles Fit ta pressing the Fit button transfers the curve with the selected number in the field to the right of the button to the Fit Data window see chapter 7 4 where various fit functions can be used to analyze curves in more detail In all graphics the Add graph J l button can be used to copy all visible curves simultaneously to the Comparison window During this account is taken of whether a curve belongs to the
102. e is corrected via the Correct button Only after surface slope correction results will be shown in the text field on the right Measurement data from Scratch_500mN_Silicium_D_S10 6_0001 DAT Max force mN 497 818 Max distance pm 7 833 Roughness before scratch m Ra pm 0 002 Rq pm 0 003 0 25 Rt pm 0 018 Rp pm 0 010 Rv pm 0 009 Ss Average friction 0 057 0 50 Maximum friction 0 155 fai Max displacement 9 Under load pm 1 438 S 2 pe 7 Show on bottom axis Show on left axis Q 0 75 D Distance Depth gt p K o r Scratch_500mN_Silicium_D Scratch depth l Scratch_500mN_Silicium_D Lateral force Y Scratch_500mN_Silicium_D Pre scan depth 1 00 Scratch_500mN_Silicium_D Post scan depth nf j Scratch depth Marks 1 25 V Pre Scan l Marks f Subtract V Post Scan Marks Normal force Marks W Lateral force Marks B Marks 0 50 100 150 200 250 300 V Show legend IV Show cursor Distance um Goes desl Normal Fhi Curve Lateral Fih Curve Normal data over time Lateral data overtime Scratch results Approach Image Fig 91 The Scratch page in the Measurement data window after surface slope correction Three depth curves are initially shown in the Evaluation window as default Scratch depth shows the indentation depth during the scratch test under load This curve also contains the elastic deformation por
103. e squared e 1 Derivative F h 1st derivative of force displacement curve e 2 Derivative F h 2nd derivative of force displacement curve e Local Exponent f h local exponent of force displacement curve The sign means to the power of The loading and unloading curves are considered separately The upper axis shown in red belongs to the unloading curve also in red To use the same scale for upper and lower axes check Equal scale top bottom Both curves can be fitted with a linear function or with second or third order polynomials The fit function is taken from the drop down selection list The fit results are shown in the Results field at top 63 asmec ADVANCED SURFACE MECHANICS right and can be copied by selecting the lines in question and transferring them to the clipboard Ctrl Insert or Ctrl C Linear fit range beginning and end of the fit range as a percentage of the X axis Do fit starts the fit for the selected range The curve is extrapolated in the area outside the selected range also Average results koba QuarzffB2_B2_0009 DAT X axis 0 60 0 50 0 40 0 30 0 20 0 10 In Displacement Y axis Smoothing In Force 0 Function number 1 a Number of terms 2 ia Results for loading curve sessetsteeseteeeteteenee Reset const 4618731924 x 1 831586191 Fit range From 3 35506 iY Maks To 0 0473747 Fit marks Pa Exponent of loading curve m
104. e the e mail link below Your Disk ID no is A 1264330191 Updates available at hitpviwww asmec de Contact info asmec de Fig 1 Welcome window with information on use and automatically displayed Disk ID The access code should be entered in the input field Software access code of the Configuration window see Chapter 3 3 Fig 2 Configuration im Main Modules Instrument Indenter Analysts normal Results Other Selected configuration file Zwick Vickers CFG S Instrument Program owner i Software access code Get Disk ID Na 0 Time code Fig 2 Configuration window with fields for Software access code yellow and Time code red border For the full version the Software access code is required Each group of three digits must be separated by a dot in this code For a limited time trial of the full version the Time code is also required The remaining time for the trial is displayed in the Welcome window when the software is restarted 2 2 First steps d The program is started by a click on the program icon if Nf IndentAnalyser in the program menu or on the desktop The program will start automatically when a file in the program specific AVR format is clicked In the program manager the program icon should be visible in connection with this file type When the program is used the first time some steps are necessary to prepare the program for the analysis of instrument specific data a
105. e useful function is the consideration of the area function of the indenter currently in use via Use current area function This enables investigation of the influence of tip rounding of a pyramidal indenter on the indentation depth for example as shown in Fig 125 With real area function Elastic deformation For ideal Berkovich Elastic deformation above Ac Plastic deformation Elastic plastic deformation Load mN Load mN 000 42020 42 040 oeoo ogo 000 O20 4040 42060 ogo Displacement um Displacement um Fig 125 Force displacement curves for the various deformation portions for the pressure distribution of a spherical indenter and the parameters for fused silica left and the difference in the calculation with ideal tip and actual area function of a Berkovich indenter right If spherical indenters are used small jumps in the curve may occur with certain parameter combinations as not all combinations produce reasonable values Additionally no choice is permitted with pressure distribution Power function is always used Nevertheless really good simulation of the elastic plastic transition is possible even with spherical indenters The radius of the sphere can be varied in the Radius field The value from configuration is used there as default 119 asmec ADVANCED SURFACE MECHANICS 7 3 Modulus converter The Modulus Converter is used to convert elastic constants and is accessed
106. e window Data is saved as DAT file when the window Measurement data is active Data is saved as a DAA file when the DATA overview window is active Data is saved as a AVR file when the Results window is active Select the folder and file name by clicking on the icons and input lines in the File Selection dialog The folder will remain as the default path for saving until you select a different path or close the program Data can also be saved in other formats via the menu item File in the top menu bar Here several data files can be saved at once Batch Export in text format Excel format or the special fdop format for the supplementary software FilmDoctor ASMEC GmbH InspectorX Version 3 0 6 Demor Information Setup Calibration Configuratio Open Data File Save Data The data always contain time force and displacement for the Special file actions normal and lateral if present measuring heads In the case of Open AVR files for area function measurements using precision stages the stage co ordinates Batch export to EXCEL XLS are also included Batch export to ASCI TAT Batch export to FilmDoctor SIO format Open Template File Save Template File Print Printer Setup a Fig 4 Export functions in the file menu it Pit Print The button prints the status window as text if it is the active window Otherwise the complete active window is printed including graphs buttons input lines and result fields The printer di
107. easurements with spheres kg Yield strength determination by cyclic measurements with spheres for UNAT and UMIS 2000 E Stress strain measurements with spheres NN J NN Neural Network module requires purchase of a separate module Fatigue test with spheres normal direction E Only UNAT yy Loading mode Normal lateral indentation ear Fatigue test with spheres lateral direction Only UNAT Aw Friction test normal lateral force Only UNAT 10 asmec ADVANCED SURFACE MECHANICS Oscillatory wear test Only UNAT Scratch test Only UNAT Oscillatory scratch test in Y direction H E Only UNAT ES Loading mode Tensile test Tensile test normal force only Only UNAT Tensile test with additional lateral force male Only UNAT 3 The Main Menu The main menu for Inspector X consists of a menu bar with buttons which will be explained in the following AECI W a il g X Coo w S nae Save Print Information Analysis Configur Open CFG Results Repot Stress strain Compare Graph Open T Save T Fig 3 Menu bar for data analysis in main window 3 1 The menu bar for data analysis Oper Open Open one or more files containing test data The file extension depends on the device selected in the configuration The default file extension for ASMEC devices is DAT Other file types are also available and can be selected via a drop down menu ASMEC UNAT Data File DAT
108. ed at Stored at the date on which the stiffness function was determined is automatically saved and shown in this field Obtained from enter here which reference material was used to define the stiffness function or from which external source the function originates Comment enter any remarks concerning the stiffness function Function between upper and lower force limit Data table Fit function no 5 Y Lower force limit mah 0 001 Edit Upper force limit ret 2038 1 Coefficients s7179 5939 159 174 2888 2 27 2 156 51 W 0 3929867 Fig 11 Fit parameters of the function for instrument stiffness Function between upper and lower force limit All values shown here are determined in the Calibration gt Area function and instrument stiffness menu and automatically transferred Fit function no number of the fit function This number is selected during calibration and cannot be changed here The link between the number and the corresponding function is given in the Help menu and chapter 8 4 The button 2J next to the fit function number opens the Fit Data window in which the function is displayed graphically see chapter 7 4 Lower force limit mN lower force limit for the instrument stiffness function Below this force value constant stiffness is assumed The lower limit is determined during calibration but can be changed here 20 asmec ADVANCED SURFACE MECHANICS OERE oa Upper force limit
109. eing used Read data E modulus Poissonr Calculation of the area function can now be started by pressing Sample 1 7200 017 Area calculation sample 2 410 0 234 Indenter 1140 0 07 Additional functions N l l mpo ou lt lt Additional settings are possible for special investigations these are accessible via the lt lt more button This will usually not be necessary f 4 fitfunction C Spline function C 2 fit functions Fit method i P m j Radial displacement correction bs ae bate Spline function Variable epsilon factor DSS Beta factor I a There is a choice of three methods for describing the area f Stiffness function from configuration function f Const stiffness mN um 0 2 Allow negative compliance e one fit function e two fit functions External area function from text file e use of a spline function not available in this version AFMfunction par Smooth area function 1 N FAY 2 fN Fig 103 Panel with additional functions for the calculation of the area function 99 asmec ADVANCED SURFACE MECHANICS The use of one function is standard Using two functions allows somewhat more accurate description of data in the area of very small indentation depths where curves are more bowed However this method should only be employed when at least 10 or more different loads were used to create the area function Radial displacement correction This correction which exceeds the
110. en trained like in the scheme in the figure above One neural network each is responsible for determination of zero point Young s modulus speed dependent overstress hardening behavior The neural network optionally enables the determination of the kinematic hardening of the material as a part of the hardening behavior from a unloading reloading hysteresis at the end of the measurement This is of significance for the analysis of the cyclic deformation behavior of the metal Various solution methods are available to the user within the module 1 With the classical neural network approach complicated non linear relationships are solved very rapidly through an approximation of the inverse relationship 2 With a probabilistic neural network an estimate of the uncertainty in the form of confidence intervals is also supplied Unlike classical networks these networks require no verification examples during learning A With the Gauss approximation the distribution of the results is approximated with a Gauss distribution in each local optimum and the solutions are then averaged B The Markov chain Monte Carlo calculation provides the correct random samples from the distribution of the solutions thereby characterizing the distributions more accurately Both probabilistic methods supply by a weighted average of the stress strain curve an error for the neural curve determination upper and lower 90 confidence interval The evaluation
111. enu Insert the command line NPKB in front of the Output commands for the measurement data A number of ASCII data files are supplied with the program in the Example directory If you have problems importing data check the structure of the data file with an ASCII editor and try to reproduce the same file structure with your report An example follows The row Nullpunktbestimmung is followed by data from below 0 4mN The Loading segment follows after the words _ Krafterhohung This expression is used for identification of the Loading segment Caution If the Fischerscope software uses a different language data import will not work In this case please contact your supplier and send one of your ASCII data files Applikation Kalibration 300 Datum 06 03 2002 Uhrzeit 18 56 Messung Datum 06 03 2002 Uhrzeit 12 18 Laufende Nr 46 Kommentar FS 30mN 1 Indentor 1V14 02 02 letzte Formkorrektur am 14 02 2002 um 17 45 Uhr letzte H rtekorrektur am 19 02 2002 um 14 01 Uhr Nullpunktbestimmung Nr Kraft Tiefe Zeit 1 0 020 0 000 8 5 2 0 041 0 001 8 0 3 0 061 0 002 fs5 4 0 081 0 002 7 0 5 0 102 0 004 6 5 6 0 122 0 003 6 0 134 asmec ADVANCED SURFACE MECHANICS 7 0 142 0 005 545 8 0 163 0 004 5 0 9 0 183 0 005 4 5 10 0 203 0 005 4 0 11 0 224 0 007 3 5 12 0 244 0 007 3 0 13 0 264 0 007 2 5 14 0 285 0 008 2 0 15 0 305 0 009 1 5 16 0 325 0 009 1 0 17 0 346 0 010 0 5 18 0 366 0 010 0 0 Krafterh
112. erman The illustrations were produced using an IndentAnalyser Version 3 0 4 or higher Later versions may display differences from these illustrations but these will have no effect on general operation Where there are several input fields in one window values will usually be applied when the Tab key is pressed The Enter key can only be used in a few selected instances The software is suitable for the analysis of depth sensing indentation measurements from a large number of different instruments and from the macro to the nano range according to the international standard ISO 14577 With an additional module stress strain curves of metals can be obtained from indentation measurements with spherical indenters and by using neural networks For some instruments also dynamic tests QCSM and CSM module can be analyzed Additional al test methods can be analyzed which can be carried out by ASMEC instruments especially such which use a Lateral Force Unit as second measuring head This concerns for instance scratch tests oscillatory wear tests or Surface scans 2 Program Startup and first steps 2 1 Starting the program as a trial version After the installation the program will start as a trial version which only permits opening of previously analyzed data files in the program s native format DAA and AVR files The original data files for the measuring devices usually DAT files cannot be opened This is indicated by the words Trial Version in
113. erred to the layer fields Adjust the Young s modulus and Poisson s ratio values for the layers and the substrate to the correct values for the sample The layer with the highest number is always the uppermost layer Enter the thickness values in the appropriate fields Please note The fit result can only be as accurate as the defined thickness and modulus values The thickness should therefore be determined as accurately as possible The Young s modulus for the substrate can be measured using the same method if it is not known Fit parameter select the required result type Young s modulus gives the elasticity modulus for the uppermost layer or the substrate if no layers are present Sohere radius allows a fit for the indenter tip radius if the elastic parameters are known Nominal tip radius the radius of the indenter is required for fitting the Young s modulus The value from the configuration is entered in this field and can be changed here Use radius function this checkbox is only available if an effective radius function is used in configuration instead of an area function An effective radius function can improve fit accuracy especially when the tip radius varies by more than 5 in the indentation depth range of the measurement Points for calculation select the first and last data points of the chosen curve for calculation Period if a large number of data points are present 50 or more it is better not to use all of them but t
114. esseccceesececeeeceeeeueecesauseeessugeceesenes 47 4 3 Zero point correctiOn s ssssessesseessesseseeseesorseeroeroerosroeressessessesrosresrosresresrrorsortorssrseaseaseeseeseeseesees 51 Mies CONE E AENA O a E 52 4S Averaging measured CUTVE S encar 54 PAY 1S Te Daia A T 57 5 1 Evaluating hardness and Young s modulus MEASUFEMENKS ccccceeeeeeeeeseceeeeseees 57 5 1 1 L ad displacemeMm PIBE errean EEE 57 5 1 2 Creen PIE E aa E E den E E EEE 60 5 1 3 TADE eee eee ee eer errr 61 5 1 4 Time dependence PAE cccccssscccssecccsecccneceescceescecascecsececeneceeeeesssceesuscesenecessueeeneneetes 62 5 15 APPO 812 1 eee ee ee Oe E E ee ee eee eee 62 5 1 6 PED 21 gt ae ee eee ee eee ee te eee eer eet 63 Sle Resultsover depth page gene ne eno eo Br tne nO nen ee ese ee ee 64 5 1 8 VIET OND O N ee ere 65 5 1 9 Extrapolation of the indentation modulus to zero indentation depth cccccceeeeeeeees 66 5 1 10 Determining a hardness ratio or difference to a reference measurement esccrne 68 AB o 5 2 Evaluation of variable load displacement measurements ccesccessssesssccessecessseeeasesenees 70 5 3 Evaluation of cyclic hardness measurements cccccceesecceeessececeesececeeeecceeeuseceeeeaeceeseees 71 Wik 5 4 Evaluation of CSM QCSM measurements ccccccccccccccccccccccececcccccececccececceceececeeeceeeeees 73 5 5 Elastic Young s modulus measurements with spherical indenters
115. esses In the event that the force during the hold period is not at least 10 lower than the preceding maximum force the hold period for correction of thermal drift will not be accepted It is also possible to use and analyze several hold periods during a measurement 52 asmec ADVANCED SURFACE MECHANICS A hold period at maximum force is always associated with creep plastic flow if plastic deformation occurs and should only be used for correcting thermal drift if the measurement was completely elastic The use of a creep segment for correction of thermal drift in the Configuration window is permissible If manual correction has been selected the Thermal drift correction window will open when the Analyse button or the Start correction button is pressed The window is not visible if automatic correction is selected The displacement data over the time within the hold period plus a linear fit are shown in the Thermal drift correction window The linear fit is used to determine the drift rate in nm s The start of the linear fit range is defined as a percentage of the maximum hold time The fit range always ends at the maximum time tmax of the hold period It is advisable to begin at 25 or more of tma to rule out relaxation effects of the materials and to use hold periods of 60 seconds or more Thermal drift correction for QuarzfrB2_B2_0009 DAT feel Fit start oftime 25 Drift at 9 98mN Fit end of time 100
116. etween the force and displacement signals is then determined by subtraction of the two phase signals The Contact stiffness is calculated from the quotients of the vibration amplitudes of the force and displacement signals under consideration of corrections with regard to the mass of the moving parts of the measuring head and to frequency dependent damping 74 asmec ADVANCED SURFACE MECHANICS Average results La taz QuarzfrB2_B2_100mN AVR Cycle 1 Normal vibration 5 Segment 3 Load Frequency 8 49 Hz Smoothing Amplitude 0 180 V o Segment 4 Creep Frequency 8 49 Hz Amplitude 0 180 V O pe Reset i rid V Marks E D Fit marks 2 a z Z 5 d G 5 k Show Amplitude Phase Force amplitude C Stiffness Phase difference Displacement amplitude Force phase Show Displacement phase IV Force amplitude V Displacement amplitude IV Force phase WV Displacement phase 0 10 0 20 0 30 0 40 0 50 0 60 0 70 0 80 0 90 i Z Normal Displacement um Vv Load Displacement Creep T Drift Time dependence Approach Special Results overDepth yibration Fig 76 Phase shift and amplitudes of force and displacement signals during QCSM measurements on the Vibration page of the Average results window icia re 260 Quareft82_B2_0002 DAT Cycle Normal vibration 1 E 240 Segment 3 Load Stiffness Frequency 8 49 Hz Smoothing Phase difference Am
