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1. 17 4 Method Selection Introduction The methods used in TestWorks are under several headings depending on the system and material used in testing These headings are Indentation UTM Scratch and Polymer Methods This section of training will walk you through reviewing data from a couple of these methods There will not be a differentiation between reviewing methods in the XP and DCM mode because the results of the methods are formatted the same in both cases Objectives The user will be able to o Usethe PDF file associated with the method to investigate the purpose input requirements and the applicable materials for the method o Usealist of descriptions for test methods to determine which might best fit their testing needs 18 Using PDF files for Method Selection In the methods folder inside the TestWorks program file every method has a pdf file describing the method inputs results and material applicability Each method has some unique features that will be described in the pdf file The following exercise helps the user investigate unfamiliar methods Accessing the methods folder it is suggested that the user create a short cut to this location Go to My Computer gt Program Files gt MTS Systems gt TestWorks gt Methods Exercise Investigate an unfamiliar method We will use the method XP Basic Hardness Modulus at a Depth 1 Using the method s associated pdf file
2. 2 Running Your First Batch Introduction For the first time user learning a new program can be a daunting task This section is designed to get you moving fast In this section the user will go through testing a sample and reviewing the real time and post test data Objectives By the end of this section the user will be able to O O O Load a batch of tests Change the data that is displayed on the real time graph Add meters to the Test page Review the sample post test Print a Sample Summary report with any edits 10 Loading a Batch and Starting the Test The following steps walk the user through loading a batch of tests from the TestWorks Training files and testing a sample at five locations using either the XP CSM Standard Hardness Modulus and Tip Cal indentation method or the XP Basic Indentation method to a penetration of 2000nm 10 Mount one of your samples the user may want to start with testing fused silica to the aluminum sample pucks and load it into the sample tray Then load the sample into the instrument and close the cabinet Details on mounting samples and loading the sample tray can be found in Section 11 Commonly Used Procedures Open TestWorks and log into your account Open the method XP Basic Hardness Modulus and Tip Cal at a Depth In the top menu bar click on Mode and select Batch Mode Right click in the Sample Name Display Window the right most panel a
3. Scratch Testing Many parameters affect the results in scratch testing Given the parameters are kept constant between tests the results can provide very meaningful comparison data Objectives After completing this section the user will be able to O O Understand the parameters involved in scratch testing Chart the test flow process of the scratch test Review scratch data using standard review channels Understand the makers associated with scratch testing Output the data to Excel 45 Some scratch tests parameters Scratch speed 0 1um s 2 5mm s Scratch length 104m 500mm Maximum lateral force 250mN All orientation Maximum Lateral force resolution 2uN Noise level 300 uN without contact lateral force Scratch orientation 0 360 Required inputs for scratch test Starting Scratch load Maximum Scratch Load Scratch length Scratch velocity Cross Profile Location Profiling Velocity Load Applied during profiling The Standard Scratch Test Four phases composed the scratch test l A first profile of the surface is realized by applying a very small load equal to Load Applied during profiling 20 uN for example in order to have the original morphology of the surface before the scratch Then along the same path the normal load is increased from Starting Scratch Load 0mN for example to Maximum Scratch Load 500mN for example A last profile is realized by applying a very smal
4. Where Famp is the forcing amplitude hamp is the displacement amplitude is the phase shift K is spring constant m is the equivalent mass of the system o is the damping of the frame and K is the frame stiffness Following this measurement the elastic modulus of the sample is determined using equations 3 and 4 above Hardness The hardness of the sample is determined using Equation 1 above A more detailed description of the calculation of hardness and modulus is provided in Section 8 of the User s Manual 75 Method Modification Introduction As a professional user with creator privileges several aspects of the method can be modified The user has the option to disable test segments and add formulas that determines the value of a test at a given index point averages the values of a channel between two points returns a channel value based on the input of another channel and determines the channel value of a marker Objectives Upon completion of this section the user will be able to o Create formulas that determine the maximum or minimum values for a given channel o Create a function that determines the Load Applied on Sample at a penetration depth of 200nm o Create a formula that averages the load applied to the sample during the Thermal Drift Correction segment o Create a formula that determines the value of a channel at a given marker 76 Menu Options for Method Modification In the Edit Met
5. 11 12 13 Choose Specific Value and fill in 200nm Do not designate a marker for this item you would designate a marker if you wanted to see the location on the review graph Click OK At this point the channel index for the location of 200nm has been determined and now we need to determine the value of the load applied to the sample at this index Choose Create Formula again from the Edit Method menu under Method Choose Value at Index Point Function enter the display name as Load at 200nm and click OK In the dialog box choose Load On Sample for the Channel choose 200nm Index for the Index Point and click OK Notice that the Load at 200nm has appeared in the results The Value of the Reduced Modulus at the Maximum Load 14 15 16 17 18 Under the Method menu in the top bar select Edit Method and select Create Formula Choose Channel Value Function enter the display name Reduced Modulus at Max Load and click Create The Modulus at Max Load is determined by the point at which the stiffness is greatest Therefore set the following inputs i Channel Reduced Modulus ii Search Channel Stiffness iii Select Peak Maximum iv Start Index Surface Marker Click OK Notice that the Reduced Modulus at Max Load is now a result 7o get units of GPa on the re