117. evaluation DAT files are not suitable for this 6 1 3 Third step creating an AREA file In this step the recently produced AVR file is used to create a so called AREA file which is then used in the final calculation of the area function The AREA file is a text file which is used to calculate the area function It can be opened with the text editor and has the following structure Fmax hmax ho S m 0 51661 0 038271 0 009040 16 91126 1 5000 e Fmax maximum force where a stiffness value is available e hmax maximum indentation depth e h0 depth after unloading e S contact stiffness e m exponent of the unloading curve The menu item File gt Open AVR files for area function is used to create the AREA file All AVR files associated with measurements of a reference material should be opened together Since IndentAnalyser Version 3 0 7 it has been possible to import multiple QCSM measurements or measurements with QCSM module and fast hardness measurements together and create a single AREA file from them The AREA file must then be named in the Save dialog The suggested name is Areafunction_sample name AREA We recommend using the designation of the reference material and the number of the indenter e g Areafunction_Quarz_B1 AREA Note for creating the AREA file all results in the Results table will be deleted The procedure described for determination of the area function should now be carried out for sapphire as well 6 1 4
118. fault is Points from 1 to maximum number of points Caution To calculate the area function four artificial points are added below the lowest measuring point lowest force or indentation depth and a spherical indenter tip is assumed in this depth range These points are used to guide the fit function in the area of very small indentation depths and improve accuracy The number of points is therefore greater by four than the initial number in the AREA file 102 asmec ADVANCED SURFACE MECHANICS 0 504 0 404 T 0 30 2 0 20 5 O WY 0 10 e Data from sample 1 A Data from sample 2 ldeal Tip Fit average 0 000 0 020 0 040 0 060 0 080 he um Fig 105 Begin of the area function with the results for fused silica and sapphire Artificial points are located below 0 20nm The match between the two materials is very good The result should now be saved in a new Configuration file CFG via the Save configuration button Caution The area function must not be saved until a correct stiffness function has first been saved If this is not the case calculation of the area function may have to be repeated C Calculation of instrument stiffness The instrument stiffness function considers the contribution of instrument components such as frame stage system sample fixing holder or indenter holder to the measurable displacement The instrument contribution must be subtracted from the absolute displaceme
119. file will be used The file name is displayed on the Main page of the Configuration window and in the status bar of the main window The configuration data are saved in CFG configuration files See also section 3 3 Oren CFG Open CFG Open a configuration file Configuration data are stored in configuration files with the extension CFG The file used after the program has started is indicated on the Main page of the Configuration window and in the status bar of the main window For various instruments and indenter tips example files are delivered together with the program A configuration file contains the parameters which are available in the Configuration menu The file contains units instrument parameters instrument type indenter type area function instrument stiffness values and much more A separate CFG file should be created for each device each indenter tip and each new area function The default storage path for the configuration files is CFG Files As many configuration files as required can be stored under any name It is recommended that a short informative name is used e g B1_2013 11 01 with the code for the indenter number and the creation date Results Results Open the Results summary window The program permits analysis of a large number of measurements at the same time The results accumulate in the Results Summary table until the table is cleared Details on using the results table can be found in Section 3 7
120. fined by double clicking on a point on the curve They are indicated by green points Switching is done via Normal Force mN 1 000 1 200 1 400 1 600 0 Define by double click Leftend C Right end Data Fit 2 00 1 75 1 50 1 25 1 00 0 75 0 50 0 25 0 00 Normal Displacement um Fig 120 Tensile test curve from a solid sample with a linear fit over the right half of the curve The standard setting for a linear fit is used The results are shown in the information field at top right const 6 191801546 X 769 4111199 mN um The value x for the linear term gives the instrument stiffness in mN m 116 asmec ADVANCED SURFACE MECHANICS The value so obtained can now be entered in the Configuration window and saved Configuration Pe Main Hardware Instrument Indenter Analysis normal Analysis lateral Results Calibration Other Instrument ASMEC UMAT Instrument no O4080002F The instrument and software version is connected with the raw data format Orly data files belonging to the chosen instrument can be read To any Instrument belongs additionally a unique instrument stifness function normal and lateral Data file extension DAT Second extension Instrument stiffness function Normal direction Lateral direction no Function type Average instrument stiffness in normal direction mH pm Fr O Sthinees iuetion Compliance function Stiffness descri
121. first few data points up to a depth of around 30nm should be used Linear linear force displacement dependency e g in flexure experiments with beams Quadratic quadratic force displacement dependency e g for measurements with high contact force and pyramidal indenters or cones This should be the default method for high load experiments in the many Newton range Thermal drift correction E re Manual the measuring points of a hold period after unloading are displayed in Manual the Thermal drift correction window You can select which range of measured Automatic values is to be used for correction This is normally the most accurate method None Automatic The Thermal drift correction window is not shown and there is no opportunity for intervention None no drift correction is carried out Selecting options for correction of thermal drift C Use average drift rate from measurements Use average drift rate from measurements uses a drift rate Allow hold period use at Fmax averaged from several measurements which have been analyzed Use average drift rate from hold periods before Allow hold period use at Fmax allows use of a creep segment i e a hold period at maximum force Fmax to determine thermal drift Material creep normally prevents accurate calculation of a drift rate In purely elastic measurements there is no creep A creep segment of this type can then also be used for correction of thermal drift Use a
122. h range below 5um always an area function should be used Every pyramidal or conical indenter has an approximately spherical end with a radius between about 50nm and ium depending on quality and wear status The area function should be determined as accurate as possible since it will influence all subsequent analyses of hardness and modulus The most difficult calibration is the calibration of the instrument stiffness especially when the stiffness is not fully constant with force Please find more information in chapter 6 For flat punch indenters or other indenters where no quantitative analysis especially of hardness and modulus shall be done there is no calibration necessary For these indenters an instrument stiffness can be used which was determined with a sharp or a spherical indenter For fully elastic measurements with spherical indenters the calibration is more easy and only measurements with one force are necessary see chapter 6 2 2 2 6 Results summary The software allows the analysis of a large number of measurements at once All results which have been obtained during one session of the program will be collected in a table The table can be opened using the Rests Results button For details of the presentation of results see chapter 3 7 and 3 8 2 2 7 Pre defined applications For data from ASMEC instruments the type of the analysis is connected to an application type which was chosen during programming of the measureme
123. he Modulus Converter window 7 4 Fit Data window The Fit Data window is a powerful tool for fitting many different sorts of data and displaying the originals with the fitted curve It is opened via Tools gt Fit data window It also opens if a curve is copied from the Comparison window by clicking the Fit Ee button If the window is opened without a curve being copied it will initially be empty Data can be imported via the Read TXT button Only text files can be imported and these must exist either in the IndentAnalyser export format for text files or in the old IndentAnalyser GRA format Otherwise any text files can be imported if their format is known The data must be saved in columns with any desired number of columns of equal length Number of headers or footers can be ignored The 120 asmec ADVANCED SURFACE MECHANICS amp button opens the ASCII import configuration window with which the format and the file extension can be specified ASCI import configuration Line number of header top of file 2 to exclude from reading Line number of footer end of file io to exclude fram reading Column delimiter Tabulator Hhersig E Data file extension TXT OK Fig 127 Window for specifying the import format for text files If there are more than 2 columns in the file the columns for displaying the X and Y values can be selected in the X column and Y column pull down menus As default Column 1 is used fo
124. he sphere from the sample Displacement control during unloading was carried out up to 50nm Signals over time 45 Av Force mN x1 40 Displacement um x544 11 35 Signal a u gt A 8 ab on 10 0 5 10 15 20 25 30 35 40 45 Time s Fig 71 Force and displacement signals for an adhesion measurement on Si over time The moment at which the sphere is snatched away detached from the surface can be identified in the displacement time signal by the negative peak at about 30s The force at this moment is 0 5mN corresponding to the adhesive force Displacement control then causes a movement back to the required position for this time Mult 5 3 Evaluation of cyclic hardness measurements The evaluation is performed in the Average results window like for any other type of hardness measurement The only difference is that the loading unloading cycle for the evaluation can be selected in the Cycle field at top right Fitting the unloading curve can then be performed for the corresponding cycle The red fit curve and the tangents are calculated for the local maximum and displayed The example in Fig 72 shows data for cyclic measurements with 10 cycles on fused silica Cycle 8 of 10 was selected for evaluation and the results for this cycle are shown in the information field on the right hand side of the window Additionally hardness or Young s modulus for each cycle over indentation depth are shown on the
125. hold periods of a cyclic measurement on fused silica 5 4 Evaluation of CSM QCSM measurements The Quasi continuous Stiffness Measurement method is a module developed by ASMEC to enable the contact stiffness of the sample to be determined not only by using the unloading curve at a single depth but for many points during the indentation process This allows a depth dependent determination of hardness and Young s modulus at one and the same sample location In addition the measurement sensitivity at low forces is increased enabling stiffness values to be determined for very low forces and indentation depths With the QCSM module the load increase is paused for a short time typically 3 seconds and a sinusoidal vibration is superimposed on the piezo voltage In contrast to other methods the amplitude for force or displacement is not specified directly Amplitude and vibration phase are determined using a lock in filter Stiffness is calculated from the quotient of force amplitude and displacement amplitude This is equivalent to determining contact stiffness by adjusting the unloading curve and using the gradient at maximum force as the stiffness result of AF dh Ah The high contact stiffness gradient of the unloading curve often causes a very small displacement signal of the vibration even with greater piezo deflection The greater part of the piezo displacement is required for displacement of the springs for the force measurement The piez
126. ideal spherical form on the load indentation curves and calculates the curves accordingly The functions of this network is not fully reliable Consider kinematic hardening a neural network performs evaluations according to the kinematic hardening model The relevant information is obtained from the hysteresis of the loading and unloading curves at the end of the measurement This option is always recommended to use Calculation method The calculation is performed with the classical Gauss or Markov model as explained above The classical NN calculation is quickest lt 1s but does not calculate error curves for the stress strain curve The two other methods supply the correct 90 confidence interval but in some cases take more than 60 seconds for the calculation The individual steps of 3 729 can be tracked and the calculation can be interrupted at any time After an interruption the most recently calculated stress strain curve will be displayed At the end of the calculation the stress strain curves obtained will be displayed in the graphic The input and output data with reference to the training intervals are only shown for the classical calculation method in an interval from O to 1 at bottom left below the graph in Fig 86 with red interval boundaries This can also be used as an accuracy criterion for the calculation If all points lie between zero and one the networks are being used within their training range If several points l
127. idual roughness peaks initially undergo plastic deformation which would violate the model The calculation is performed in a very similar way to that for plastic deformations The sole difference is that only measurements with one force are required as the contact stiffness can be calculated for each loading point provided loading and unloading curves match Preliminary tests are used to determine in which force range purely elastic measurements are possible With a 10um indenter for example 7OMN is generally used for fused silica and 100mN for sapphire The first step measurement of the reference material and the second step evaluation of raw data are the same as for plastic deformation except that only one AVR file for a maximum force must be generated not for many forces The third step creating an AREA file is not necessary When a new spherical indenter is calibrated for the first time the following must first be done e Open the Configuration window and go to the Indenter page e Select Sphere in the Indenter type field and enter a number in the Indenter no field The following must also be entered descriptions for the ndenter material values for the Young s modulus GPa and Poisson s ratio of the indenter and the nominal tip radius Tip radius e Press Save to save the entries in a new Configuration file which should be named in accordance with the indenter number and the saving date Calibration takes place via
128. ie outside this range this indicates insufficient adaptation by the network The Rp 0 2 straight line can be shown in the stress strain curves by checking the appropriate box straight line parallel to the elastic range and at 0 2 strain on the strain axis The shape corrected and uncorrected force indentation depth curves can be saved in the data directory as ASCII files gcr and ucr again by checking the appropriate box The material parameters which have been determined are listed in full with units in a text field at RTA bottom right They can be copied to the clipboard e g via Ctrl C or saved as an RTF file using the button All curves in the top graph can as usual be printed out copied to the Comparison window or exported as text files With the Show radio buttons the type of curve shown can be selected AFTER calculation e True stress strain true stress strain curve e Technical stress strain technical stress strain curve e Plastic stress strain plastic portion of the stress strain curve e Kinematic stress strain portion of the curve resulting from kinematic hardening e Original and corrected measurement shows the original and zero point corrected curve with its supporting points for the calculation e input data overtime shows the measurement data over time 86 Result for Messing2 TRA asmec ADVANCED SURFACE MECHANICS Result for Messing2 TRA 300 250 T 250 200 5 N
129. ill allows you do to decide later to evaluate all measurements individually rather than averaging them Allow average of data from different samples Sometimes measurements are repeated and you forget to set the correct sample designation By default such measurements are not accepted as the same Checking this field allows data files in which different sample designations are stored to be averaged also Allow average of data from different indenters The same thing can happen with the indenter designation If you forget to import the correct configuration file before measurement an incorrect value will be saved in the data file and averaging of measurements for which a different indenter is registered will be rejected This can be prevented by checking this field Tolerance limits for averaging The lower part of the window contains criteria for which measurements will be accepted as equal The 56 asmec ADVANCED SURFACE MECHANICS relative limits in for force the number of the point in a segment and the measuring time of a segment will be checked It should be noted that the limits for each segment must be observed If for example a creep time only lasts 2 seconds a time of 2 22 seconds would already be 10 outside the limit The limits are especially significant when averaging measurements in open loop mode as all segments normally have a better than 1 match in closed loop mode Add files allows extra data files to be added
130. indenter BS4reatunction BS 22 05 200850uarz 65 0009 DAT H SMessdaterS UNAT Datensindenter bSAreafunction BS 22 05 2008 Quaere_BS 0010 04T H SMessdatenS ONAT Datensindenter BSAreatunction BS 22 05 2008 Quarz_B5 0011 04T H MesedatenSU NAT Datensindenter BS4reafunction BS 22 05 200850uarz BS 0012 DAT H MessdatenS UNAT Datensindenter B S4reatunction BS 22 05 200850uarz B5 0013 04T H MesedatensSUNaAT Datensindenter BS4Areafunction BS 22 05 2008 Quare_BS 0014 04T H SMessdatenS ONAT D atenslndenter B S4reatunction BS 22 05 200850uarz B5 0015 04T H MessdatensUMAT Daten lndenter bo areatunction BS 22 05 2005 Quere B5 0016 04T H MessdatenS UNAT Datensindenter B SAreatunction BS 22 05 2008 Quare_BS 0017 DAT H SMessdatenS UNAT Datensindenter bS4reafunction BS 22 05 2008 Quarz_B5 0018 0A4T H SMessdatenS ONAT D atenslndenter B S4reatunction BS 22 05 200850uarz B5 0019 DAT H MessdatenS UNAT Datensindenter BSAreatunction BS 22 05 200850uarz BS _0020 0AT H MessdatenS UNAT D atensindenter E S4reatunction BS 22 05 200850uarz B5_0021 0AT H SMessdatenS ONAT Daten indenter BSAreatunction BS 22 05 20080uarz B5 0022 DAT H SMessdatenS ONAT D atenslndenter B S4reatunction BS 22 05 200850uarz B5 0023 04T H MessdatenSU NAT Datensindenter bSAreafunction BS 22 05 200850uarz BS 0024 DAT H MessdatenS UNAT Datensindenter BS4Areatunction BS 22 05 2008 Quare_BS 0025 04T H MesedatenSUNAT Daten lndenter BS44reatunction B5 22 05 2008 Quare B5 0026
131. ined The area function for the stiffer material with the greater Young s modulus reacts much more strongly to changes in instrument stiffness than the material with the lower Young s modulus so that the two functions overlap at certain stiffness This may be load dependent with the result that instead of a constant stiffness value the end product is a stiffness function which depends on the load At low loads under 50mN this calculation is generally quite inaccurate so points below this load should be omitted for the stiffness function To start the calculation press the Stiffness calculation button The view in the graphic will change to Instrument stiffness function 104 asmec ADVANCED SURFACE MECHANICS E Instrument stiffness function coe emcee Read data E modulus Poisson r S Sample 1 715 O17 Sample 2 410 0 234 Indenter 1140 0 07 7 000 lt lt more 6 000 Fit function 5 sI Ed Pointstrom b to 25 2 E 5 000 Fit type f Function Constant value E Presentation Y 4 000 Stiffness C Compliance 3 000 Tip radius upper limit um 0 197 2 000 Average stiffness mN ym 3694 8 1 000 Instrument stiffness M Stiffness iv Fit Fit Area calculation Stiffness calcul 0 10 20 30 40 50 60 70 80 90 100 Save in CFG file Force mN we N mN HS oe Fig 106 The Indenter stiffness function window after calculation of the instrument stiffness function In an ideal case the s
132. ire The blue line represents the shape of an ideal sphere with the nominal radius defined in configuration The points represent the calculated area values for the measurement data while the line drawn through them represents the fit function By default the data for both materials are used for the fit Save area function Average Estimated tip radius From the fit curves an averaged indenter radius is calculated shown here in microns It may differ considerably from the nominal radius as only the first 150nm 300nm of the indentation depth is considered here while the manufacturer determines the radius over a depth range of 10 20 of the radius 109 asmec ADVANCED SURFACE MECHANICS ee i All other fields and the additional subwindow accessed via the mare button have the same functions as described in Section 6 C Calculation of instrument stiffness Click on Stiffness calculation to start the instrument stiffness calculation This again involves an iterative process which may take some time The view in the graphic will change to Instrument stiffness function As pile up and sink in effects are not relevant to purely elastic measurements a highly constant instrument stiffness is usually recorded The Average stiffness field shows the average stiffness over all points of the stiffness range following the calculation All fields have the same functions as described in Section 6 To save the result of the stiffness calc
133. is If no QCSM results are available use estimated indentation hardness or Martens hardness 3 Press Read reference and read the AVR file with which you want to compare the hardness e g a pure substrate or another layer The hardness curve for the second sample is also shown although without error bars error bars are only available here with QCSM measurements Then click on Results ratio and the depth dependent hardness ratio between Specimen 1 and Specimen 2 the reference sample will be shown When both files are the same a horizontal straight line with the value 1 would be shown 68 ADVANCED SURFACE MECHANICS E Average results koekoea 12 06 01_B14_100mN 1 4VR Cycle Parameter for X axis 1 x Smoothing Parameter for Y axis 0 V Adaptation to unloading modulu Read Reference Clear Ref Reset MI 2 07 02_B14_100mN 1 AVR Show WV Marks Fit marks Both results C Results ratio C Results difference a ki Indentation hardness GPa Add results to table V Show parameter graph 0 00 0 10 0 20 0 30 0 40 0 50 0 60 0 70 0 80 V Show reference values Contact depth um Show error bars Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 67 The Average results window with the hardness depth curves for two samples ai deere results a 12 06 01_B14_100mN 1 4VR Cycle Parameter for X axis 1 Zz 0 80 Co
134. is that the contact pressure corresponds to a Hertz contact Comparisons with finite element calculations have shown that this assumption is correct provided the modulus difference between layer and substrate is not greater than 1 4 to 1 8 depending on the ratio of the layer thickness to the contact radius The method can only provide accurate results if this condition is satisfied The method is available for up to three layers on one substrate Only the modulus of the uppermost layer can be fitted The elastic properties Young s modulus and Poisson s ratio of the other materials must be known The calculation time and computer memory requirement increase markedly with the number of layers Ei Elastic fit of load displacement curve E Se Young s Modulus GPa Poisson s R i Fit parameter pienes sete Nominal tip radius um pe Nolayer Substrate 71 876 0 47 Thickness um s304 Youngs modulus C4 layer i eooo 1 oT oO C Sphere radius C Qlayers i veri a i a ia 32 nea Tae Fit of gt C Loading curve ik 3 layers OT oS OS g C Unloading curve f Average of both Elastic fit of load displacement curve Points for calculation First 1 Last 63 aj Period al Results E Mlod Delta Show With maks M Measurement 7 Iw Fit E I Show title 0 00 0 10 0 20 0 30 0 40 a ie Displacement um Calculation Close Fig 79 The window for fitting elastic measured curves with spherical indenters
135. is the average angle between Projected area of contact for the distance h from the tip without Consideration of the Radial Displacement Correction Ac is obtained from the stored area function of the installed indenter for the depth hc Ac does not consider pile up or sink in effects Projected area of contact for the distance h from the tip with Consideration of the Radial Displacement Correction Ac is somewhat smaller than Ap because the elastic radial deformation is directed towards the center of the indent Ac is obtained from the stored area function of the installed indenter for the depth hc Effective depth dependent radius at a certain depth h for spherical indenters 126 asmec ADVANCED SURFACE MECHANICS Creep rate at the beginning of the creep curve after reaching maximum force Creep rate at the beginning of the creep curve before unloading Coefficient 1 of the fit of the creep curve with a logarithmic function Ah C In C t 1 t creep time Coefficient 2 of the fit of the creep curve with a logarithmic function Rul Rc Ratio of unloading rate at the beginning of unloading and creep rate at the end of the creep segment This ratio is used for the validation if creep may have an influence on the stiffness calculation The ratio should be larger than 10 8 2 Explanation of scratch tests results The following roughness parameters are obtained from a first surface scan with low contact force before a sc
136. it is used for calculation of the area function For spherical indenters it is used to determine the transition depth from sphere to cone Comment remarks on indenter properties and or determination of them can be entered in this field During the calibration procedure the data file with which the values were calculated is noted here Indenter area function Use area or radius function the area or radius function is only used if this box is checked Otherwise an ideal form is assumed Use area function for Martens hardness If the box is checked the same area function is used for calculation of Martens hardness as for indentation hardness Martens hardness is often calculated with no area correction this results in an apparent increase in hardness at the surface Validity range this field defines the validity range of an area or radius function from start date to end date The range of validity is determined automatically during calibration begins a few days before calibration and ends one year after calibration The validity range can be changed During calculation of hardness or elasticity modulus a warning message will be displayed if measurements with a measuring date outside the validity range of the area function are being analyzed Stored at the date of the area function calibration is automatically saved and cannot be changed Validity range from 23 11 2013 To 30 11 2014 Stored at 01 12 203 Correction type states with which
137. l drift Creep means the change in depth over time when force is maintained constant and a new maximum was reached immediately beforehand The curve is fitted using two different functions Logarithmic Function Ah A In B t 1 t time 1 2 1 4 1 8 t t t Polynomial function Ah c t c C C Function 1 is used to calculate the recommended hold period Function 2 has more parameters and can therefore follow the data better It is used to calculate the creep rate at the end of the measurement QuarzfrB2 B2 0009 DAT Creep time 20 0 3 F at t 0 99 826 mN h at t 0 0 954 um CIT 0 44 Creep curves Reset iV Marks I Fit marks Depth Change nm D lp Smoothing range for rate calculation points left right x Creep C Creep rate Depth C Creep rate V Show logarithmic fit 0 2 4 6 8 10 12 14 16 18 20 Time s Load Displacement Creep Time dependence Approach Special Results over Depth Vibration Fig 55 The Creep page of the Average result windows There is a choice of three different types of diagram 60 asmec ADVANCED SURFACE MECHANICS creep shows the change in depth over time for constant force creep rate shows the creep rate over time creep rate depth shows the quotients from creep rate and indentation depth over time The result should be virtually load independent for homogeneous materials The results for the analysis of the creep
138. l increase in force over time If the measured exponent of the loading curve into a homogeneous sample is less than 1 96 2 0 this is due to insufficient or totally uncorrected instrument stiffness Metal hardness reference blocks are suitable as samples for high loads in the macro range The same requirements apply to reference samples as stated in 6 1 1 The following example was measured with a Zwick universal hardness measurement head in the Kilonewton range Calibration is performed via the Calibration menu gt Instrument stiffness from large indentations with with the Open button This file must be created beforehand by averaging several measurements to increase accuracy The window allows simultaneous evaluation of two measurements to enable better result comparison The Name of the imported file is shown in the field next to the Open button sg E Instrument stiffness function o Read data File 1 eS New Test Block 10HV_1125N AVR 1 100 000 File 2 No file init aii Desired exponent near 2 11 97 900 000 Mean compliance nm mN 0 000662 jv Allow negative compliance ane Fit function Aa EJ 700 000 Points from 1 to 42 imi Fit type 600 000 Function Constant value l Presentation 8 500 000 C Stiffness Compliance Save stiffness function e 4 a c 400 000 Show 300 000 Load Depth 1 Load Depth Loading exponent Inf Load Depth C 200 000 j Show point marks 400
139. le the position was held for 5 seconds after reaching the programmed maximum displacement and then unloaded for 5 seconds The wire was not disrupted during the test Unloading is purely elastic At the beginning of the measurement the wire is initially pulled straight so that the actual zero point is displaced If the cross sectional area of the wire is known and entered in the Sample cross section field the technical or true stress strain curve can be evaluated immediately The gage length Sample length is automatically determined and displayed using the approach position and Z stage co ordinates Automatic calculation of Young s modulus is currently not available in this software version but is planned Measurement data from Draht 400um Stage_0004 DAT cee cs 650 Sample length mm 8 554 Sample cross section mm 0 00125 600 Presentation C Load displacement curve C Technical stress strain curve True stress strain curve 200 150 100 True stress strain curve 50 0 0 000 0 005 0 010 0 015 0 020 0 025 0 030 0 035 0 040 0 045 Ee V Show legend Strain fc be Show marks Normal F h Curve Normal data over time Tensile test Approach Image Fig 101 True stress strain curve for the above test 96 asmec ADVANCED SURFACE MECHANICS 6 Determination of Area Function and Instrument Stiffness 6 1 Calculation from plastic indentations pointed indenters 6 1 1 First step me
140. lel to the blue line of the ideal area and lie slightly above it If the graph intersects the ideal area line or consistently diverges from it an incorrect instrument stiffness has very probably been used or the indenter is defect The red points indicate the measured values of fused silica and the green points those for sapphire The points are described with a fit function visible as a solid line 101 asmec ADVANCED SURFACE MECHANICS Save area function 7 d fi2 f Average oe S Save area function specifies whether the result for Material 1 2 or the average value of both is saved as the area function Default is the average value Average for the two materials provided two were imported as this is normally the most accurate Tip radius upper limit provides an estimated value for the upper limit of the tip radius It is determined using the two points closest to the zero point Through these a circle function is laid The closer these values lie to zero the more accurate is the estimated value In the example the first sapphire point is at 14 5nm The actual value of the tip radius can be slightly better than 0 2um but not worse If the first point is at too great a distance from the zero point e g 50nm or more the estimated value will always be significantly too high Area deviation at 500nm states the percentage deviation of the calculated contact area at a depth of 500nm from an ideal area without tip rounding Thi
141. les are available and have been purchased When the checkboxes are inactive they have not been purchased Available modules can be disabled by removing the check mark for instance if a used shall not consider them Configuration zl Main Modules Instrument lndenter Analysis normal Results Other Modules W Surface scan enabled W Elastic curve fit enabled if Tension mode enabled w LOCSM mode enabled W QCSM mode enabled i Oszillatory scratch test enabled if Scratch mode enabled i Materials Database enabled Ww Stress strain curve analysis NN Fig 9 The Modules page of the Configuration window Surface scan enabled enables the analysis if surface scans using the XY stages profilometer function only UNAT Tension mode enabled enables analysis of tensile tests to get stress strain curves only UNAT QCSM mode enabled enables analysis QCSM or CSM measurements Scratch mode enabled enables analysis scratch tests over longer distances using the X or Y stage only UNAT Stress strain curve analysis NN module for determining stress strain curves of metals using neural networks Elastic curve fit fit module for determining the Young s modulus of thin layers or substrates from purely elastic measurements LQCSM mode enabled enables analysis of dynamic measurements in lateral direction requires data from a Lateral Force Unit only UNAT Oscillatory scratch test
142. listed in the table for the results display Modify any changes of symbol icon digits and color for the current row of the table will not be applied until Modify has been clicked Basic units Length unt jum Force unit rN Hardness unit GPa Time unit E Basic units Length unit length unit options are mm um and nm Force unit force unit options are kN N mN UN kp p kgf gf and mgf Hardness unit hardness unit options are GPa MPa N mm2 kp mm7 and kgf mm Time unit time unit options are h min s and ms Selecting the results presentation Symbol Unit Digite Color Bold Description F rN f E Black E Maximum normal test force gt Up Down All equal All equal All equal This order defines the output order screen printer Symbol Unit Digits Color Bald Description Mo a F m 3 Black MoO Masmum normal test force E A row in the table becomes activated by a click into it The active row is indicated by a red dot The data for the selected row are shown in the fields above the table and can be changed there Symbol symbol of the test parameter Unit unit of test parameter Digits specifies the number of digits in which the test parameter is given in the selected unit Color selects the color in which the test parameter is to be shown Bold bold presentation of letters Description freely selectable description for the test parameter shown example Maximum
143. llow negative compliance The result of such a case is shown in Fig 117 14 0 Dat at 1 975 13 0 1 950 1 925 12 0 l In Load mN Loading exponent S l S oe N oa aia 1 8507 10 0 1 8254 40 50 60 70 80 90 100 3 0 l 4 0 Displacement um In Displacement um Fig 116 Logarithmic presentation left of the loading curve from Fig 115 and the local exponent of the curve as a function of the indentation depth right Only at depths larger than 30um it is above 1 9 lai pene stiffness function z Read data File 1 D New Test Block 10HV_1125N AVR File 2 bje oo 0 035 Desired exponent near 2 1 97 Instrument compliance 1 Fit 1 Mean compliance nm mN 10 000521 0 030 M Allow negative compliance Fit function 7 2 z TaS Pointsfrom 3 j to 42 i Fittype F 0 020 C Function Constant value Presentation S C Stiffness Compliance z 0 015 E Save stiffness function 5 C 0 010 Show Load Depth C Loading exponent C In Load Depth Instr compliance 0 005 V Show point marks gee Oe eve oe j Measurement 1 V Fit4 0 000 ETETE a SS E EEES h Fi Stiffness calcul 200 000 400 000 600 000 800 000 1 000 000 Save in CFG file Save in Database Force mN SS T Close Fig 117 The Instrument stiffness function window after calculation of instrument compliance and permitting of negative values It makes sense to fit with a constant v
144. lso the indenter type is saved together with an area function which describes the tip shape The indenter and its calibration will not be valid for your own data Therefore the first step is the calibration of area function and instrument stiffness to enable the software to calculate correct hardness and modulus values The configuration window is explained in chapter 3 3 2 2 2 Measurement of reference materials for calibration For an accurate data analysis the instrument stiffness function or a constant value and the area function of the tip have to be calibrated For this measurements on two well known reference materials with a large difference in modulus are necessary with a lot of different forces Fused silica or another glass is recommended for the calibration of the area function and sapphire single crystal or another homogeneous material with a high Young s modulus is recommended for the calibration of the instrument stiffness For the first reading of the calibration measurements the correction functions in the example CFG files can be used as start values The functions can later be changed The calibration procedure is described in chapter 6 2 2 3 Processing the raw data After reading the raw data form the reference materials several corrections have to be applied They are describes in chapter 4 This concerns always a zero point correction and if possible a thermal drift correction The corrections can be done manually or au
145. m the rows of the Results summary window is now displayed in the Comparison window 4 Press the Fit be button in the Comparison window The Fit Data window appears 5 Press the Calculation button in the Fit Data window A linear fit will be performed this corresponds to Fit function 1 which is preset 6 Now press the Extrapolation to X 0 button The linear fit will now be extrapolated to X 0 and the result for Young s modulus or hardness at zero indentation depth will be shown in the field to the right of the button see the red arrow in Fig 65 66 asmec ADVANCED SURFACE MECHANICS PEX Fit Data 93 6697 1 40505 t point number 1 Modify WV Show Data WV With marks WV Show Fit M With marks Show residuals V With marks Show range only Start at 0 0 Points for fit curve 100 From f 3 S point 1 xi point B Fit function 2 fi 3 ReadASCII cS Read PAR x column i No action gt Y column 2 No action l x factor fi Y factor 1 SAAAE fel Fit Data 93 6697 1 40505 At point number 1 Modify V Show Data WV With marks V Show Fit M With marks Show residuals With marks M Show range only Start at 0 0 Points for fit curve f 00 From g To point 1 X point 1 v Fit function Read ASCII amp Read PAR x column fi v No action v Y column 2 v No action v x factor 1 Y factor fi Fig 65 The fit curve after extrapolatio
146. mal Analysis lateral Results Other Special parameters for instrument ASMEC UNAT Mot used for this instrument Mot used for this instrument a Use special signs for results output Data import Maxinun point number for loading unloading segment i O00 Maximum point number for hold periods 500 Fig 22 The Other page of the Configuration window Use special signs for results output For non Latin char sets there may occur some formatting problems in the Average results window This can be seen with signs like u or 2 To prevent such format problems remove the check mark in this field 3 4 aly The Information window Each data file for ASMEC instruments contains in addition to the actual test data a large amount of metadata which can be shown in the Information window The Information window can be opened if a measurement has been performed a data file has been imported If several data files have been opened at the same time the window will receive the data from the most recently opened file The window is automatically updated as soon as a new file is imported The Instrument and Indenter pages correspond to the pages in the Configuration window with the exception that data can only be displayed and not changed see Sections 3 2 3 and 3 2 4 Main page This pages shows which instrument which hardware configuration which indenter and which software version were used for measurement It also contains all the sam
147. mately over each other at the start at minimum force When doing this it is a good idea to zoom the curve area out a little see Fig 92 in contrast to Fig 91 The drift rate in the example was 0 18 nm s i E Measurement data from Scratch_500mN_Silicium_D_510 6_0001 DAT 72 Max force mN 497 818 a Max distance pm 7 833 0 004 annaa nnd Af An 70 Roughness before scratch HO oaia a i tae rt pr and yn Rq um 0 003 v V 68 Rt pm 0 018 Rp pm 0 010 Rv pm 0 009 A An aN 66 Average friction 0 057 4 af Ah Z Maximum friction 0 155 L laf 0 10 eae T A 64 Z oe i ei Max displacement ENAN v Under load um 1 438 we i 623 Show on bottom axis Show on left axis x x A 2 D Distance Depth pan 60 the X pm 87 83 hm pm 0 434 Fn mN 147 150 Fl mN 3 144 0 20 u 0 021 od ii T Scratch depth 58 Seratch_500mN_Silicium_D Lateral force Scratch_500mN_Silicium_D Pre scan depth Scratch_500mN_Silicium_D Post scan depth Read background image Shift post scan distance um M Scratch depth Marks 5 um V Pre Scan Marks Subtract WV Post Scan Marks 0 30 l ejo Normal force Marks Estimated offset ym WV Lateral force M Marks y Marks Drift rate nm s 0 18 0 20 40 60 80 100 120 140 16 V Show legend V Show cursor Distance um Normal F h Curve Lateral F h Curve Normal data over time Lateral data over
148. methods have been used for a range of materials and verified with tensile tests For details of the evaluation methods we would refer you to 1 and for a detailed presentation of the experimental application to 2 1 E Tyulyukovskiy and N Huber Identification of viscoplastic material parameters from spherical indentation data Part I Neural networks J Mater Res 21 664 676 2006 2 D Kl tzer Ch Ullner E Tyulyukovskiy N Huber Identification of viscoplastic material parameters from spherical indentation data Part Il Experimental validation of the method J Mater Res 21 677 684 2006 The neural network module is called up via the Stress strain Ic button in the main menu This button is only enabled when the Average results window is open i e if already corrected and if necessary averaged test data are present The analysis includes instrument stiffness correction and optional zero point correction There is also a check whether the required measurement sequence with 3 shorter and one long hold periods has been implemented Without the correct loading sequence the use of the module for this data will be rejected 84 asmec ADVANCED SURFACE MECHANICS E Stress strain curve calculation with Neural Networks fs fon Result for Messing2 TRA CNCA a V Zero point correction M Shape correction V Consider kinematic hardening 300 Calculation method Stress strain curve without error 250 C Gauss Approxim