6. 54 Table 5 Cross Profile Parameters Scratch Total Height Of Residual Pile Up Width the Groove Scratch Depth Height um nm nm nm 11 436 1022 487 707 45 315 037 11 181 1011 799 681 098 330 701 11 184 1019 878 684 457 335 422 11 506 1017 199 692 183 325 016 Mean 11 413 1019 941 694 831 325 111 Std Dev 0 242 6 142 12 867 8 245 COV 2 12 0 6 1 85 2 54 1 2 3 11 756 1028 344 708 966 319 378 4 5 It is important to remember that these parameters are measured at a normal load specified by the user in this example the parameters were measured at the point in which a normal force of 5mN was applied to the surface during the scratch segment The user should note that the cross profile will not provide any useful information if it is performed past the Critical Load The Scratch Width refers to the distance between points O and P It has been observed and documented that there is very little horizontal elastic recovery during a scratch test therefore this parameter is a good representation of the plastic deformation that takes place during the scratch segment The Total Height of the Groove refers to the average vertical distance between the points G and P and the points G and O This height is the depth of the after the scratch has been completed and includes the height of the Pile Up on the edges of the scratch caused by the indenter the pile up is represented by
7. Loading Samples section above Go to the Tools menu item and select Microscope to Indenter Calibration newer versions of the software have access to the Microscope to Indenter Calibration from the video microscope panel At the window verify the site you have chosen for the calibration and click on Yes A series of five indentations will be made by the XP one at each corner of a square with a single indentation in the center When the stage returns to the microscope the cross hairs should be directly centered on the indentation in the center of the square A message will display for you to find the indents Do NOT click OK Move the dialog to the side and use the video handset to locate the red cross hair over the center indentation Now press OK Another dialog will be displayed indicating that the calibration is complete 62 Changing the Objective Objective lenses for the Nano Indenter XP optics system are mounted on precision slides so that they can be interchanged easily Parcentricity adjustment of the objectives is also enabled by these slides so that each objective can be aligned and interchange can be accomplished without a need to re find positions A picture of the microscope objective mounted on the slide is shown in Figure 1 Figure 1 Microscope objective mounted to the slide To remove the objective 1 Grasp the objective 2 Slide it out of the mounting rails
8. To insert an objective 1 Grasp the objective turn the slide so that the side labeled Front faces out of the gantry 2 Insert the slide into the mounting rails on the microscope until it snaps into place 63 Changing the Workspace from XP to DCM Mode 1 Open TestWorks and click the icon in the bottom right corner that indicates XP mode Figure 1 Basic hardness Mosli mmm rs ay KE tere NJ Click the XP icon to switch to the DCM mode Figure 1 Workspace mode icon 2 At the dialogue box asking if you really want to switch the work space modes of operation Click Yes 3 THIS IS A VERY IMPORTANT STEP Place the locking pins in the XP head Major damage may be caused if the XP head is not pinned when the cable is disconnected The pinned head is shown in Figure 2 Figure 2 Locking pins correctly inserted in the column 4 At the dialogue ensure that the pins are placed in the XP head and click OK 5 Atthe dialogue box asking the user to shut down all of the electronics and plug in the DCM head click OK and close TestWorks and shut down all of the electronics 6 Unplug the head cable and plug it into the DCM slot shown in Figure 3 64 XP Head Location _ i Figure 3 Head cable locations 7 Start up all of the electronics open the TestWorks program and select a DCM method You are ready to test 65 12 Appendix 66 Basic Indentation Processes I
9. e S UM E MTS A NANO INSTRUMENTS TestWorks Professional Training XP Document Number D3416 XPA 13112 0 Product Class Nano Indenter XP Product Title TestWorks Professional Training XP Project Type Software Training Author Bryan Crawford Date 11 06 2006 Distribute to MPJ BC KHP WCO JLH JS Document Introduction This document is to be provided along with the XP User s Manual This document provides training for the TestWorks and Analyst software e 4 i z NANO INSTRUMENTS e Professional TestWorks Training for MTS Nano Indentation Systems Open the possibilities Table of Contents 1 INTRODUCTION 2 RUNNING YOUR FIRST BATCH LOADING A BATCH AND STARTING THE TEST FUNCTIONS ON THE TEST PAGE REVIEWING THE INDENTATION DATA 3 SETTING UP USERS IN TESTWORKS CREATING A USER AND DEFINING THEIR ACCESS LEVEL 4 METHOD SELECTION UsiNG PDF FILES FOR METHOD SELECTION 5 RUNNING TESTS AND SETTING UP BATCHES SETTING UP AND SAVING BATCHES RECALLING AND RUNNING A PREDEFINED BATCH 6 THE REVIEW PAGE EXPLORING THE REVIEW PAGE CHANGING SURFACE CONTACT LOCATIONS COMPARING MULTIPLE SAMPLES IN TESTWORKS CHANGING INPUTS POST TEST REVIEW PAGE MENU OPTIONS 7 ENSURING QUALITY FUSED SILICA DATA PROPERTIES OF FUSED SILICA AND TROUBLE SHOOTING OPTIONS 8 USING ANALYST TO PERFORM A TIP CALIBRATION COLLECTING
10. 0 25 At the prompt check Do not show this message again and click Close Hit the recalculate sample button calculator with 3 dog bone specimens Again in the panel with the test numbers right click and select Select All Tests Note the new value of the average modulus What is the percent change From the main menu select File then Print Preview then Sample This automatically launches Microsoft Word and shows the report Scroll down to the table titled Calculation Inputs and note that the value used for Poisson s ratio is reported there Close TestWorks Note that different methods have different calculation inputs that may be modified post test The procedure for modifying these is always the same Modify the value and then recalcu late the sample The values for the calculation inputs that may be modified by the user are always provided on the printed report and in the exported Excel file Review Page Menu Options Table 2 Table shows a list and description of the menu options available on the Review Screen 2 Menu Options Available on the Review Screen to get these options right click in the designated panels Test Panel Left Most Panel Submenu Option Options Description Select all Tests NA Selects all of the available tests for the sample 29 Deselects all of the available tests for the Deselect All Te