149. mi rive BOLA gt 4 if wt Fr yes bug A E ELE EE 17 Fig 21 The Results page of the Configuration window Set default clicking on the Set Default button defines a preselection of key parameters and their properties and sets them as default values Automatic result calculation when this box is checked results are calculated and automatically displayed without the need to press any buttons after reading a data file or at the end of a measurement In this case corrections zero point and thermal drift correction are also performed automatically Automatic results export as TXT file this option causes a small text file to be saved containing all results which are also to be found in the Results summary table if automatic evaluation has been selected The individual values are tab separated so that they can easily be imported into EXCEL 30 asmec ADVANCED SURFACE MECHANICS Always average equal measurements this field is only available if Automatic result calculation has been selected The average data files AVR are created automatically in the event that multiple tests with the same measurement parameters and at the same maximum force have been read or measured Results are only calculated for the averaged data Averaging multiple measurements can improve result accuracy Select all click this button to select all the values listed in the table for the results display Select none click this button to select none of the values
150. mum but better 60 s or more The change in indentation depth during this time is described via a linear fit function We recommend not using the first few seconds of the drift segment for the fit The fit range should lie between a lower limit Start and an upper limit End of the hold time The default values are 25 and 100 26 asmec ADVANCED SURFACE MECHANICS Fit range for thermal drift conection 2 of trax Start 25 End fioo Get contact stiffness from the unloading curve is adjusted using two different functions The first derivative of both functions at maximum force gives the contact stiffness Function 1 is a second degree polynomial F c C h c h The result is given in the stiffness value S1 Function 2 is a power function of type F C h h The result is given in the stiffness value S2 Parameter S is the average value of the two results S1 S2 2 Get contact stiffness trom n the field Get contact stiffness from you can select which of the three e 5 Average of bath stiffness results is to be used for calculating hardness and Young s modulus C 51 Polynomial fit C 52 Power low fit Hardness and modulus calculation Epsilon factor the epsilon factor describes the ratio of elastic deformation over the contact surface to that under the contact surface There is a correlation between epsilon and the unloading coefficient m when a power function is used for the fit
151. n Close on A a pre wih ai a N ww S E Modulus GPa lt e Oo Fig 66 The Fit Data window with data for a QCSM measurement on soft DLC on Si 5 Now press the Extrapolation to X 0 button The linear fit will now be extrapolated to X 0 and the result for Young s modulus or hardness at zero indentation depth will be shown in the field to the right of the button 5 1 10 Determining a hardness ratio or difference to a reference measurement For very thin coatings or indentation depths less than 50nm the use of a hardness ratio instead of absolute hardness values is recommended as the influence of the substrate or the tip rounding of the indenter cannot be corrected completely The limit for the coating thickness where reasonable hardness values can be obtained depends on the tip radius and the hardness ratio between coating and substrate It is not always necessary to use a CSM QCSM measurement A hardness ratio can also be determined from Martens hardness or the Estimated indentation hardness A QCSM measurement is better however as it is more accurate in the smaller depth range Moreover it is possible to calculate the ratios of other values in addition to the hardness ratio The following steps are necessary 1 Read the first AVR file Display the results in the Average results window and go to the Results over depth page 2 Select H Indentation hardness as parameter for the Y ax
152. n the keyboard shift the curve to left or right The overall movement is shown in the Move field The fit is then performed again and h0 is determined When the best fit has been achieved the movement to left or right has no effect other than to exclude data points from the fit range The result of the zero shift does not change in this case but only occurs for very large movements gt 500nm The vertical arrow buttons vt or the arrow keys on the keyboard increase or reduce the number of data points for the fit in the upper area of the curve The first and last points for the fit are given in the fields in the top right hand corner of the window The first point will normally be Point 51 if data for the surface detection exist The blue arrow keys modify the number of points for the upper end of the fit range The green arrow keys modify the number of points for the lower end of the fit range The Back 5 button with the blue circle restores where possible the original status of the fit not available for every step Click on OK to perform zero point correction or on Cancel to discard the results 4 4 Correcting thermal drift Thermal drift is corrected using a hold period at constant force For this reason displacement controlled measurements are not suitable for this type of correction It is advisable to employ a hold period at relatively low force compared to the preceding maximum force in order to avoid creep or other relaxation proc
153. n to zero depth and the result red arrow The same procedure can also be used for QCSM measurements which are better suitable for extrapolation purposes 1 In this case use the Results over depth page in the Average results window 2 Press the Add Graph ofc button to copy the curve of Young s modulus over depth to the Comparison window 3 Press the Fit tad button in the Comparison window The Fit Data window with the transferred curve is shown The green points define the fit range Double click on a point to specify the left hand limit of the fit range Click on Right end in the Define by double click box to specify the right hand limit of the fit range with a double click 67 asmec ADVANCED SURFACE MECHANICS 4 Press the Calculation button in the Fit Data window A linear fit will be performed this corresponds to Fit function 1 which is preset Et ata Soc Points 9 Mean difference 0538085 Mean differ 53 8085 Max difference 1 19061 Atpointnumber 0 Sigma difference 0 67508 Modify Read TXT amp Read PAR V Show Data V With marks MV Show Fit M With marks Showresiduals V With marks M Show range only Start at 0 0 Points for fit curve 100 a Define by double click C Leftend Right end From To f point E point E zi Fit function 1 2 X column 1 v No action v Y column 2 v No action v Xfactor 1 Yfactor 1 pease Contact depth um Calculatio
154. n using fully elastic measurement ccccccssseccceesececceesceeceeseceeeesecesseeceesauecetsuneess 108 6 3 Calibrating the effective indenter FACIUS ccccceessccccssseccccesecccceecceseesececsuseceeseusceesauecetseners 111 6 4 Determining instrument stiffness from high load indentations with pyramidal indenters 113 6 5 Determining the instrument stiffness in tensile GireCtiOn ccccceeescceesseeeecseeecseeneseeeneeeeees 115 PG IOAN WIGAN erea usps tanciadus tenn seaesgeycgnt roster actecesasmenuiaciouth hcceceumciantieauchonvarebnenaiecsetvaaereioe 117 Fd INGENTATION TONGS SSUIMGATION mscrterncd vid snarsivcsswncandeasnscctninddarnesoued soneossaubeaubouin otieavresiucnsndeeuniuiess 117 Fa Mod IN acer sears sarees nc ec S 118 Tos AVIO GUIS CONV ELLER erea E E E meni es 120 LA Tae asses etree trea ote cea ncn cc ed on cate ct ches E E 120 Explanation Of Results and Formulas os snucaseseetcesesanwirouraansegedtncnmanesin tegtonenasaiainoehad sonedeaaintatvaasicbaasmnanenaciate 123 8 1 Explanation of results of hardness t Sts cccccssseccccsssccccsseccccesececeeeseceseesecessueeceesesecessegeses 123 82 EXplanation or SCT ate tests resulti necmi 127 Oo 143 Calculation OF eTO esonta eR ESNAERA ARER REN O 128 SA FUCO ee A R E E E E E E 130 Boe RECOMMMENG aer UE a E E cbhgactonsentimicbbennautoaties 131 Raw data formats of various instruments essssssseeesssssssserresssssrerrresssseerrresssssrerereresss
155. nerally requires a long measurement time This makes accurate thermal drift correction necessary At the end of the measurement cycle there is a hold period for determination of thermal drift However the drift rate must be constant over a long period which cannot always be guaranteed Measurements lasting over one hour are therefore not recommended This has no effect on measurement of the friction value however After completion of a measurement or reading of a data file the lateral curves are shown on the Lateral F h Curve page in the Measurement data window E Measurement data from 60_1327_S10 7_0001 DAT Points 10060 i N F N h pm t 3 0 00 3 EE 0 013 0 000 0 00 2 0 033 0 003 0 06 3 0 006 0 002 0 13 4 0 032 0 001 0 19 5 0 028 0 002 0 25 6 0 016 0 002 0 31 7 0 000 0 002 0 38 8 0 005 0 000 0 44 _ 9 0 027 0 002 0 50 z 10 0 032 0 002 0 56 11 0 006 0 001 0 63 m Fd 12 0 022 0 9000 0 69 Q 13 0 017 0 000 0 75 14 0 046 0 000 0 81 y z 15 0 069 0 9000 0 88 oO 16 0 104 0 001 0 94 ha a 17 0 086 0 001 1 00 Ka 18 0 098 0 001 1 06 g Oo 19 0 084 0 002 2323 o 20 0 077 0 001 1 193 r 21 0 120 0 090 1 25 Fa 22 0 109 0 000 1 31 Z 23 0 164 0 001 1 38 24 0 199 0 001 1 44 25 0 243 0 090909 1 50 26 0 299 0 0091 1 56 WV Corect spring force V Use Reference WMV Correct indenter compliance Show friction J Normal lateral displacement graph f Marks V Lateral force displacement graph
156. nformation amp 2 3 Measurement data from TiN_81_QCSM_3 0012 DAT secon ox Measurement with instrument z TL a iia E RT RATT TARTS ERR LETT LETS LEME URIS TTT IN RERL SOCCER NULNT A UREN EERIE TERT NUEREL QGREREDNSTT R aaa No 0412001 Force Displacement curve F m um indenter Berkovich No B1 Force amplitude FES Area function no 14 Displacement amplitude x100 gt i 0 091 9 001 ii From 22 11 2013 F 0 119 0 092 51 3 0 145 003 76 Sample TIN s 0 178 0 005 01 Sample no 11 5 0 216 0 006 26 Absolute position reference point 0 263 0 007 51 X 46 326 mm 7 0 311 0 009 76 Y 36 182 mm 8 0 480 0 013 43 katan i ang ke po Relative measurement position 20 805 0 4 D 12 6 X 250 000 pm F 12 2 969 0 057 16 2 Y 100 000 ym S 12 466 0 076 20 09 Z 0 091 um E 13 6 29 0 095 23 76 Maximum normai force 150 000 mN Z i4 460 0 114 27 Application Hardness modulus measurement 2 as aoe 0 293 31 with QCSM method rr a a se Seat z if Ha 17 16 94 0 172 38 441 0 191 42 a 268 0 211 45 76 o Z 428 0 230 49 z lt L 32 921 0 24 53 09 74 0 268 56 2 904 0 287 60 8 394 9 306 64 09 54 21 0 32 67 6 60 37 0 346 7i 66 860 0 366 75 68 386 8 6 80 635 406 85 321 1 425 6 444 Vibration V Show V ration results Ampituds C Phase 0 00 0 10 0 20 0 30 0 40 0 50 7 Showgaph IY Maiks Normal Displacement um Colect Anaboe a i Clear Save Close i eo ene pel Rieke O
157. normal displace _ l H Indentation hardness A E Indentation modulus Your Percent Width defines a relative value for the width of the bars Er Reduced modulus E Plain strain modulus wit Percent Depth defines a relative value for the depth of the bars ns Sample Poisson s ratio Ei Indenter Young s modulus Start height axis at zero ends automatic scaling of the left hand axis and ni Indenter Poisson s ratio Ea ara eae begins the display at zero HMs Martens hardness from HV Equivalent Vickers hardan Presentation changes the type of presentation 41 asmec ADVANCED SURFACE MECHANICS Contour plot contour lines are drawn for areas of uniform hardness or other values see Fig 111 3D grid the results are shown as a three dimensional grid Line graph of 1row column single rows or columns can be selected for display in 2D form To select a row click the Choose row option and enter the row number To select a column use the Chose column option 26 32 O 26 485 26 156 O 26 312 O 25 992 O 26 139 O 25 828 E 25 966 E 25 663 E 25 793 H 25 499 E 25 62 H 25 335 E 25 447 m 25 17 m 25 274 E 25 006 E 25 101 E 24 842 E 24 928 E 24 678 m 24 755 133 B 24 513 E 24 582 E 24 349 E 24 41 ae 123 24 185 E 24 237 E 24 02 E 24 064 E 23 856 E 23 891 E 23 692 E 23 718 E 23 528 E 23 545 E 23 363 E 23 372 E 23 199 E 23 199 AN Aa WoX 200 300 400 500 600 X um Fig 34 Results
158. nt loads 2 Multiple measurements have to be averaged and evaluated automatically or manually The results will be shown in the results table el Results summary No fie __ ssnple Same a Beverg _ fp ff get yt reep a a T T E e a E E a Frobe_2_565_3mM AYA Probe_2 2 5 al nt 0 093 16 221 143 50 132 55 0 200 13 13 T 1 0 6 Probe_2 BS 1OmM AYR Probe_ 2 3 0 182 16 244 155 84 142 15 0 200 11 46 1441 5 af Probe_2 BS 30mM AYR Probe_ 2 4 30 008 0 329 14 658 169 56 153 26 0 200 10 50 1385 5 43 Fig 62 Results table with 3 results for the same sample but different forces 3 A graph of the Young s modulus over depth has to be generated from these results To do this click zi the Graph a button in the Results summary window The Data selection for Graph window will open Select Column h with indentation depth values for the X axis and press OK Then select the Young s modulus Column E for the Y axis and press OK twice 3 002 0 093 15 22 43 90 0 10 003 0 182 15 244 155 64 142 19 0 30 008 0 329 14 658 163 56 153 26 0 Data selection for Graph AKIS h ae Y AXIS E Pa With error bars if available Use the focus rectangle in the summary table to choose the column for 4 axis and press OF Then use the rectange to choose the column for y axis and press OF again Finally press OF a third time Cancel Close Fig 63 Window for selecting columns for the graph display The graph with at least 3 points fro
159. nt sequence is shown on the Graph subpage as in the Application parameters definition window see Section Fehler Verweisquelle konnte nicht gefunden werden Two very practical functions are restoring the application parameters and retrieving the measurement position on the sample Go to position below indenter Moves the sample stage to the position below the indenter at which the measurement was performed The Z stage is raised 3mm beforehand for safety reasons As long as the sample has not been removed from the holder the measuring position can always be found again Go to position below camera Moves the sample stage to the position below the camera at which the measurement was performed The Z stage is raised 3mm beforehand for safety reasons and then lowered again slightly Restore application parameter Restores the application maximum force and the exact measurement sequence used for this measurement The values are transferred to the Application window This allows effortless programming of new measurements with the same sequence It will ensure that the application parameters are always the same even if they were not saved as a PAR file 33 asmec ADVANCED SURFACE MECHANICS Information for TiIN_B1L QOCSM_3 220mhLAVR as Main Position and segments Instrument Indenter Applied comections Hardware Application Normal force unit Normal vibration Graph Segments 7 Absolute time s 199 4 Absolute points 12
160. nt to obtain the pure deformation of sample indenter No instrument has an infinite stiffness Depending on the type of instrument stiffness may vary between 100 mN um and a few thousand mN um Even instruments with relative displacement measurement against the sample surface using a cylinder or a reference contact have residual compliance which must be taken into consideration compliance inverse stiffness In principle the stiffness result cannot be differentiated from depth and force calibration errors Stiffness results are therefore always influenced by calibration When a strange stiffness function is obtained this can also be caused by a wrong depth or force calibration Calibration of instrument stiffness is one of the most difficult operations in nanoindentation praxis It requires carefully selected reference materials with well known elastic properties Use of glass with a Young s modulus between 60 and 100 and other materials with a large modulus e g sapphire is recommended The materials should display no pile up effect if measurements are performed in the plastic range pile up occurrence of upward bulges at the edges of the indentation so that the contact area is enlarged Stiffness and area function calibration are interdependent and can only be carried out in an iterative Way Theory The contact depth is calculated according to he Anax F C m F E z f 103 asmec ADVANCED SURFACE MECHANICS
161. ntact depth X b Smoothing Parameter for Y axis 0 H Indentation hardness x 0 70 i l V Adaptation to unloading modulu 0 60 Read Reference Clear Ref Reset Mv 2 07 02_B14_100mN 1 4 R ae V Marks 0 50 C Both results Fit marks C Results difference gt D w Indentation hardness ratio D i 0 20 0 10 Add results to table V Show parameter graph 0 00 0 00 0 10 0 20 0 30 0 40 0 50 0 60 0 70 Sh Contact depth um Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration 1of2 4 gt Fig 68 The Average results window with the calculated hardness ratio of 2 samples More AVR files can now be imported and the ratio to the reference measurement will always be shown In addition to the hardness ratio the hardness difference can also be shown by clicking on Results difference With QCSM measurements the ratio of additional values can be shown including that of Martens hardness The illustration below shows the calculated hardness ratios of Martens hardness and indentation hardness for the same samples The difference arises from the inclusion of elastic deformation contributions for the Martens hardness 69 asmec ADVANCED SURFACE MECHANICS gt o oO gt o o D oO Q oe co Oo oO oO Hardness ratio oO oo oO Hardness ratio from Martens hardness 0 10 e Hardness ratio from Indentation hardness 0 00 0 10 0 20 0 3
162. ntered in the Software access code field Purchasing the licenses is described in 1 Clicking on the Get Disk ID No button causes the current hard drive ID number to appear in a decimal number format in the field to the right of the button This is required for calculation of the software access code if the Run with log file box is checked the measurement sequence will be saved in text file LogFile TXT This file is in the same directory as IndentAnalyser exe The test sequence is recorded in the log file exclusively for the manufacturer s information for service and support purposes equipment failure or program crashes The default folders for the following file types are defined in the following fields e configuration files CFG or CFU files e parameter files PAR files e position files POS files 17 asmec ADVANCED SURFACE MECHANICS e test data DAT files The file path can be selected by clicking on the S button to the right of the relevant field All changes in the Configuration window which are required for a CFG file are only saved permanently if the Save button at the bottom of the window is pressed If the changes only apply temporarily for the current session pressing the OK button is sufficient These changes will be lost when the software is re started To discard all changes press Cancel 3 2 2 Modules page The Modules page Fig 9 oft he Configuration window is used to show which software modu
163. nts This can be test methods with one or two measuring heads The second head called Lateral Force Unit LFU is for instance used for scratch or wear tests For all other instruments there are only one or two applications available in the software and the analysis is limited to data from only one measuring head These are the applications asmec ADVANCED SURFACE MECHANICS Variable normal load displacement measurements Yield strength by cyclic measurements with spheres This application is additionally available for the UMIS 2000 only The following overview shows all available application types The analysis type is coupled to the application type That means for instance that the scratch analysis is only shown when the data file contains the information that it was produced with the application Scratch test l oadin mode Normal indentation Fast hardness modulus measurement ISO 14577 Fast tests in open loop mode default for most of the instruments ISO 14577 standard hardness and modulus T Slow tests in closed loop mode for UNAT and UMIS 2000 Ultra fast hardness modulus measurement Only for UNAT Variable normal load displacement measurements T Application for any force or displacement control in open or closed loop mode only UNAT Cyclic hardness measurement y Hardness modulus with QCSM or CSM method Dynamic test method only for UNAT and Nanoindenter XP G200 Elastic modulus m