11. Channel Data This selection displays the collected data for all of the data arrays for a selected point on the graph 8 Select a data point on the graph and use the arrow keys to move around 9 When the tests have finished running and all changes to the sample have been made print the sample from the File drop down menu 13 3 Setting Up Users in TestWorks Introduction Users can be defined to restrict access to certain methods and to certain options available in the TestWorks interface This allows the administrator to define access levels to methods and require certain training to take place before that option or method be made available to the user This would be especially important in a large facility where multiple testing functions such as indentation with the XP and DCM heads scratch tests and tip changing are taking place Objectives By the end of this section the user will be able to O O O Add a new user to TestWorks that requires an entry password Limit the accessibility of a user Change the Access level of a method Specify new directories for data storage Limit the functions available to the user 14 Creating a user and defining their access level 1 Launch TestWorks and Click OK at the User Login screen or login as the administrator 1f passwords have already been set up and open any method 2 From the top menu bar select the User menu then click on the Us
12. Folder in the files XP Basic Silica and XP CSM Silica respectively Export this data to Excel using the Excel menu option Calculation of Tip Area Coefficients Using Analyst Open the program Analyst and press the Calculator icon in the main menu Save the project as Tip Cal Tip Name and Date From the main menu select Tools then Calculate Tip Area Coefficients In the dialog box titled Select Tip Sample Data make the following selections a Sample Fused Silica 37 b Displacement Data Displacement into Surface c Load Data Load on Sample d Stiffness Data Stiffness select Harmonic Contact Stiffness for CSM data e Ifthe CSM method was used for data collection leave the box labeled Stiffness data is from CSM checked otherwise uncheck the box Click OK At the dialog box titled Tip Coefficient Lead Term enter the value supplied with your diamond tip or it the value is unknown enter 24 5 Then press OK When the dialog box titled Load Frame Stiffness and Area Function Calibration has appeared press the Go button For more options in tailoring the tip area function to your needs see the description of the advanced options listed below or seepage T 102 in the User s Manual Print the fitted coefficients that make up the tip area function These values must now be entered into TestWorks Plotting Fractional Differences i
13. Sample Tray Mount your sample onto a Sample Disk Slide your Sample Disk into the Sample Tray and snug down the set screw using the appropriate sized allen wrench 5 Turn the sample mount system upside down onto a clean and flat surface Loosen the set screws and allow the samples to adjust to the height of the side rails Then retighten the set screw Do Not mount samples higher than the side rails on the Sample Tray this can cause the sample to crash into the indenter head Turn the Sample Tray upright and carefully slide it back into the dovetail rails in the instrument Running Samples 1 Open TestWorks and Login 2 Select a method for testing your samples 2 oL 3 Click on the Batch Mode icon located in the main menu bar 4 Enter the Define page to setup your testing parameters 5 Use the Next Step button to navigate through the setup process If you do not know what the input value should be do not worry the methods are developed using standard default input values that work well for many samples 6 Return to the Test page and press the Play button the big green arrow in the middle of the screen 86 Is Your Fused Silica Data OK Run Fused Silica data every time you test samples with a Berkovich tip this ensures quality control and helps to track the performance of your instrument In addition if your tip calibration is off you can calibrate your tip a
14. THE DATA CALCULATION OF TIP AREA COEFFICIENTS USING ANALYST PLOTTING FRACTIONAL DIFFERENCES IN ANALYST ENTERING THE NEW TIP AREA COEFFICIENTS INTO TESTWORKS ADVANCED OPTIONS DURING A TIP CALIBRATION 9 USING ANALYST TO REVIEW INDENTATION DATA 10 11 12 13 14 15 18 19 22 23 24 25 26 27 28 28 29 CREATING A REPORT TO COMPARE MULTIPLE SAMPLES 10 SCRATCH TESTING SOME SCRATCH TESTS PARAMETERS REQUIRED INPUTS FOR SCRATCH TEST THE STANDARD SCRATCH TEST SEQUENCE OF THE SCRATCH TEST REVIEWING SCRATCH DATA ON THE TESTWORKS REVIEW PAGE READING SCRATCH RESULTS IN EXCEL 11 COMMONLY USED PROCEDURES MOUNTING AND LOADING SAMPLES CHANGING AND CLEANING THE XP INDENTATION TIP PERFORMING A MICROSCOPE TO INDENTER CALIBRATION CHANGING THE OBJECTIVE CHANGING THE WORKSPACE FROM XP TO DCM MODE 12 APPENDIX BASIC INDENTATION PROCESSES SURFACE FIND TEST SEGMENT SURFACE APPROACH INPUTS IN TEST METHODS STANDARD LOAD AND UNLOAD METHOD CONTINUOUS STIFFNESS MEASUREMENT CSM INDENTATION PROCESSES METHOD MODIFICATION MENU OPTIONS FOR METHOD MODIFICATION CREATING NEW FORMULAS FOR ANALYSIS LOAD APPLIED TO THE SAMPLE AT 200NM INTO THE SURFACE THE VALUE OF THE REDUCED MODULUS AT THE MAXIMUM LOAD AVERAGE LOAD DURING THERMAL DRIFT CORRECTION THE VALUE OF THE LOAD AT THE START OF THE HOLD FOR THERMAL DRIFT COMMONLY USED PROCEDURE POSTERS SELECTING A METHOD LOADING SAM
15. a new location 30 Rather than using this option it is recommended that the user clicks and holds on Loading the graph and box in the section of the graph Zoom Segment for zooming Gridlines NA Adds or removes the gridlines on the graph Only displays tests data with lines If there are not two or more points than no lines will Line Display Lines Only appear Lines and Points Uses lines and points to display data Points Only Only uses points to display the data Legend NA Adds or removes the legend on the graph List of Channels Allows the user to select the data displayed on Y Axis Channel Available the Y Axis List of Display Allows the user to select the units displayed on Y Axis Units Units the Y Axis List of Channels Allows the user to select the data displayed on X Axis Channel Available the X Axis List of Display Allows the user to select the units displayed on X Axis Units Units the X Axis Defines the data displayed and the axis scales Properties New Page for the graph Print NA Prints the Image Copy to Clipboard NA Copies the image to the clipboard Save Image NA Saves the image to a file Save Review Page Allows the user to save a set display of panel Configuration NA for reviewing data Load a presaved display of panels for reviewing tests The user may have to reset the Load a Review Page properties for the graph after switching Configurat
16. and elastic moduus E as a continuous function of 1 XP CSM Standard Hardness Modulus and T ip Cal penetration into the test surface Load using a conetant strain rate User spexifias dyneric fraquancy amplitude strain rate end maximum penetration depth This is our most popular method Similar to 1 vath fever usar inputs Good for first time users i be CSM Heriess Modus for Thin Fi Simia to 1 wn defaut irputs optimized or tena thin ns especial 4 XP CSM H and E using Const Disp Rete Similar to 1 but loading occurs et a constant displacemert rete With nenapositioning accuracy method automatically indants scans the XP CSM NP Auto Inert and Scan impression then repeats for the next test No user interaction requred from test to test Indentation is performed using the same algorithm es for 1 With nanopositionimg accuracy method performs an indentation using the XP CSM NP Pteractive Indent same alaorithm as for t1 2 D cH a With nanopositioning accuracy allows interactive 2D surface imaging XP CSM NP iteractive Scan scans Used to tune scan settings before using 5 5 6 8 XP 3D Prafilomatr Similar to 6 but allows imaging of much larger areas Returns Hand E vs penetration depth using a series of test in which paak force is reraduced at each new test site Constant bading rete force S XP Basic T ip Cal application User sets loading tima max loads and hold times Orignaly for bp calibrat
17. can be fixed during the calibration procedure If the tip has large tip rounding 7500nm or if the tip is ill defined fix the modulus of the fused silica Do not fix both values at the same time Min max depth for the calculation of E assuming perfect area this is the min max depth for which the assumption of perfect tip area is valid This value is usually well past the tip rounding and well less than the maximum depth limit of the tip Min max depth for area function calculation does not use the data outside of this range for the generation of the tip area function Determines the number of coefficients used in generating the tip area function Use as few coefficients as possible to attain a quality area function for the tip The more coefficients that are used will create larger errors during when indenting to large depths and extrapolating the area function These parameters are used in cases where the frame stiffness has not been calibrated in TestWorks Field installed instruments have been calibrated and the user should not have to use these parameters It is recommended that the Fix Value box stays checked Beta and epsilon are geometrical constants that should be determined before a tip calibration 1s performed Beta is 1 for any circular projected contact area and takes on different values for other geometries Beta for pyramidal geometries is approximately 1 07 Epsilon is determined empirically form the Oliver Pha
18. click on the Graphical display panel and select Y Axis Channel this option lists all of the possible channel selections Select Load on Sample All of the tests are displayed and can cause confusion Therefore right click in the left most panel and select Deselect all Tests Then click on an individual test number make sure that you click on the actual number so that the test highlights in blue This allows crosshairs to appear when you click on the graph if the Tracking and Crosshairs selections are checked to check these items right click in the graphical display panel 12 Now right click on the right most panel and select Raw Channel Data This option allows you to view the values of any channel at any point on the graph 26 Click in the Graphical Display and use the arrow keys to move the crosshairs over data points and see how the channel data changes 13 Finally right click in the Graphical Display Panel and select Line Display This brings up a menu letting the user select line styles Select Lines Only Notice the graph now shows a continuous smooth line 14 Take a few moments to look through some of the other menu options Changing Surface Contact Locations Sometimes during an indentation experiment an event will happen that will make the instrument falsely detect the surface a person might bump the cabinet or an environmental vibration may occur In this case the indentation data will appear to
19. hardness value the modulus at a depth of 200nm will be determined Next the average Load over Stiffness Squared will be calculated between 100nm and 300nm Finally the load applied to the sample will be determined at the minimum calculation value The method file used from the TestWorks Training folder in this exercise is l iii ii iv XP Basic Hardness Modulus at a Depth Open TestWorks and login Under the Method menu select Open Method and open the method titled XP Basic Hardness Modulus at a Depth msm in the XP methods folder Select Method from the main menu and save the method as XP Modified Basic Tip Cal Take a moment to examine the review page There are a few values that are not listed in the results that could be of interest these values are The load applied on the sample at a depth of 200nm The value of the reduced modulus at the maximum load The average load on the sample during the hold segment for thermal drift correction The value of the load at the start of the hold for thermal drift Load Applied to the sample at 200nm into the surface 4 Under the Method menu in the top bar select Edit Method and select Create Formula Choose Index Point Function and enter the display name as 200nm Index Click Create In the Point Formula dialog box choose Displacement into Surface for the Channel Surface Marker for the Start Index 79 10