164. nts will be automatically identified 9 6 Shimadzu DUH 202 data The original files with extensions DA1 or DA2 in binary format are not readable only data in ASCII format with file extension ASC can be read Use the export software ASCIl Transformation from Shimadzu Select Save Mode with the F3 key after file selection After correct selection an asterisk will appear next to the hardness average value Always answer the number of points query period with Zero 0 default to use all points otherwise you will receive an error message A number of example files are supplied in the Data Examples directory After ASCII export the file structure appears as follows DUH 202 ASCII FILE RTL MOB IDT LUT P DUT 2 50 VICKERS gf um TMD SPN SPB TLD j LDS AFT FLD MMO f MA2 MI2 CCT DAN P PAV TSP TDS 2 Testprobe 8283 10 1 00 2 10 10 Diamant Nr 10 00 02 3 gr 0 00 En 9 10 136 asmec ADVANCED SURFACE MECHANICS GAs DCT DAT KLO KDP KHD KLG KLH j MXL MXD MXH MID MIH 769 10 18 101 9 35 1 0042 286 465 8 00 8 000 1 0042 8 286 465 8 139 1967 No LOAD DEPTH CLOCK TEMP 1 0 0422 5 604 147 2 0 0 2 0 0424 5 627 147 3 0 0 9 7 Shimadzu DUH 201W data CSV files can be imported in ASCII format The file header rows in the file are ignored The start of
165. o use every third or fifth This can noticeably reduce the calculation time The Period property gives the number of points between one calculation point and the next The first and last points are always used in accordance with the First and Last fields The last period can therefore be smaller than the others Calculation starts the calculation The fit curve is shown in red Results the Results field shows the fit result for the modulus or radius and the mean absolute difference Mean D between each measurement data point and the associated fit point The difference provides an indicator for fit accuracy and should be below 2nm for a displacement less than 1um or below 1nm for a displacement less than 100nm A tab character separates text number and unit of measurement in the field The contents of the field can be selected highlighted with the mouse or arrow keys copied to the clipboard and pasted into a worksheet or text program Show check boxes the measured curve or fit curve is shown when these boxes are checked default Show title displays a line of text in the top part of the diagram With marks if this box is checked markers will be shown for each data point non default This should only be necessary if the number of points is smaller than around 100 Cancel a Cancel button appears when a calculation is running and can be used to stop the calculation This is particularly useful with 2 or 3 layers as the calculation time can
166. o voltage amplitude selected must give a vibration displacement signal of at least 2 3nm The default setting of the QCSM application mostly produces displacement amplitudes between 4 15nm depending on the material The difference between the vibration frequency and the resonance frequency of the measuring head must be sufficiently great to enable accurate determination of contact stiffness Frequencies up to 20Hz should therefore only be used for most applications Use of a frequency between 8 and 9Hz is recommended default value If accurate determination of contact stiffness is not an issue as in fatigue tests frequencies up to 200Hz can be used 73 asmec ADVANCED SURFACE MECHANICS Instead of QCSM measurements IndentAnalyser Version 3 can also be used for CSM measurements in which oscillation is always switched on and the vibration amplitude is determined continuously Measurement then takes place in open loop rather than closed loop mode Note In this case the vibration frequency must be greater than the data rate or equal Evaluation of measurements with the QCSM module is carried out as with a normal hardness test Read the data file and carry out zero point and thermal drift correction If possible drift correction should always be performed as the measurement time is significantly longer than with fast hardness tests and thermal drift has a greater influence Force Displacement curve e Force amplitude
167. oading The networks are trained on this range The value should be as near as possible to 10 of the indenter radius 2 Between the first 4 loading phases follows a 100 second creep phase at constant force 3 The 4th loading phase is followed by a 600s creep phase 4 Finally the indenter is fully unloaded once at the same speed and loaded again up to above the last loading force Signals over time 30 28 26 N N pe oO o e gt Signal a u So N R O 200 400 600 800 1 000 1 200 Time s Fig 87 Required measurement sequence as force over time Unloading in the first 3 cycles is not essential 85 asmec ADVANCED SURFACE MECHANICS InspectorX or IndentAnalyser automatically calculates the corresponding network input data for the neural network from the test data During configuration the correct values for instrument stiffness must be saved as either a constant value or a function and the correct area function for the spherical indenter saved as either a constant radius or a function If this is not the case the results will be incorrect Calculation options Zero point correction an optimum zero point location can also be determined via a neural network The result may differ somewhat from the zero point correction already implemented in the program Shape correction a neural network considers the effects of a non
168. oisson s ratio Pile up correction factor Unload g fit range From 4 98 Top 40 f Ps j j Show fit 1 Full range 0 i 5 I Show fit 2 Full range 0 00 0 10 0 20 0 30 0 40 0 50 0 60 0 70 0 80 0 90 R Show tangent Tangent startiathenas Displacement um Show plastic depth Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 52 Load displacement page of the Average results window During configuration it is defined which values will be shown in what colors and with how many positions after decimal point Unload fit range The unloading curve is fitted between an upper From and a lower To force limit by means of two different functions These limits are expressed as a percentage of the maximum force The upper limit should lie between 100 and 90 and the lower limit between 80 and 20 The default values are 98 and 40 Show fit 1 shows the fit to the unloading curve using a second order polynomial shown in red in the graph Show fit 2 shows the fit to the unloading curve using a power function shown in green in the graph F C h h Full range fields show when checked the fit curves over the entire range between O and 100 This allows you to check whether the fit curve follows the measured curve outside the fit range This is of particular significance if the fit is was not started at 100 as the gradient of the fit curve at 100
169. on has been carried out the data points which have been generated can be smoothed so that they can follow the fit function better This can be done independently and only once for each reference material by clicking on Smoothing i This area will then change smooth area function 1 Y 2 Y o The letters N No or Y Yes indicate whether smoothing has been performed It is recommended that smoothing is carried out before calculation of the stiffness function This gives significantly better results for the instrument stiffness B Calculation of area function ieie area function ba a a i Read data E modulus Poisson r D Sample 1 71 3 0 17 eS Sample 2 405 0 234 indenter 1140 0 07 Data from sample 1 r 4 Data from sample 2 lt lt more deal Tip f Fit function e i3 Fit average Pointsfrom 1 j to 34 i2 Save area function A A Average Tip radius upper limit um 0 2 Area deviation at 500nm 5 0265 Square root A um V Sample 1 V Fit V Sample 2 3 Area calculation Stiffness calcul 0 00 0 10 0 20 0 30 0 40 0 50 0 60 0 70 Save in CEC file he um x Ea coe Fig 104 The Indenter area function window after calculation of area function with 2 materials After you have clicked on Area calculation the calculation will take place and the result will be shown as a graph As in the example in Fig 104 with greater depths the function should run approximately paral
170. ond Young s modulus GPa 1140 Poisson s ratio 0 07 It is necessary to define the indenter material and its elastic constants in order to be able to calculate the correct Young s modulus for the sample Young s modulus GPa elasticity modulus the standard value for diamond is 1141 GPa Poisson s ratio the standard value for diamond is 0 07 For indenter materials other than diamond the data must be modified to avoid incorrect results Tip radius pm l P upper limit i Fd Effective opening angle w 1 qe wo Comment Determined with 4reatuncton Quar_ neu AEA Tip radius for spherical indenters this is the nominal tip radius entered by hand for pointed indenters it is the estimated tip radius The tip radius of Berkovich or Vickers indenters is estimated during the calibration process from the data which are closest to indentation depth zero This value is therefore only an upper limit not an exact value The closer the initial measured values are to zero indentation depth the more accurate the tip radius value will be Effective opening angle describes the angle between sample surface and indenter surface when the 23 asmec ADVANCED SURFACE MECHANICS indenter is regarded as a rotationally symmetrical body The Vickers indenter angle of 22 is for example converted to an effective angle of 19 7 This value is in most cases only for information and is not required for calculations For conical indenters
171. ons can be displayed The sign means power to y C C x C x y C C x C x C x 3 2 _ 1 2 2 1 2 1 2 1 4 3 2 m _ _ m m e m N UI U N m Wn W N be O y e2 130 asmec ADVANCED SURFACE MECHANICS C x C x C x ac C C x C Xx Function 15 is often used for the fit of the area function in accordance with the Oliver amp Pharr method and is used for example with the nanoindenter XP G200 8 5 1 2 4 5 6 Recommended literature ISO 14577 1 2002 Metallic materials Instrumented indentation test for hardness and materials parameters Part 1 Test method CEN 2002 W C Oliver G M Pharr An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments J Mater Res Vol 7 No 6 1564 1583 1992 T Chudoba N M Jennett Higher accuracy analysis of instrumented indentation data obtained with pointed indenters J Phys D Appl Phys 41 215407 2008 K L Johnson Contact mechanics Cambridge University Press 1985 Antony C Fischer Cripps Nanoindentation Springer NY 2002 Antony C Fischer Cripps Contact Mechanics Springer 131 asmec ADVANCED SURFACE MECHANICS 9 Raw data formats of various instruments 9 1 Introduction The import filter attempts to automatically identify the different segments loading creep unloading and hold period for all instruments
172. or i Corrections 22 paint conection gt Standard fit method Thermal drift correction f Manual f Hertz f Manual C Automatic C Linear C Automatic C None C Quadratic C None Use average drift rate from measurements Allow hold period use at Fmax Use average drift rate from hold periods 40 Inm Default depth range for zero point back extrapolation Instrument stiffness compliance correction Area function calculation f Use data fram present configuration f Use data from present configuration C Use data stored in data file if availalble f Use data stored in data file if availalble Statistics Acceptance range for measurement average times standard deviation 2 Black white output in results window during printout Fig 19 The Analysis Normal page of the Configuration window Fit range Fit range of unloading curve of Fmax the unloading curve is fitted using two different functions between an upper Start and a lower End force limit These limits are expressed as a percentage of the maximum force The upper limit should lie between 100 and 90 and the lower limit between 80 and 20 The default values are 98 and 40 Fit range of unloading curve 2 of Froax Start 38 End fao Fit range for thermal drift correction of tmax a hold period at a force between around 10 and 30 of maximum force can be used to correct thermal drift during a measurement This hold period should be 30 seconds in mini
173. or is 0 0926 Creep Absolute creep as depth difference between begin of unloading and end of loading Relative Creep as relative depth change during a hold period at maximum force C Creep h 100 Relative force relaxation Obtained from hold periods where the depth is kept constant depth control Total mechanical work It is calculated from the area under the loading curve including the depth change during creep at maximum force Elastic reverse deformation work The mechanical work indicated during the indentation procedure is only partly con 124 asmec ADVANCED SURFACE MECHANICS sumed as plastic deformation work During the removal of the test force the remaining part is set free as work of the elastic reverse deformation It is calculated from the area below the unloading curve NIT Elastic part of the mechanical work We Wtot in percent Estimation of the yield strength by the iterative formula 1 154 2 3 E ane which was derived using the expanding cavity model Alpha is the angle between indenter and surface 19 7 The value for H Y is limited to the maximum of 3 which can only be achieved for metals Work for plastic deformation as difference Wp Wtot We Estimation for the radius of plastic zone around an indent using the formula o ca pl 93 2 T Only valid for Vickers or Berkovich indenter See B R Lawn A G Evans D B Marshall Journal American Ceramic Soc 63
174. or the 40 asmec ADVANCED SURFACE MECHANICS graph if at least 2 fields or more are selected then only these fields will be used for the graph The With error bars if available field is checked if the error bars in the Results diagram are also shown in the event that error descriptions are available Then press the OK button again to display the diagram in the Comparison window 3 7 3 ol Displaying results as a 3D graphic or a contour plot The doll button opens the 3D result presentation window with all hardness values contained in the Results table shown as columns at the relative measurement co ordinates Note This function will only work correctly if the measurements in both directions are performed in a uniform pattern The distance between measuring positions must be constant e g 50um The grid spacing for the X and Y directions can be different however 3D result presentation f Parameter for presentation H Indentation hardness Presentation Bar chart C Contour plot C 3D grid C Line graph of 1 row column Chose CR 1 5 of 4 Percent Width 600 a Percent Depth 600 4 Start height axis at zero GB ie Fig 33 3D result presentation window Parameter for presentation Parameters for presentation this drop down menu is used to select the parameter which is to be shown in the graphic The default setting is F Maximum normal test fore indentation hardness h Maximum
175. owing the Windows conventions It is recommended to use an informative name which includes the symbol for the indenter and the creation date for instance B1_2013 11 01 CFG The software must be informed from which instrument the data shall be read and which tip was used for the measurements The menu to select the appropriate CFG file can be opened via the Open CFG button El Open Conhowoion rae n Path for configuration files CFG H E LaufwerksD elphilnspectors CFG Files Instrument gt Instrument number gt Indenter gt indenter number gt Area function number Configuration file aA E O4080002F Eleak Berkovich era 410 614_2012 09 06_newLFU cfg Valid until 06 09 2013 oto F214 2013 01 24 new LFUcig Valid until 21 01 2014 8 Bl4 2013 01 21 cfg Valid until 04 05 2014 o H Sphere HE unknown Ee Berkovich Flat Punch Sphere Cancel Open CFG file Full expand ev Gar Open CFG folder Fig 5 Window for the selection of the correct CFG file There are 4 hierarchy levels Instrument type The software can analyze data from other devices as well as from UNAT Generally however the only option will be ASMEC UNAT Instrument number Where several similar devices are in use they will be differentiated via the instrument number Indenter type illustrated via a symbol showing the geometry Area function characterized by an increasing number at every recalibration of the same test tip A large
176. own as the first column in order to define the rows clearly Max letters for file name defines how much room is provided for the file or sample name in the first column With longer file names the whole name may not be shown This value must be increased in this case Conversely a lot of space may be wasted if the file name is short Image file for Logo the ASMEC logo which appears at top left of the page can be replaced by your own logo To do this a graphic file will need to be imported in BMP format The file should be approximately 600 x 150 pixels Where logos have a different page to height ratio the remaining space must be filled with a white area 3 8 2 Report preview Each change to the formatting is immediately displayed in the Preview window The size of the page can be increased or reduced in preview by clicking on the grey area outside the page If the report is more than one page additional pages can be accessed with the Page up and Page down keys or via the scroll bar at the bottom edge of the screen The normal program interface only becomes visible again when the report is closed via the Close button in the Report Preparation window 45 sasmec ADVANCED SURFACE MECHANICS If a statistic has been calculated in the Results table the statistical values mean value standard deviation etc are stated for each column A grey line appears ahead of the statistical values to provide a visual separation Clicking on the
177. ple information 32 asmec ADVANCED SURFACE MECHANICS Information for TIN_B1_ QCSM 3 130mN AVR Emn Man Position and segments Instrument Indenter Applied correctione Hardware l Used instrument ASMEC UNAT Number 04080002F Instrument Program owner NTNU Used indenter Berkovich Number Bt o Area fia Measurement date and time 22 11 2013 23 47 24 File produced with program version 3 0 06 Normal force head used w Scratch option used X Vibration option used w Lateral force head used X External chanels used X Sample Sample name IN sample no Ba For customer NTNU Comment 1 Pe Comment 2 CO ca leet Ber SS CCCCCSC E taeae a Copy laaz Fig 23 The Main page of the Information window Click Edit to switch to Edit mode This enables sample information and instrument owner to be changed The title on the button will change to Save Pressing the button again ends Edit mode and saves the data file with the new information Copy allows all lines of sample information to be moved to the cache simultaneously and transferred to the Information window of a different measurement using Paste This saves a lot of writing if you have forgotten to enter the correct sample data and now need to do this retrospectively for several measurements Position and Segments page The application the complete measurement sequence and the measurement co ordinates are shown on this page The measureme
178. plitude 0 180 V 220 o Segment 4 Creep Frequency 8 49 Hz 200 Amplitude 0 180 V a Reset E 180 pri 3 O 5 MV Marks 160 S Fit marks pe o c 140 2 E E uw 120 a z fi S 100 5 7 5 t 80 AD Show C Amplitude Phase 60 Stitiness Phase difference Show 40 20 Vv Ti 0 10 0 20 0 30 0 40 0 50 0 60 0 70 0 80 0 90 7 Stifness Normal Displacement um V Phase difference h F Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 77 The same window after switching to display contact stiffness and phase difference Contact stiffness and phase shift as a function of indentation depth are displayed by clicking on the Show button on the right hand side of the window The Information field shows the parameters used with the QCSM method for all segments for which vibration was activated The parameters for the X and Y axes can be selected in the appropriate pull down menus The following can also be shown on the Y axis e H E ratio as a measure of yield strain e H E ratio as a measure of resistance to plastic deformation e H ratio as a measure of energy dissipation Error bars are shown if the curve is an average value from several individual measurements The error bars represent the statistical error which is calculated in accordance with a Student s t distribution as 75 asmec ADVANCED SURFACE MECHANICS AX eo vn with t n as the Stu
179. pressed for the first time 4 5 Averaging measured curves If several DAT files are read at the same time two windows will open Data overview and File selection for analysis The Data overview window shows all imported measurement curves The number of selection fields on the right matches the number of curves Unchecking individual curves excludes them from evaluation This is recommended for curves which differ significantly from the others To find out which curve number is involved when there are a large number of curves simply mouse click exactly on the curve it may be necessary to zoom out partly The curve number will be shown top left in the Data overview window In the Analyse field of the File selection window you can specify whether each curve should be analysed individually Every single file or if average value curves should first be generated from all equal measurements and only the averaged curves evaluated Average files with equal parameters first 54 wo M Normal Force mN M 3S on 500 450 400 Q9 an on ga 0 00 Normal F h Curve f Data overview 075 100 125 150 Normal Displacement um 0 25 0 50 1 75 asmec ADVANCED SURFACE MECHANICS Sex Use Meas Point marks C All C All x C None None A Test 1 m Test 2 B Test 3 Test 4 i Test 5 a Test 6 B Test R Test 8 E n Test