20. indenter is completely unloaded and the next test is started If the next test site is less then 100um away the surface find will not be completed again Comments on how the hardness and modulus are calculated for the Load and Unload method Hardness The hardness is calculated at the maximum load as the Load divided by the projected contact area between the indenter and the sample as detailed in Equation 1 the projected contact area is determined using the Oliver and Pharr method 1 P ar 1 70 Elastic Modulus The elastic modulus is calculated using the data from the unloading portion of the indentation test As the load on the indenter is withdrawn the rate at which the load with respect to displacement changes determines the stiffness of the material as shown in Equation 2 Q Where S is the stiffness P is the load and h is the displacement into the surface This stiffness allows the determination of the reduced elastic modulus the combined response of the indenter tip and the sample by the following relationship in Equation 3 I Vr S E 2 3 B 2 JA Where f is a geometric factor of the tip S is the stiffness of the material and A is the projected contact area determined using the Oliver Pharr method 1 Since the properties of the indenter are well characterized the modulus of the sample can easily be determined from the following relationship in Equation 4 kaa eal amp rs zi S
21. s L Where E is the reduced elastic modulus v and E are the samples Poisson s ratio and elastic modulus respectively and v and E are the indenters Poisson s ratio and elastic modulus respectively A more detailed explanation of the modulus and hardness calculations can be found in Section 4 of the User s Manual 71 The basic loading and unloading curve with the stiffness calculation Load P vs Displacement into the Surface h 72 Continuous Stiffness Measurement CSM Indentation Processes This method produces the hardness and elastic modulus as a continuous function of displacement into the surface of the sample in addition to the elastic modulus and hardness at the maximum load Load After the final surface approach the indenter is pressed into the surface of the sample at a constant strain rate the default strain rate is 0 05 1 s to a depth determined by the user During the loading cycle a 2nm oscillation is imposed on the indenter at a frequency of 45 Hz with the XP head and 75 Hz with the DCM head these are default values and they can be changed by the user Hold The indenter is then held at a constant load for a time specified by the user and the CSM function is turned off Unload The sample is unloaded by 90 of the tests maximum load Hold for Thermal Drift Determination The load is held constant at 1096 of the tests maximum load Then the correction for thermal drift is deter
22. the aluminum puck then the sample can be epoxied to the slide This mount is shown in Figure 2 Using this process the sample can easily be discarded after testing is completed simply heat the mount to 70 degrees C and remove the glass slide Many adhesives can be used to affix the samples to the pucks Figure 1 Sample mount The sample is mounted to the glass slide with epoxy which 4 and the glass slide is mounted to the puck using Crystal Bond Slide your Sample Disk into the Sample Stage and snug down the set screw using the appropriate sized allen wrench as shown in Figure 3 Figure 3 Fixing the sample in the Sample Stage 5 Turn the sample mount system upside down onto a clean and flat surface as shown in Figure 4 Figure 4 Turn the Sample Stage upside down onto a clean surface 6 Loosen all of the set screws and allow the samples to adjust to the height of the side rails Then retighten the set screw Do Not mount samples higher than the side rails on the Sample Tray this can cause the sample to crash into the indenter head 7 Turn the Sample Stage upright and carefully slide it back into the dovetail rails in the instrument as shown in Figure 5 58 Figure 5 Slide the Sample Stage back into the dovetail rails 59 Changing and Cleaning the XP Indentation Tip The following procedures will walk the user through changing and cleaning the XP indentation tip A schematic of the tip holding system is shown
23. this ensures quality control and helps to keep track of the performance of the instrument Objectives Upon completion of this section the user will be able to o Identify problems in fused silica data o Troubleshoot problems that might be causing poor results on fused silica 33 Properties of Fused Silica and Trouble Shooting Options 1 In the Review page ensure that the fused silica data looks clean and tag any outlying tests Trouble Shooting Check for good surface detections using the Load vs Displacement slope or the Harmonic Contact Stiffness vs Displacement graphs If the data is scattered and it appears that there are many false surface finds perform a microscope to indenter calibration in single crystal aluminum and rerun your tests this usually will clean off any debris that may be adhered to the tip 2 Right click in the Graphical Display panel and change the Y Axis channel to Load Over Stiffness Squared Ensure that the data flattens out to a value between 0 00135 and 0 00152 the tail of the data should not trail up or down Trouble Shooting If the data is around the correct value but trails up or down adjust the Frame Stiffness and the Harmonic Frame Stiffness only with CSM in the right most panel of the Review page under Inputs Editable Post Test Adjust these values in increments of 10000N m for CSM systems adjust both frame stiffnesses at the same time and by the sam