180. ption by f Constant value f Function with up to 10 parameters f Data table Fig 121 Inputting instrument stiffness in the Configuration window The Stiffness description by field must be set to Constant value For Function type use Stiffness function That concludes the determination of instrument stiffness in tensile direction 7 Additional Means The software contains a number of means for planning and evaluating experiments 7 1 Indentation force estimation The Indentation force estimation window is accessed via Tools gt Indentation force estimation It is used for planning tests If the hardness and Young s modulus of a material are known the values can be used to estimate the force required to attain a given indentation depth or contact depth during indentation with a pyramidal indenter This calculation is not possible for other indenter types e g spherical Use the Set button next to the relevant field to decide whether the force required for a given maximum depth or a given contact depth should be calculated The other depth is always calculated and displayed also Indentation force estimation Hardness GPa a Youngs modulus GPa j220 set Maximum depth um 4 i Contact depth um Required force mN 156 06 Fig 122 Window for calculating force for attaining a given indentation depth 117 asmec ADVANCED SURFACE MECHANICS When the Average results window is open the results for hardne
181. r pttttstteeteeeeeceeeeeeecessesesessteeeeeeeeeeeceessessnsteseeenereeeeeeeaeeees V Automatic result calculation Set Default poan SEN seats Set Default M Automatic results export as TXT file Basic units Length unit um Force unit mN v Always average equal measurements Hardness unit GP a Time unit s pr Select all Select none Modify Symbol Unit Digits Color Bold Description IN 0 a E Black g Measurement number gt Up 4 Down All equal All equal All equal This order defines the output order screen printer Symbol Unit Digits Color Bold Description No a N 0 Black N Measurement number 0 C Cycle 0 Black N Cycle number 1 a O x um 1 Black N Relative measurement position x co ordinate 2 7 Ses um 1 Black N Relative measurement position Y co ordinate 3 Cj Zz um 1 Black N Relative measurement position Z co ordinate 4 Sno 0 Black N Sample number of current application 5 F mN 3 Black N Maximum normal test force 6 h um 3 Black N Maximum normal displacement 7 H GPa 2 Black N Indentation hardness 8 E GPa 1 Black N Indentation modulus Young s modulus 9 O Er GPa 1 Black N Reduced modulus 10 O E GPa 1 Black N Plain strain modulus without indenter 11 Vo ns 3 Black N Sample Poisson s ratio 12 Ei GPa 0 Black N Indenter Young s modulus 13 O ni 3 Black N Indenter Poisson s ratio 14 O HM GPa 2 Black N Martens hardness 15 O HMs GPa 2 Black N Martens hardness from slope 16 is
182. r X values and Column 2 for Y values In the selection fields to the right of the above data can still be converted with e No action no change to data e Square Y square Y values e Square root Y extract square root of positive Y values e 1 Y invert Y values e Ln Y logarithmize Y values X and Y values can also be multiplied by factors which should be entered in the X factor Y factor fields E Fit Data Function number 0 1882 Number ofterms 2 const 0 18741309 0 1880 x 6 572565331E 06 Fit range 0 1878 From 23 525 To 127 265 Points 831 0 1876 Mean difference 0 000241675 ji Mean differ 0 0241675 0 1874 fi ful i Max difference 0 00100413 Inte a 7 j Modify 0 1872 a i i e _ jja ir a _ i Ny i it i i i l i S ReadPan s x lt M Hi I p He i it i Is i l Lie id ShowData 7 With marks Z i bi Ml Y i Le i V Show Fit M With marks gt 0 1868 A il t 1 t W t i M Show residuals With marks Y j i itt ri Nt H V Show range only Si 4 0 1866 h j I yj J l ml ae Points for fit curve 100 i i Define by double click C Leftend Right end 0 1864 wie STEPIE 0 1862 Fit function 1 sj 2 X column 1 No action 0 1860 Y column 2 v No action x f No action 0 1858 nici Square Y Extrapolation to X a Fay Ba 30 40 50 60 70 80 90 100 110 120 gt C Time s Calculation Close Fig 128
183. r has been changed Inspectorx You are using a new indenter of different type than before Please Read the belonging CFG File or Read the belonging data From the database with Open DB TF you want bo use a new indenter without existing area or radius Function please Write the indenter parameters into the Fields by hand indenter number material elastic properties radius Do the calibration of area or radius Function using the menu Calibaration in the main window The input of calibration data is not possible by hand Fig 16 Warning when the indenter type is changed It points out that the appropriate calibration data for the indenter must be entered or determined Indenter No enter a unique number which will allow the indenter to be identified later It is advisable to use typical abbreviations e g B for Berkovich or S for sphere Area function No for every indenter there is an area function which describes the indenter area as a function of the contact depth Normally the tip of an indenter diverges from the ideal shape and a corresponding correction is necessary The actual shape is described using the area function During the service life of an indenter there are further changes in shape due to wear tip rounding A new area function is therefore necessary from time to time Every such function receives a unique area function number and a validity period Indenter material Indenter material Diam
184. r number for the area function is normally associated with a later calibration date This need not always be the case especially if CFG files are created on a different computer and then transferred to the instrument computer Ga Open CFG fold a he I The Open CFG older button can be used to select the file directly via the file name in the file manager 15 asmec ADVANCED SURFACE MECHANICS The file selected is opened by double clicking on the name or via the Open CFG file button When a new indenter is used for the first time no CFG file will exist and one must therefore be created This is done by opening the Configuration window with the Configur button and selecting the indenter type on the Indenter page When the indenter selection menu is left the message below appears Inspector i Soe You are using a new indenter of different type than before Please Read the belonging CFG File or Read the belonging data from the database with Open DB If you want to use a new indenter without existing area or radius function please Write the indenter parameters into the fields by hand indenter number material elastic properties radius Do the calibration of area or radius function using the menu Calibaration in the main window Fig 6 Message after definition of a new indenter pointing out that calibration data must still be assigned or a calibration performed A unique number from which
185. rach Arithmetic roughness average along the scratch length before scratch Root mean squared roughness average along the scratch length before scratch maximum peak height and maximum valley depth R Maximum height of the roughness profile along the scratch length as difference between hp Maximum plastic deformation as largest height difference between last and first surface scan 127 asmec ADVANCED SURFACE MECHANICS Maximum normal displacement under load Maximum normal displacement after unloading maximum depth of last surface scan Maximum depth difference between the scan under load and after unloading Difference between hm_ul and hm_au Lateral position for the begin of plastic deformation if detectable Normal force for the begin of plastic deformation if detectable Friction coefficient for the begin of plastic deformation if detectable Lateral position for pre defined depth limit 1 under load The depth limit is defined in the X_1 configuration window page Analysis lateral Normal force for pre defined depth limit 1 under load Friction coefficient for pre defined depth limit 1 under load Lateral position for pre defined depth limit 2 of residual depth change The depth limit is F n_1 ul defined in the configuration window page Analysis lateral X F f n_f u_f Surface slope in the direction of the scratch obtained from the first surface scan before the scratch
186. rce Marks JV Lateral force Marks M Friction Marks 0 50 100 150 200 I7 Show legend 7 Show cursor Distance um Se more d Normal Ffh Curve Lateral Ffh Curve Normal data over time Lateral data overtime Seratch results Approach Fig 93 The Scratch page in the Measurement data window after import of a background image Two depth limits for the scratch curves can be entered in the configuration see Section 3 2 6 They can be changed on the Scratch page The position and force values at which these limits are exceeded are shown in the text field All results shown in the text field are also displayed in the Results table allowing different tests to be evaluated one after the other and the results collected It is not possible to mix the evaluation of scratch tests with that of hardness tests 5 10 Analysis of friction and wear tests The lateral force unit is required to perform friction and wear tests To EJ Normal indentation evaluate a wear test the normal lateral indentation mode is required in apy Norma lateral indentation the main menu When Normal indentation mode is used the following message will appear x Warning the present mode ignores lateral force parameters Warning The present mode ingnores lateral Force parameters 91 asmec ADVANCED SURFACE MECHANICS A wear test consists of a few to several hundred cycles with the same parameters and therefore ge
187. rea function is shown as an ASCII table with the contact depth and the square root of the area in two columns This option is not available in Version 2 Radius function this option is only used for spherical indenters Instead of an area function a radius function effective radius over effective depth is used to describe the indenter shape Fit function No number of fit function The number is selected during calibration and cannot be changed here The link between the number and the corresponding function is given in the Help menu 24 asmec ADVANCED SURFACE MECHANICS The Fit Data window is opened with the button and is used for graphic display of the fit function see Fig 14 This window is an effective tool for data analysis and fitting Coefficients this field shows the coefficients of the fit function and their range of validity between a lower limit from and an upper limit to Outside this range an ideal indenter shape is assumed The data can be changed manually by pressing the Edit button A new Coefficients window see Fig 17 opens the fit function and coefficients can be changed here Note you should use this program option if you are working with an area function from an external source Use the polynomial function which is used for description of the area function and select the associated number of the fit function Comment Determined with Are indenter area function lw Us Fit Function
188. repeated When the calculation is complete a new diagram will show average friction over the number of cycles and new checkboxes will appear on the right hand side of the window They allow the following to be displayed e average maximum and minimum friction over number of cycles or time e average maximum and minimum displacement over number of cycles or time e work per cycle over number of cycles or time Both vertical axes of the diagram are used for the display The black axis belongs to the black curve and vice versa The slope of the average displacement over cycle number curve corresponds to a wear coefficient and can be expressed in nm cycle The Fit data window see chapter 7 4 can be used to calculate the slope With this test method a resolution of better than 0 1nm cycle can be reached 94 asmec ADVANCED SURFACE MECHANICS Lateral Data Analysis o E eE Surface slope o o Correct Show Complete cycles Average of back and forth Average cycle results over cycle number Average cycle results over cycle end time Cycle 100 3 to 100 4 of 100 Point 1 to 82 4 of 82 Point shift fo 41to 41 WV Average friction jv Marks Maximum friction jv Marks F Minimum friction WV Marks F Work per cycle jv Marks vV Average displacement V Marks V Start at zero Maximum displacement W Marks i lV e Average friction Mean displacement Calculation for cycle 100 Average friction 0 10
189. rix with headers extension TXT ASCII matrix without headers extension ASC Excel file file extension XLS Windows Metafile format file extension WMEF This format saves the complete diagram Note all files contain just two data columns with the X and Y data for the visible curves Please use the Save button in the main menu if you also wish to save the time data stiffness data or piezo voltage Normal F h Curve Normal signals over time 48 asmec ADVANCED SURFACE MECHANICS Page Normal signals over time the chronological sequence of the measured data is shown here The piezo voltage can also be shown which is not required for the evaluation of the test data By checking the Graphs and Marks boxes in the Measurement points subwindow you can specify which curves are displayed and whether the point markers should be shown The Y axis is shown in arbitrary units a u Due to the different units it is possible for one curve to be displayed using the entire graph area while the others may lie closer to zero To make viewing curves easier it is possible to scale them automatically or manually so that the maxima and or minima of the curves coincide Auto scale starts automatic scaling The scaling factor determined is shown in the Factor fields and in the legend The measurement units for the curves are also shown Av Force mN x1 in the legend The legend can be positioned wherever required in
190. s HUpl or indentation hardness If more than one unloading cycle was measured cyclic measurements or if depth dependent contact stiffness values are present e g when using the QCSM CSM option during the measurement there are much more choices available The desired parameter to be displayed can be selected from the pull down menu at top right 64 m Ei Average results E Modulus GPa 0 0 00 0 10 0 20 0 30 Contact depth um Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration 0 60 asmec ADVANCED SURFACE MECHANICS Quar2ffB2_B2_100mN 1 4 R Parameter for gt lt axis 1 Z Contact depth Smoothing Parameter for Y axis D 0 Er Reduced modulus HM Martens hardness Reset HMd Differential Martens hardt Reset H Equivalent Vickers hardne S Contact stiffness of sample a Equivalent contact radius M i Ac Projected contact area witk l Fit marks H E measure for yield strain H E GPal measure for resista E H GPa measure for capac Add results to table MV Show parameter graph V Show error bars Fig 60 The Results over depth page of the Average results window with the result of a QCSM measurement on fused silica The Read reference button allows you to read a reference data file AVR file and calculate a hardness ratio or a hardness difference in relation to the dat
191. s allows an estimate of the manufacturing quality or degree of wear of the tip and gives a good basis for comparison by always referring to the same depth Fit function Fit function S Area function and instrument stiffness function will be described by a fit function to use them later in a simple way for analysis The function should therefore follow the data points as accurately as possible In the program the square root of the contact area as function of the indention depth can be described by various fit functions A visual check on the match between fit function and data points is recommended The small depths range of the graphic should be zoomed out as the course of the function there is particularly important see Fig 105 In the Fit function field the function type can be selected see section 8 4 The question mark button opens a small window which describes the terms of the function The sign stands for the power e g x 2 x The number of terms C can vary between 1 Function 4 and 9 Function 12 The number of terms must be less than the number of data points otherwise a warning will be displayed and the calculation will not be performed In the example chosen fit function 8 was selected with 5 terms C 1 2 1 4 3 2 Fit points from to Points from l to 34 l Determines the fit range for the area or stiffness function Point 1 is the value with the lowest indentation depth or force De
192. s are only available when a graphic is displayed in 3D Normal resets the 3D command setting deactivates the following 3 buttons and allows zooming by dragging with the mouse a Move allows the diagram to be moved relative to the window by clicking the left mouse key and dragging with the mouse The function is specified in the status bar of the Graph Commander The legend does not move with the diagram Aa Rotate left mouse click and drag to rotate the diagram relative to the window The function is specified in the status bar of the Graph Commander window E Zoom left mouse click and drag to zoom the diagram compared to the window size The function is specified in the status bar of the Graph Commander 3 7 a The Results Table 3 7 1 Working with the table The table in the Results summary window summarizes all the results for the parameters which were selected during configuration The symbols for the headers are also defined in configuration Each time a measurement is evaluated at least one new row is created in the table The number of rows therefore continues to increase until the table is deleted or the program is closed The table is only used for evaluation of hardness measurements with the Average results window or for evaluation of scratch tests Itis not used for other measuring procedures When a statistic is generated the window consists of two tables see Fig 30 otherwise only the upper table is visible
193. s checked The Acceptance range for matching is set in the Statistics area on the Analysis normal page of the Configuration window The standard deviation determined for the maximum depths of the measurements is multiplied by this factor If the depth of individual curves lies outside this range around the mean value of the depth it is recommend to exclude these curves from averaging It is recommended to exlude measurement iz 23 64 From the average Excluding measurements as recommended is done in the Data overview window pressing OK automatically unchecks the relevant measurement number In the example measurement Nos 12 23 and 64 are excluded Sample Poisson s ratio The Poisson s ratio is necessary for the calculation of Young s modulus from depth sensing measurements If it is not known it can be estimated or taken from the database available from ASMEC separate module The value entered here is applied to all data files If data from different materials is evaluated together it may be necessary later to correct the Poisson s ratio Save all files with equal load depth after correction as DAA specifies that a new data file with the extension DAA for all data will be stored for each averaged curve default setting This file will contain all curves from which an average value is generated after correction This has the advantage of avoiding the need to repeat the correction if the data are being evaluated again and st
194. se Thus the use of Power function only makes sense for elasto plastic indentations and is also most accurate in this case as the unloading exponent can be considered Fig 123 shows the calculated curve for the parameters of fused silica with an unloading exponent of 1 25 With the lt lt Results button a field containing the calculated data can be opened see Fig 124 The symbols are explained in Chapter 8 Pressure distribution Result m coh Load Foints F 100 0000 mN mE 0 2 x a hl C Flat punch he 0 6651 um M Constant i apab as f Power function 5 254 6859 mN um 100 ur 46237 Ba ath Ap 11 5230 un Hardness GPa 9 5 AC 10 5270 pm Young s modulus GPa 72000 a 1 8305 um Poisson s ratio i f Creep length nm o Fig 124 Results field in the Theoretical curve window for the data from Fig 123 Theoretical curves can be saved as data files in the InspectorX IndentAnalyser format via Save as DAT and then evaluated as test data to check the model accuracy Please note that either the actual instrument stiffness should be entered in the Instrument stiffness field and used for the calculation or else the evaluation should be performed later with an infinite instrument stiffness The influence of thermal drift can also be simulated in the calculation This requires values to be entered in the Thermal drift and Loading rate fields as the effect of drift also depends on the loading and unloading rate On
195. seerrreessseeere 132 9A MOGUO ee nee ree tents reece eer eerer earn ee er rrreeec rr ee eee ere 132 92 Nan indenterXP G200 data wiceciveiececenssnctiavacarenenccncesiatdusueaniavedcansceveneneeusshicdietiemearebeieeeneeick 132 i UM 2 a appara tse ecceeaciv E E E soon catia lesen cata E E 133 oa EIS CING 1S CO Mi aa nan boca ustsiestecnaiepaastunnninast nd aGaaeuncranenciensantiaaoanee sed aeneeusaiaeentaaconecbanninesbans 134 ga 25121 gE 2 Lc ae ee nee ee eee eee ee 136 Io SAA DURO A I n EE uses deaautea E werteaareaunaauness 136 97e Sina 2 DUH 20IW Uat aeere eper ern E AEE 137 2e NDO TAa a E A E si deerocsnaaucaeedeaieeneseecs 137 23 AC MNATO e E E cthacetouseutimcobennautontiets 138 9 10 Data from a Zwick hardness measurement head cccsccccccccceesesseececcessaaeeeeeeeceeesseaeeaeees 139 asmec ADVANCED SURFACE MECHANICS 1 Introduction This user manual is designed to assist you in using the IndentAnalyser software Some of the modules described are not always available The requirements for using the modules are generally indicated The functional scope of the software depends on the software modules which are purchased This user manual requires basic knowledge of the operation of computers using the operating system Windows 7 or higher together with some knowledge of English as the user interface is only available in English No explanation is provided for specialized expressions which are similar in English and G