24. PLES IS YOUR FUSED SILICA DATA OK 42 45 46 46 46 46 53 57 58 62 63 64 66 83 84 85 87 1 Introduction Welcome to the first level of TestWorks training This manual has been created with years of experience in training customers It will introduce the new user to the different screens of TestWorks main menus ways to run tests and how to review data The manual is set up to walk the new user through the following steps 1 Running Your First Batch of Tests 2 Setting up TestWorks for a lab with multiple users 3 Understanding the basics in indentation testing and selecting methods for testing 4 Running indentation tests and reviewing data 5 Running scratch tests and reviewing scratch data 6 Performing basic functions to ensure quality data collection 7 Modify methods to tailor testing to the user s needs Every concept will be presented as an exercise that will present different functionalities useful to the user By the end of this training the user will be able to run tests review results and make sure that instrument is performing well This manual is written so that anybody can go through the training with minimal supervision The objectives of each section are listed below Running Your First Batch O O O O O Load a batch of tests Change the data that is displayed on the real time graph Add meters to the Test page Review the sample post test Print a Samp
25. age When the test starts running the instrument will find the surface of the sample and pause until the thermal drift of the sample and system drops below 0 05nm s After this criterion is reached the instrument will continue with the test due to temperature differences in the room this process can take some time to settle out The first step in the test after the pause is a surface approach At this time the indenter approaches the surface of the sample at the test location The next exercises will walk the user through monitoring the tests l When the test has started after the Approaching Surface dialogue box has disappeared right click in the Graphical Display Window The menu in this window allows you to choose the X and Y axis data arrays for display on the graphs The X and Y Axis Channels display all of the available data arrays that are available for viewing during the test The default display is either Modulus vs Displacement into Surface or Load on Sample vs Displacement into Surface For practice change the graphical display to Load on Sample vs Time Right click again on the Graphical Display window and choose Properties Go through the tabs at the top of the new window and examine the contents of each page Using these options the user can change the properties of the graphical display Exit the Properties window right click on the meters that are displayed on the bottom of the screen and cho
26. be skewed The following exercise will show how to manually change the surface location for a test so the data is not wasted This exercise will use the same TestWorks sample file from the previous exercise Basic Load Unload Data 1 Select and highlight only Test 2 in the test panel and plot Load vs Disp Slope vs Time on Sample 2 Setthe graph s Y and X axis to have limits of 50 to 200 and 50 to 50 respectively 3 Notice that the graph starts out level and then quickly increases around zero Click and hold to drag a box around the point of contact make this box large enough that some pre and post contact data is visible 4 Click on one of the data points to display crosshairs that allow tracking The Surface marker is currently at 156N m change the surface location to about 70N m by placing the crosshairs on a data point that has a Load vs Disp Slope around 70N m and typing the S key on the keyboard 5 Move the surface location around to a few locations and watch how the results change 6 Close TestWorks and do not save the sample 27 Comparing Multiple Samples in TestWorks In the next exercise two indentation sample files will be compared in the TestWorks Review page The sample files that are used in this exercise are 10 Sample 3 mss Sample 4 mss Open TestWorks and select Open Sample from the file menu Open the folder 1 TestWorks Training and selec
27. ble 3 each individual scratch test is labeled in the left most column and the top row labels several scratch parameters You can divide this table into two sections The first sections circled in red are the columns Critical Load and Penetration Depth at Critical Load these columns describe parameters linked to the fracture of the sample These parameters circled in red are determined during the actual scratch test and represent measurements made at the critical load marker The second section circled in blue are measurements made on the cross profile The location of the cross profile is specified by the user The location is given by a specified normal load that is reached during the scratch segment in this example these parameters were measured at the point where a normal load of 5mN was applied to the surface 1 Pa 3 4 5 Both sections of this table are described individually in detail below In the summary you will find a set of bullets to help you quickly identify the parameters Red Parameters Critical Load and Penetration Depth at Critical Load Table 4 shows only the parameters circled in Red these parameters are the measurements taken during the actual scratch segment 53 Table 4 Results linked to the fracture Penetration Depth At Critical Load Critical Load m Mean Std Dev COV N nm 22 42 3761 66 20 905 3565 371 The parameters i
28. box You can click on the Browse button to locate the desired method 15 6 Select the Password option and type in the requested user password and click OK 7 Under the Directories tab select Browse beside the Data Directories text field and enter user s name onto the end of the current text Repeat this step for the Export Directory tab These steps will create a folder specific to the new user and store data into their file 8 Select the Properties tab and check all the options that apply to the user Now you can log out and let the user log back into TestWorks for their own testing experience Note that the access level of a method can be changed by a creator under the Edit Method selection under the Method menu Changing the Access Level for a Method In TestWorks select Method in the menu bar gt Select the Edit Method gt Configuration Items gt Select the Miscellaneous option gt the first option on the screen is the Access Level Exercise Defining a User e that has the highest privileges for method access and data manipulation and e for whom the preferred method XP CSM Standard Hardness Modulus and Tip Cal is automatically loaded at logon and e that has a password of NanoMan and e for whom all samples are stored in a specific subdirectory 1 Launch TestWorks 2 At the User Login prompt cli