196. senecessenes 6 Bites PE E a E ea reneneaaien 7 2 2 1 HAVU COMIC CA O aera EEE 8 22 2 Measurement of reference materials for Calibration ccccccsssssssseecccceesseeseeseceeeesaaeessees 8 22 a Processing the raw dat a eesesereneerrresereresrrrerereressrrerereressrrersreressrressreresserersreressererereressenes 8 2 2 4 Averaging and saving of measurement data cccccccsseccccessececeesececeeeceeeeeseceseeneceeseneeeeeas 9 2 2 5 Calibration of area function and instrument StIFFNESS cccccccccceessseseeceeceessaeeeeeseeeeeeeeaas 9 2 2 6 FESCUE CS SUMAN a E EE E sas 9 Zidid Predefined ADDI CAUIONS scale eciavecenacysnevateansonsancanbsaniasecsnapyseeeeteenasntee EE 9 i TIS DV aN VS N ea santos E E E E E A 11 Sols Themenu bar for data analysis ecceactessaeance easartusenanseeesetattcsatnancsseatantens NEn EASE E E rE 11 3e a 69 18 Er E eee ee en er een een re ee ee ene eres 15 3 3 im The Configuration WiINdOW c ccccccssscessecesscessecssseceascessscesecsseessaseseceasecsasersecenseesaeeens 16 3 2 1 Pet DON PEE E E E E E E ON A E EA E E A E E E 16 3 2 2 Module PaE eee E N 18 3 2 3 BURY SFE UN a gts st a E oanceeotieg aaa narmen ober aaeneeeeoncntereneeacuneoamereeeneeeonans 19 3 2 4 EET E Renee meres eee ne eer ee ee ee ee ce eee ee eee ere 22 3 2 5 Analysis Normal DaB E eisasscactoe sa cnsediranccisetviticoasswwanctieas conte sauirondesseivoeawenticosatenes seansatgnedeocevsncnncecaneuee 26
197. smec ADVANCED SURFACE MECHANICS 2 2 1 Individual configuration During start of the program certain parameters will be loaded which determine the utilization of the program A large part of these parameters is saved in Configuration Files CFG The files are normally stored in the separate directory with the name CFG Files one level below the program path Only from there they can be read automatically during the first program start Later also other directories can be used When the specified CFG file is not found during program start an error message occurs and you get the request to read a configuration file The path can then be chosen by hand Once a CFG file was chosen the software will try to read it again during every program start until you chose a different file The instrument type from which data shall be read as well as the indenter type and the parameters for the analysis are fixed in the CFG files After the first start of the program a CFG file has to be chosen which belongs to the instrument type For several instruments there are CFG files delivered together with the program which include the instrument type in their name Reading a CFG file is done using the 7 Open CFG button in the main menu Another possibility to choose the correct instrument exist in the Configuration window on the page Instrument This 3 window can be opened using the Configuration button in the main menu In the example CFG files a
198. ss and Young s modulus are automatically transferred to the Indentation force estimation window During calculation the contact area is automatically calculated using the hardness and the contact stiffness using the Young s modulus The depth is then obtained from the inverse area function The result is consequently quite accurate usually better than 2 7 2 Modelling The menu item Modelling not only allows calculation of the indentation depth at a defined force hardness and Young s modulus but also the calculation of the entire loading and unloading curve When the Average results window is open the results are automatically transferred to the Theoretical curve window This window is used for investigating the various factors which influence the shape of the force indentation depth curve The Pressure distribution selection field is used to simulate different pressure distributions on the surface They are determined by a constant pressure or the sample geometry The Power function option correlates pressure distribution with the exponents of the unloading curve With an Unloading exponent of 1 5 pressure distribution corresponds exactly to that of a spherical indenter See the following T Chudoba N M Jennett Higher accuracy analysis of instrumented indentation data obtained with pointed indenters J Phys D Appl Phys 41 2008 215407 The lower selection field is used to specify which deformation is calculated e Elastic
199. stiffness of the system in tensile tests A tensile test with the NFU Normal Force Unit is then programmed short high resolution test using NFU as only small displacements are to be expected On the Normal force unit page of the Application parameters definition window select Without approach It may be necessary to carry out the test several times in succession to enable the sample to be properly aligned to the grips The following evaluation must be performed on the uncorrected curve As instrument stiffness is corrected immediately when a data file is read instrument stiffness must be set in advance to a very high value in the Configuration window e g 1 10 written as 1E8 so that the correction is close to zero Alternatively the measured curve can also be saved as a text file directly after the measurement as it has not yet been corrected The uncorrected measured curve is not copied to the Comparison window using the button with the 115 asmec ADVANCED SURFACE MECHANICS Plus symbol ois or the text file is re imported Normal Force mN 1 000 1 200 1 400 0 200 400 600 800 2 00 1 75 1 50 1 25 1 00 0 75 0 50 0 25 0 00 Normal Displacement um Fig 119 Measured curve of a tensile test on a solid sample loading and unloading The curve is copied from the Comparison window to the Fit data window using the Fit ita button In this window the left and right hand fit ranges can be de
200. strument can be read To any Instrument belongs additionally a unique instrument stiffness function normal and lateral Data file extension DAT Second extension Instrument stiffness function Normal direction Lateral direction Function type Average instrument stiffness in normal direction mM m 2437 1 O Sinees neiaa C Compliance function Stiffness description by f Constant value f Function with up to 10 parameters f Data table Stored at 01 12 2013 Obtained from Comparison of the area functions of two different materials Comment Determined with Areafunction_Quarz_neu AREA and Areatunction_ Saphir ne waa ladent amp nalyser algorithrn Function between upper and lower force limit Data table Fit function no 5 Bie Lower force limit mM 0 001 Edit Upper force limit rit 2038 1 Coefficients x178 5939 159 14 2088 2 142 15651 x 0 3929867 Open DE ey Save in DB Fig 10 The Instrument page of the Configuration window Instrument stiffness function Here can be found the values for the average instrument stiffness in normal and lateral direction The value for the normal direction is determined during the calibration of area function and instrument stiffness and will be automatically shown here see chapter 6 The lateral instrument stiffness is normally given by the manufacturer Tabs can be used to switch between the two pages for normal and lateral stiffness 19
201. strument compliance Allow negative compliance Compliance is inverse stiffness If stiffness has already been over corrected in the measurement data this can happen especially with data from instruments other than UNAT instrument stiffness can no longer be calibrated correctly In this case it is better to use a compliance function instead of a stiffness function The over correction can be cleared using negative compliance The use of negative instrument compliance must be confirmed however as it must not occur in normal situations Use of an external area function External area function from text file Areafunction tet cal 1 he 2 sqrtta 100 asmec ADVANCED SURFACE MECHANICS If an indenter function is available which was obtained via direct measurement e g with an AFM atomic force microscope this function can be displayed directly in the graphic and it can be used to calculate the instrument stiffness This type of measurement requires a very well calibrated AFM A standard calibration using a conventional AFM is usually not accurate enough The AFM function must be saved in a text file ending in TXT There must be two columns separated by a tab in the file The first column contains the contact depth hc and the second the root of the contact area sqrt A The test file is imported by clicking on Open S button Smoothing area functions Smooth area function 1 N 2 N If calculation of the area functi
202. t Preparation window Print options page page formatting settings and print settings are performed on this page All 44 asmec ADVANCED SURFACE MECHANICS dimensions must be entered in mm Report Preparation Seo Resulta Sample Customer Print Options Top Margin Relative text line distances Data field Customer S ample Band Title Customer lines Lett Margin Aight Margin UE j5 E E I i 5 E Column Header sample lines Result lines Bottom Margin 5 aj Show in first column Filename Sample name Width Height Chart 51 135 l 76 l Max letters for file name a a a i Image file for Logo about 600150 E Delphilnspectors Version S 45MEC Logo neu bmp S Printer Setup J Print Fig 40 Print options page of Report Preparation window Relative text line distances e Band Title width in mm of the space between the title e g Results and the header e g file name of the table or enlargement of the spacing between the row groups e Column Head space between the table header e g file name and the first row of data e Values spacing between table rows data e Customer lines spacing between customer data rows e Sample lines spacing between the sample data rows e Chart Size defines the size of the graph with the force displacment curves e Width width of the graph e Height height of the graph Show in first line here you can select whether the file name or the sample name is sh
203. t force FO Ac hc Indentation hardness H as force divided by contact area under load H 1 v 1 1 2 E E is equal to the Young s modulus Clear differences can exist when pile up or sink in effects appear Indentation modulus E according to E Under ideal circumstances it Reduced Modulus vx s It is calculated from contact area Ac and contact stiffness S E _ The 2B Ac beta factor is a correction close to one It can be defined in the configuration Plain strain modulus E Poisson s ratio of sample assumption The default value for the analysis is defined in the configuration The value can also be modified in the Results window E modulus of the indenter For diamond it amounts to E 1141 GPa See J E Field and R H Telling Research Note The Young modulus and Poisson ratio of 123 asmec ADVANCED SURFACE MECHANICS diamond PCS Cavendish Laboratory Dep Of Physics Madingly Road Cambridge CB3 OHE UK February 1999 Poisson s ratio of the indenter For Diamond it amounts to ni 0 07 see reference above Martens hardness HM a force divided by real contact area 26 43 h The Martens hardness is determined from the maximum depth under applied test force It contains plastic and elastic parts of the deformation and can therefore not easily be compared with H r According to the elasticity of the materials the hardness order of Martens hardness
204. t zero The curve effectively shows how much material flow was still present in the first seconds of the hold period and how rapidly it subsides In the example in Fig 133 for fused silica the change is only around 1 2nm and shows the high resolution of the instrument s displacement measurement If no drift correction has been performed the curve will show the actual drift behavior Average results x QuarzfrB2_B2_0009 DAT Hold period after thermal drift correction 0 50 0 75 Depth Change nm 1 00 5 10 15 20 25 30 35 40 45 50 55 60 Time s Load Displacement Creep T Drift Time dependence Approach Special Results over Depth Vibration Fig 56 The T drift page of the Average results window 61 asmec ADVANCED SURFACE MECHANICS 5 1 4 Time dependence page On this page all data are shown as a function of time As well as force and displacement this may also include contact stiffness from CSM or QCSM measurements or if available additional channels e g contact resistance between indenter tip and sample The force signal black curve can be shown as e force over time e loading rate The indentation depth signal red curve can be shown as e displacement over time e displacement rate e strain rate as displacement rate divided by displacement The curves for the loading rate or displacement rate may show considerable scatter preventing clear identification of the rate In
205. th Yes Whenever this action is performed only the newly calculated functions will be saved All other data in the Configuration file will remain unchanged The saved CFG file will be set as default and used in all future software starts until another CFG file is chosen This concludes the calibration of area function and instrument stiffness Caution If the instrument stiffness is not constant the stiffness correction will influence the curvature of the unloading curve This will cause a change in the unloading exponent m from a fit with a power function However this value is also used for calculation of the area function when the variable epsilon value is being used Therefore the calculation of m and the stiffness function affect each other It may therefore be necessary to perform Steps 3 export as AREA file and 4 stiffness calculation iteratively two or three times one after the other if the stiffness function curve is more sharply bowed In such a case it is best to use a constant stiffness value fit type constant value initially as in Fig 109 and create then the AREA file and only permit a function in the second iteration 107 asmec ADVANCED SURFACE MECHANICS 6 2 Calculation using fully elastic measurement Complete deformation can normally only be obtained with a spherical indenter and sufficiently hard materials It is not possible with polymers and soft metals Surface roughness must also be low otherwise indiv
206. the Calibration gt Area function and instrument stiffness from elastic deformations menu The Indenter area function window will open Measurements on two different reference materials with significantly different Young s modulus are required if both area function and instrument stiffness are to be calibrated A Inputting data Located top right in the Read data section of the window is the Open icon Click on this to import one of the AVR files for Specimen 1 fused silica in the example and Specimen 2 sapphire in the example The correct data for Young s modulus E modulus and Poisson s ratio Poisson r for these reference materials and for the indenter diamond in this example should then be entered The values for fused silica Sapphire and diamond are already in the fields and only need to be changed if other materials are being used In the Show field the display can be selected between Load depth complete force displacement curve with loading and unloading part LD average average value for loading and unloading of the force displacement curve Sample stiffness stiffness curve calculated from the gradient of the curve Exponent local exponent of the force displacement curve required for determination of the variable epsilon value Following the calculation the following can also be displayed e Area function area function determined for one or two materials e Instr stiffness function of instr
207. the indenter can be identified must then be entered in the Indenter no field It is recommended that the number is prefixed by a letter standing for the type of indenter for instance B Berkovich V Vickers S Sphere ball nominal radius e g S10 CC Cube corner C Cone P Flat punch Configuration Mairi Hardware Instrument Indenter Analysis normal Analysis lateral Results Other indenter type Berkovich Area function no io Fig 7 Configuration window with indenter number red border The new indenter is then saved in a new Configuration file via Save CFG Here also it is recommended that the file name should begin with the indenter number followed by the date on which the file was created e g B1_2013 09 05 CFG 3 3 oiu The Configuration window 3 2 1 Main page Configuration of hardware and software is performed in the Configuration window which is activated via e menu item Configuration gt Configuration window or e Configuration button x Selected configuration file shows the name of the currently selected configuration file A configuration file contains all the correction data required for evaluation of data files including area function device stiffness type and format of results to be output but does not contain the hardware specific 16 asmec ADVANCED SURFACE MECHANICS parameters required to use the device It has the file extension CFG A CFG
208. tiffness function obtained is a straight line parallel to the force axis constant stiffness However there are frequently deviations at low forces This is to a large extent due to the deficiencies of the reference material Quartz glass for example displays a marked sink in effect at low forces which increases with the tip radius This results in over estimation of the area and hence to stiffness values which are too high This is also the reason for the upward gradient of the curve in Fig 106 towards low forces Up to 100MN a curve such as that shown in Fig 181 can still be tolerated At higher forces the line needs to be horizontal A better example with a virtually ideal curve for stiffness as a function of force is shown in Fig 107 It is highly significant that the curve runs virtually horizontally at higher forces otherwise it would not be possible to correct stiffness properly When fitting stiffness values it is therefore essential that the curve is virtually horizontal at the right end high force range and the fit curve displays no overshoots If it is not possible to achieve a horizontal stiffness curve at higher loads either the force calibration of the machine is no longer OK or there are undefined stiffness components e g due to inadequate fixing of the reference sample or the indenter tip If necessary the service should be informed and the measurement data should be transmitted 105 asmec ADVANCED SURFACE MECHANICS
209. time Scratch results 74 Surface slope fo Correct Depth limit 1 0 1 Depth limit 2 0 1 10 9 v os SB Image Fig 92 The Scratch page in the Measurement data window after correction of thermal drift 90 sasmec ADVANCED SURFACE MECHANICS The size of the drift steps can be changed with a right mouse click over the drift rate field The upper arrow keys are used to move the curves laterally towards each other if necessary Read background image allows an image of the scratch track to be placed behind the curve It should be noted that the image scale and curve scale are different It is also not always possible to show the entire scratch track in one image peansensvectvesuneensentyeasosensoed Reesecess a seuseeet Max force mN 497 818 Max distance pm 7 833 Roughness before scratch Ra pm 0 002 Rq pm 0 003 Rt pm 0 918 Rp pm 0 010 Rv pm 0 009 Average friction 0 057 Maximum friction 0 155 gt o 3 T A T E EA oo aa ANN E 5 t RES mrs a BR aS Bn Max displacement emda tes Sa etn lt R O Under load m 1 438 2 Show on bottom axis Show on left axis Q 0 75 D Distance Depth te A o 28 X pm 87 83 hm pm 0 434 Fn mN 147 150 Fl mN 3 144 u 0 021 IV Scratch depth Marks IV Pre Scan M Marks Subtract IV PostScan Marks Normal fo
210. tion Eps is further only an approximate value if there is additional plastic deformation ISO 14577 recommends therefore eps 0 75 In this program eps is calculated in a more accurate manner using the exponent of the unloading curve when this option is chosen in Configuration Analysis normal Depth of the contact of the indenter with the test piece at Fmax Elastic deformation of the surface above the contact area hs h hc Intersection of the tangent to the unloading curve at maximum force with the depth axis Permanent indentation depth after removal of the test force Permanent indentation depth after removal of the test force obtained from a fit of the unloading curve and the extrapolation to zero force This value is used for further calculations for instance for energy calculation instead of hO because it is more accurate Elastic deformation of the instrument caused by the compliance of the instrument inverse stiffness hi F Si Equivalent contact radius for pyramidal indenters A rotational symmetric contact is Ac assumed so that a T Relative elastic radial displacement normalized by the contact radius a and calculated with the formula a 0 2 v H a 2 horizontal surface and surface of the remaining indent This value is used to get a more accurate contact area with the Radial Displacement Correction The use of the Radial Displacement Correction is defined in Configuration Analysis normal COS _ a