29. ck OK 3 From the main menu select User then Users 4 Click New 16 5 Under User Name type Joe 6 Under Method Access Level select 9 7 Under User Privilege select Creator 8 For post login action select Load Default Method 9 Select the method XP CSM Standard Hardness Modulus and Tip Cal which should be in the directory C Program Files MTS Systems TestWorks Methods 10 Click the button Password Enter the password NanoMan as requested and click OK 11 Select the Directories tab 12 For both the data directory and the export directory create a new directory for the user by clicking browse beside the text boxes and adding Joe to the end of the existing text 13 Select the Properties tab and check everything that you can 14 Log out by selecting User then Logout from the main menu 15 Log on as the new user by selecting User then Login from the main menu At the User Login prompt select Joe and enter the password NanoMan You will note that the desired method is automatically loaded 16 Close TestWorks From now on whenever you log on as this user the preferred test method will automatically be loaded and all data will be stored in the personalized folder within the Samples folder For more information on defining users search TestWorks help under User Configuration
30. e actual surface of the sample If nm many false surface are indicated in testing increase this value Surface Approach Sensitivity Increases or decreases the sensitivity of the surface find A lower number indicates a more sensitive surface find but can also 76 Surface Approach Velocity trigger due to environmental noise The velocity of the indenter during the surface approach starting nm s from the surface approach distance location Approach Distance to Store The distance away from the reference surface location that data is nm recorded 69 Surface Standard Load and Unload Method Find and This method produces the hardness and the elastic modulus at one particular depth PUB dee Approach Load Once the final surface approach has detected the surface the loading is completed at a constant loading rate to a given depth this is a user input Hold The system then holds a constant load on the sample for a time specified by the user Unload Then the system unloads the indenter at the same rate used during the loading Unload 90 segment until it reduces the maximum applied load to the sample by 90 Hold for Hold for Thermal Drift Correction Thermal During this hold segment the system pauses and corrects the data for thermal drift the Pun default time for thermal drift correction is 60 seconds Complete Unload Complete Unload and Start the Next Test The
31. e edges User sets all load targets 14 XP High Load Basic Hardness Modulus Load Control Similar to 10 but uses high load option for max load up to 1kg 15 16 18 19 zjxPFeatreShaem Sd to detemine the lateral force required to break a MEMS feature 9 XP Basic Tip Cal List some of the most commonly used methods below along with their results and the materials that apply to them Method Results amp Materials 21 5 Running Tests and Setting up Batches Introduction Running indentations has never been easier using the batch wizard to set up and save batches allows the user to load standard methods and run them with ease In this section the user will set up indentation tests and learn how to recall batches of indents for standard tests Objectives Upon completion of this section the user will be able to o Setup batches of tests o Save standard batch formats for quick test set up o Recall batches to for quick test set up 22 Setting up and Saving Batches This Exercise walks the user through setting up and saving standard batches Use the batch wizard to set up and save a batch of ten indents that use the method XP Basic Hardness Modulus at a Depth Each individual test should go to a maximum depth of 750 nm 1 Launch TestWorks 2 At the User Login prompt click OR 3 Load the method XP Basic Hardness Modulus at a Depth 4 Click the button for Batch Mode button looks
32. e the advanced options in the tip calibration dialog box to tailor the tip area function to their testing needs 36 The following exercise can be performed using either the XP Basic Tip Cal method or the XP CSM Standard Hardness Modulus and Tip Cal the latter of the two uses the CSM option to perform the tip calibration Exercise In this exercise the user has the option to run fused silica data or to use example data from the 1 TestWorks Training folder To run fused silica data start with Step 1 under Collecting the Data If sample data is to be used open TestWorks and select Open Sample from the file menu In the folder labeled 1 TestWorks Training select either XP Basic Fused Silica Data or XP CSM Fused Silica Data Then continue to Step 4 under Collecting the Data Bes ppc n Collecting the Data Open TestWorks and login From the method menu select Open Method Open either the XP Basic Tip Cal msm or the XP CSM Standard Hardness Modulus and Tip Cal msm methods and complete 25 indentations spaced 50 microns apart in fused silica using the default input values for the method and name the sample Fused Silica When the method has finished running review the data and check for any tests that may need to be tagged All of the silica data should look very clean and free of outliers An example of silica data is given for both the Basic approach and the CSM approach in the TestWorks Training
33. e value Usually a negative frame stiffness correction pulls the data tail down and a positive correction pushes the tail up Should this problem persist consider recalibrating the frame stiffness by adjusting the current amount by the correction amount If the data is not at the correct value call NanoTech 865 425 0566 to talk to a service professional 34 3 Check that the results for the elastic modulus and hardness of the fused silica sample are between 69 74GPa and 8 5 10 5GPa respectively Trouble Shooting Ifthe average results are not within these ranges perform a tip calibration and recalculate the batch using the new tip area coefficients Call an application engineer or NanoTech if problems persist 35 8 Using Analyst to Perform a Tip Calibration Introduction During testing it is recommended that the user run the fused silica sample to ensure that the instrument is running well and the tip calibration is correct When the silica data is clean and the data simply indicates incorrect elastic moduli and hardness values this is an indicator that a tip calibration should be preformed This section walks the user through the process of a tip calibration Objectives The user will be able to o Complete a tip calibration using fused silica as a reference material o Compare the tip area coefficients to the ideal area required for a modulus of 72GPA by using the Fractional Difference function in Analyst o Us