211. tions Pre scan depth shows the shape of the surface before the scratch test In measurements with LFU this is the mean value from a to and fro scan Post scan depth is also determined via a scan with low contact force after the scratch test and gives the actual damage depth for the surface This depth can however be distorted by material adhering to the tip or material deposited in the scratch track and may need to be checked in the optical image The right hand axis Depth is assigned to all three curves Lateral force shows the measured lateral force and is assigned to the right hand axis Friction coefficient the friction value can only be shown instead of the lateral force To do this uncheck Lateral force and check Friction coefficient instead A vertical green line can also be seen in the graph This can be moved by holding down the left mouse key and dragging It is used to manually specify the point at which damage to the sample is identified or at which a delamination of the layer can be detected It may be the case that a critical load cannot be defined because there is no clear jump or kink in the curves The values for the position of the green cursor appear in the output field at bottom right e xX um position along the scratch axis with zero as starting point e hm um depth under load maximum depth e Fn mN normal force 89 lateral force friction value FI mN e u asmec ADVANCED SU
212. to the list before the start of evaluation 5 Analysis of Test Data 5 1 Evaluating hardness and Young s modulus measurements Evaluation is performed in the Average results window This window has several pages which are explained below Some functions apply to all pages of the window These can be seen at the right hand edge of the window a The meaning of the buttons Print Add graph and Save is explained in chapter 4 2 The print button is only printing the graph The complete page including graph and results fields can be printed by using the Print button in the main menu When the results field stays empty during printout please check the field Black white output in results window during printout in the Configuration window page Analysis normal Cycle In measurements with multiple loading and unloading cycles the evaluation for one of the cycles can be shown via this selection field If there is only one cycle the field is inactive EA Smoothing smoothens all visible curves on the currently visible page Press the Smooth curve button to execute Smoothing can take place incrementally in multiple steps Every time the button is pressed smoothing is increased up to the maximum of Stage 10 The current stage is shown in the field Smoothing can be undone via Reset Marks marks the position of a data point with a symbol The points are linked by a continuous line Fit marks marks the position of a fit curve data point
213. tomatically The correction type is fixed in the Configuration window on the page Analysis normal The corrected data should be saved in the program specific file formats DAA and AVR The saving is done automatically per default during averaging several measurements with equal parameters When the files have been saved a repeated correction is not necessary AVR files are also necessary for the calibration procedure asmec ADVANCED SURFACE MECHANICS 2 2 4 Averaging and saving of measurement data All data files which belong to the same sample and which have been measured with equal parameters especially equal maximum force and equal time periods can be averaged and saved in a so called average data file with the extension AVR This happens normally automatically if several data files are read at once Generally data can be saved by using the se Save button in the main menu The file type is determined in relation to the context which window is active then the button is pressed Data can only be saved in the IndentAnalyser formats It is not possible to save data in formats of other instruments than ASMEC UNAT 2 2 5 Calibration of area function and instrument stiffness In this step the previously produced AVR files from sharp indenters Berkovich Vickers Cube Corner will be used to produce an AREA file This is a special text file which contains all necessary parameters for the calculation of the area function In a dept
214. uding measurement description sample name area function instrument stiffness and other parameters This file format is generated by IndentAnalyser or IndentAnalyser software DAK temporary raw data files after correction of zero point or thermal drift They are normally deleted 46 asmec ADVANCED SURFACE MECHANICS automatically after use REF UNAT only lateral reference data file In this file measurements for the determination of lateral spring stiffness are stored which are carried out before every measurement series involving lateral force From Version 3 onwards this is only used for comparisons and documentation The spring stiffness data are now stored in the DAT file also SCN UNAT only data file of surface scans for determination of roughness or profile Any desired amount of raw data files as well as AVR files can be read simultaneously 4 2 Importing and displaying measurement data All data files are saved without instrument stiffness correction Correction takes place immediately after reading according to the formula h h C F F kor Wxor corrected indentation depth h measured indentation depth F force C force dependent instrument compliance When data files are saved this correction is canceled and only the uncorrected data are saved If data without instrument stiffness correction shall be displayed an infinite very large instrument stiffness or zero compliance must be set in
215. ulation as a CFG file click on Save CFG file pmm El Instrument stiffness function J a Read data E modulus Poisson r Sampe1 72 0 17 B 410 0 234 indenter 1140 0 07 2 500 lt lt more Fit function 8 a 2 000 Points from ig ai to 53 2l Average stiffness mN um 1608 1 Z Fit type 500 Function C Constant value 4 Presentation a Stiffness Compliance 5 000 u Show C LoadDepth C Area function 500 LD Average Instr stiffness C Sample stiffness C Exponent e Instrument stiffness Stiffness fit M Stifness M Fit 0 i Area calculation Stiffness calcul 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 Save in CFG file Force mN A d o cose Fig 112 The Indenter stiffness function window after calculation of the instrument stiffness function from elastic measurements D Repeated calculation of area function after calculation of instrument stiffness With the stiffness function now saved correctly the area function must be calculated again by clicking on Area calculation The new area function result is saved in the same CFG file The question about overwriting can be answered Yes Whenever this action is performed only the newly calculated functions will be saved All other data in the Configuration file will remain unchanged The saved CFG file will be set as default and used in all future software starts until another CFG file is chosen 110 asmec
216. ulus Poisson r D Quarz 51060m AR lv Use m2 017 D Sephir_s10 5 Bom AR lv Use 410 0 234 E hes o2z Indenter 1140 0 07 Average radius um fo Use of C Loading pat Average C Unloading part Use fit function 5 E 2 Use points from 3 to 67 i Smoothing o Marks at data Iv pA V Show legend Force mN Calculation 0 00 0 10 0 20 0 30 Displacement um 5 HED ki Close Fig 113 The Effective Sphere Radius calibration window with the measured curves for fused silica and sapphire A Inputting data Unlike the previous calibration windows in the Effective Sphere Radius window it is possible to import data from up to three different reference materials Open button The file names of the imported data files are displayed nearby In the example 111 asmec ADVANCED SURFACE MECHANICS Specimen 1 is fused silica and Specimen 2 is sapphire Specimen 3 is not used in the example If one of the data files is not used for the calculation it can be deactivated by unchecking the Use field The correct data for Young s modulus E modulus and Poisson s ratio Poisson r for these reference materials and for the indenter diamond in this example should then be entered The values for fused silica sapphire and diamond are already in the fields and only need to be changed if other materials are being used The Use of field is used to select whether the calculation is to take place only for the loading curv
217. ument stiffness or compliance 108 asmec ADVANCED SURFACE MECHANICS ISl indenter area function a a Read data E modulus Poisson r Sampei 72 fot 410 0 234 indenter Em 0 07 lt lt more Fitfunction 8 Points from fi al to J48 Load mN Show Load Depth Cc C LDAverage Cc C Sample stiffness Exponent Quarz_S10 6_50mN AVR 7 Sample 4 Saphir_S10 6_80mN AVR V Sample 2 Area calculation Stiffness calcul fel Close Fig 110 Force indentation curves of two reference materials for purely elastic measurements 0 00 0 10 0 20 0 30 Displacement um B Initial calculation of area function Calculation of the area function is started by pressing Area calculation fl indenter area function sE Read data E modulus Poisson r Sampei 72 fat bl o m faze Indenter fi 140 0 07 lt lt more Fitfunction 8 ka Pointsfrom 1 4 to 47 4 Estimated tip radius um 7 6104 Save area function eS C2 Average Square root A um Show Load Depth f Area function C LD Average gt e Quarz_S10 6_50mN AVR C Sample stiffness Exponent 4 Saphir_S10 6 80mN AVR Fit average l i ldeal tip shape V Sample 1 V Fit W Ideal V Sample 2 Ou l J Stiffness calcul 0 000 0 050 0 100 0 150 Save in CFG file hc um 5 He fe cose e Fig 111 Area function of a spherical indenter of approx 7 6um radius determined with fused silica and sapph
218. urements with increasing load stages are also possible This is not recommended however as they are usually not as accurate due to a longer measurement time and drift problems If the QCSM module is available QCSM measurements are the method of choice as they provide access to a multitude of data over depth and are also more accurate than fast hardness measurements It is recommended to use QCSM measurements up to a maximum force of 100mN and fast hardness tests for higher loads For fast hardness measurements the following loads should be used with the 2N head of the UNAT 500mN 300mN 100MN 50mN 30mN 10mN 5mMN 3mMN 2mN ImN 0 5mN If necessary Measurements over 500MN can additionally be used For measurements with the QCSM module a measurement series at 100MN is sufficient If calibration with higher loads or greater depths is required fast hardness measurements at 500mMN 1000mN 1500mN and 2000MmN can be performed It is not recommended to use QCSM measurements with these loads In the following example the determination of the area and stiffness functions on the basis of measurements on fused silica and sapphire is explained 97 asmec ADVANCED SURFACE MECHANICS 6 1 2 Second step processing the raw data The individual measurements with the same measurement sequence must now be corrected averaged and saved as an AVR file This takes place as described in Section 4 5 Only the AVR files can be used for further
219. ut by pressing the Analyse button on the Lateral F h Curve page The Lateral Data analysis window will open showing the second lateral force displacement cycle Lateral Data Analysis o Surface slope 0 3475 Correct Show Complete cycles Average of back and forth 1 00 Average cycle results over cycle number Average cycle results over cycle end time Cycle 2 to 2 of 100 1 10 Point 1 zi to 32 of 82 Point shift 0 S 41to 41 Lateral force mN Calculation for cycle 2 Average friction 0 126 Maximum friction 0 161 Minimum friction 0 108 1 40 ww Normal Displacement um Work per cycle pJ 11 761 1 50 Average displacement pm 1 367 Maximum displacement pm 1 655 1 60 j Lateral force displacement graph V Marks lv Normal lateral displacement graph jv Marks Friction coefficient WV Marks Normal force lateral displ graph lv Marks 50 40 30 20 10 0 10 20 30 40 50 Lateral Displacement um M Show legend Ew fd Fig 96 The Lateral Data analysis window with the data for the second cycle The yellow field at top right shows the surface slope This can be corrected by pressing Correct This changes the curves in both the Measurement data window and the Lateral Data Analysis window 93 asmec ADVANCED SURFACE MECHANICS Lateral Data Analysis re C fm Surface slope o o Correct Complete cycles Average of back and forth C Average cycle results o
220. ver cycle number Average cycle results over cycle end time Cyclelb to 6 lt j of 100 Point 1 j to 164 of 164 Point shift 0 l 82to 82 Lateral force mN Normal Displacement um WV Lateral force displacement graph v Marks Jj Normal lateral displacement graph Ww Marks Friction coefficient jv Marks Normal force lateral displ graph lv Marks 40 20 0 20 40 Lateral Displacement um Show legend A Fig 97 The Lateral Data Analysis window with the data from two cycles after slope correction The Lateral Data Analysis window allows detailed analysis of each individual cycle plus display of the average cycle results over the cycle number or the time Change the number of cycles in the Cycle to fields to switch to a different cycle or show multiple cycles Increasing the number of cycles in the left hand from field will force an increase in the right hand to field if the number is the same If the number in the right hand field is higher more than one cycle is being shown The same principle applies if the number in the right hand cycle field is reduced The start and end points of a cycle can be changed using the Point fields below the Cycle fields After the first click on the Average cycle results button of the Show field calculation of the average values for all cycles will begin This may take some time The results will be saved Clicking on the radio button again will not cause the calculation to be
221. verage drift rate from hold periods use an average value for the drift rate in measurements which include multiple hold periods during the test Default depth range for back extrapolation nm defines the indentation depth for data points which are used for extrapolating back to zero force The value should lie between 20nm and 7Onm An elastic contact Hertz contact is normally assumed This means that the force displacement curve is described with an exponent of 1 5 according to the dependency F C h h0 28 asmec ADVANCED SURFACE MECHANICS 40 Inm Default depth range for zero point back extrapolation Instrument stiffness compliance correction and Area function calculation Instrument stiffness complance conection Area function calculation f Use data from present configuration f Use data from present configuration C Use data stored in data file if availalble 0 Use data stored in data file if availalble The correction curve values stored in the current Configuration file are used as default for evaluation of data files Use correction data from configuration However if data files are received from other users and the associated Configuration file is not present it will not be possible to evaluate the data correctly In this case it is better to use the Use correction data stored in data file option Since IndentAnalyser Version 2 the correction data valid during the measurement have been stored in the data file itself
222. ween the linear fit and the hold period data points 53 asmec ADVANCED SURFACE MECHANICS Click on OK to apply the drift correction to the data or on Cancel to discard the results When OK is pressed for the first time the window changes and the corrected load displacement curve is shown Correction of thermal drift can be performed by hand in this window using the arrow buttons or the arrow keys on the keyboard Each click changes the drift rate by a defined amount usually 0 005nm s The step size of the drift rate can be altered by clicking on one of the arrow buttons with the right mouse key This feature is particularly useful for fully elastic measurements where you know that the loading and unloading curves should match In this way the use of a hold period is not necessary which reduces the measurement time The Back button sets thermal drift correction to zero Click on OK to definitively perform zero point correction or on Cancel to discard the results Thermal drift correction for QuarzfrB2_B2_0009 DAT I Era 100 90 Graph 1 Average rate nm s 0 0894 80 Use average rate Reset 70 Drift rate nm s 0 1955 a Hold period number f a Fit accuracy nm 10 1158 50 5 eo gt 40 4 Use Marks fe All C All 30 C None None 20 10 M Fit curves j A V Legend 0 0 2 0 4 0 6 0 8 Displacement um Cancel Normal Fig 49 The Thermal drift correction window after OK has been
223. wer force range is now sought by changing the thermal drift rate Drift rate and shifting the unloading curve Unloading curve shift by very small amounts 0 1 10nm The results for drift rate and the unloading curve shift are shown in the associated fields 80 asmec ADVANCED SURFACE MECHANICS fal Average results Dgr eo 6 DP33_ 510 2 70mN AVR s Smoothing 0 24 22 Reset 20 J Marks 18 Fit marks 16 2 E 14 s isson s rati T ample Poisson s ratio 0 2 T 12 Drift rate nm s 0 088506 JH 10 Unloading curve shift nm p i Find optimum ejos l 2 Calculation 0 IV Show fit 1 0 000 0 020 0 040 0 060 0 080 0 100 0 120 0 140 i Show fit 2 Displacement um M Show error band Load Displacement T Drift Time dependence Special Fig 83 The Average results window for the special type of cyclic measurements It is also possible to perform both corrections manually using the blue arrow keys Press the Up or Down keys to shift the curve with the unloading points to the right or the left The standard step size is 0 5nm This can be modified by clicking on the arrow keys with the right mouse key A pop up menu opens in which the step size can be selected Drift rate nm s 0 076661 Unloading curve shift nm EE Find optimum kit p Step inm s 100nm Step 0 5nm s 50nm Ka i Step 0 1Inm s 10nm Fi Step 0 05nm s Snm Step 0 0inm s inm e Step 0 005nm
224. window is also where you specify whether and how corrections are to be carried out For both Zero point correction see section 4 3 and Thermal drift correction see section 4 4 there is a choice between manual correction automatic correction no correction By default the correction method set in the Configuration window is used but this can be changed here 55 asmec ADVANCED SURFACE MECHANICS Using automatic correction is recommended Only if a warning regarding correction appears in the Status window should manual correction be used to find the cause Press Start correction Start correction begin When the correction has been performed the button Start analysis changes to Start Analysis id and the color of the button changes also Pressing the button again opens the Average results window or a similar window to present results If automatic zero point or drift correction has already been performed pressing for manual correction will cause corrections of all data files to be reset and the button will change back to Start correction The same thing happens if extra data files are added or additional curves are clicked in the Data overview window If the evaluation has been successfully the message AVR Files saved DAA File s saved will appear in the bottom left hand field of the window when the Save options have been selected During averaging the agreement of the different curves with equal test parameters i
225. with the mouse in a text or Excel file Save All saves all values in the table including the statistics table if present in a text or Excel file 38 asmec ADVANCED SURFACE MECHANICS Open allows table data to be re imported in text format This enables data tables to be expanded at a later time Clear T deletes the entire table and removes the statistics table Hi H E nz 3 946910 72 15620 0 170 d21 4 177 5 Delete Row 10 eee ee 4 31 Delete Columns 4 8 9 Copy to Clipboard 4 AAT AY ATTA CTT TT YATRA Delete rows select fields in one or more rows and right mouse click Select Delete rows Delete columns select fields in one or more columns and right mouse click Select Delete columns Copy to the clipboard Select individual or adjacent fields right mouse click on the selected fields and select Copy to Clipboard Rearrange rows and columns the arrangement of rows and columns can be changed to adapt presentation to your own requirements To move a table row up or down select an item from the row and click on the t Up or Down button The arrangement of the columns can be changed by dragging the column header with the mouse The column selected is shown by a bold line F H h 10 004 2210 0 140 10 004 0 140 2210 30 009 25 06 0 257 30 009 0 257 25 0E 50 013 2480 0 340 50013 0 340 24 80 100 023 24 07 0 493 100 023 0 493 24 07 300 157 23 93 0 886 300 157 0 886 23 93 500 216 22 24 1 155
226. xce Fig 18 Area function database window 25 asmec ADVANCED SURFACE MECHANICS Open DB opens the Area function database window It permits access to all area functions belonging to an indenter The top area only shows the datasets which belong to the selected indenter type The lower area only shows the datasets which belong to the indenter with the number selected above All parameters can be modified in this window Caution usually the area function is determined as part of a calibration procedure If the coefficients are changed here this can result in incorrect test results 3 2 5 Analysis Normal page The Analysis normal tab is for settings which are relevant for data evaluation of measurements performed with the Normal Force Unit NFU This refers in particular to correction of test data and calculation of hardness and Young s modulus Configuration a Main Hardware Instrument Indenter Analysis normal Analysis lateral Results Other Fit range Get contact stiffness from athe ai fe Fit range of unloading curve 2 of Fmas Start 98 i End 40 m pee ou Folynomial fit Fit range for thermal drift correction 7 of tmas Start 25 End 100 S C S2 Power low fit Hardness and modulus calculation Epsilon factor Beta factor 1 0 recommended i Default sample Poisson s ratio 0 25 f Constant Oh vaide W With radial displacement corection recommended Default pile up correction fact

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