34. ers sub category 3 Click New to add a new user Type in the users name and select the appropriate Method Level Access Each method has a designated access level from 0 to 9 The user must have an access level equal to or greater then the methods access level in order to obtain access to the method 4 Under User Privilege select the appropriate description Privilege Level Description Operator An Operator can run tests and enter the values of inputs that are required by the test method Tester Can run tests and enter values of inputs that are required by the test method The tester can also examine method properties but can not edit the method Editor An Editor can not access the Define page and edit test method settings The Editor can disable or enable test segments Definer A Definer can access the Define page and add or delete test segments from a basic set of test segments A Definer can also add delete basic data channels inputs and formulas Creator A Creator can access the Define page and add or delete test segments inputs formulas basic data channels and formula channels 5 For post login action select the option in the combo box that will determine what dialog will appear after the user has logged in If you have selected Load Default Method as the Post Login Action then type the desired method name into the Default Method text
35. hod selection under Method in the main menu several options are available for editing the current method Table 5 shows the options under the Edit Method selection and describes what each option allows Table 5 Edit Method Options the user can access these options through the Method selection in the main menu Option Submenu Description Global Units Allows the user to select the unit system for results Test Flow This option brings up a new page for the user to review the test flow and examine each test segment Under the test flow the user can enable or disable test segments This is especially useful if the user wants to disable the automatic printing of test results at the end of the test flow Configuration Channel Allows the user to examine all of the channels Items definitions formulas units and export order Formulas Allows the user to examine all of the Formula definitions formulas and result order Inputs Allows the user to examine all of the Inputs definitions and default values Miscellaneous Change method access levels and method descriptions Excel Output Configuration for exporting to Excel Configuration Hardware Status Defines the action that the instrument will take if the Status item takes place during testing To select one of the actions check the box 77 Limit Detection This configuration item monitors when any of your data chan
36. ill be able to O O O Navigate the review page Change the graphical display options Review two different samples in one TestWorks file Change input values for a sample that has already run 25 Exploring the Review Page The file used from the TestWorks Training folder in this exercise is 10 11 Basic Load Unload Data Open TestWorks and login In the file menu select Open Sample Open the folder labeled 1 TestWorks Training and select the Basic Load Unload Data file After the file opens select the Review tab Right click in the left most panel that contains the test numbers and select the option Select all Test This option allows you to review all tests at once Notice that the modulus is reported at a particular depth Each indentation results in one value of the modulus and hardness at one particular depth Also notice that tests 1 and 14 are outliers in the data Right click on Test 1 and select Tag Test This option will exclude the test from the data statistics at the bottom of the panels Which Other test might you tag to reduce the covariance in the data Right click on the Graphical Display Panel and select Properties Deselect the auto scale option at the bottom of the Y axis and set the lower limit to 0 then click OK The Properties Table allows you to adjust the display graph to represent the properties in a whole array of configurations Right
37. in Figure 1 Ideen Steet kieser Tip Tae gt Mondesies Stadt Slee ju 9 lxs Tip x Raring Collar Figure 1 Tip holder schematic 1 Before changing the tip Make certain the indenter head is parked and the locking pins are placed in the indenter column this is to prevent damage to the system The inserted locking pins are shown in Figure 2 This is very important Figure 2 Locking pins correctly inserted in the column 2 Using the tip change tool dock the change tool with the tip collar Gently dock the tip change tool with the retaining collar so that the collar fits between the collar remover flats illustrated in Figure 3 A gentle counter clockwise motion applied to the removal tool will extract the collar and tip from the shaft when the tool is properly docked to the retainer collar 60 CA Y Figure 3 removal of the indentation tip Remove the tip from the tip holder using a pair of tweezers always handle the tip by the Indenter Tip Tab To clean the tip continue to Step 4 to install another tip go to Step 5 Two methods of cleaning the indentation are recommended Both methods use Methyl Ethyl Ketone MEK to clean the diamond off MEK is recommended because it does not leave a film residue on the tip The first way to clean the tip is to saturate a q tip with the cleaner and wipe the diamond clean An alternative cleaning process is to use an ultra sonic cleaner this method is the
38. ion use has broadened Returns Hand E vs penetration depth using mubpk badunbed cycles at 10 XP Basic Hardness Modulus T ip Cal Load Control aah test site Constant loading rate force application Usar sats bad tima max load and number of cycles Ww xPBasiccCreep Returns the stress exponent for creep using a long hoki segment 12 XP Basic H and E et a Sarias cf Displacements Apples a pre Ioad ful load than ratums to pre load post load Returns 13 XP Edge Deformation Test Step Load the difference in penatration between pre and postioad Popular for testing razor blade edges Liser sets ell load targets 14 XP High Load Basic Hardness Modulus Load Control 15 18 Standard Scratch with Cross Profile Performs a controllad scratch with pre end post test profiling 17 Standard Scratch with Cross Profile and Lateral Force Like 16 but LEM option gives lateral force dunng scratch 18 XP ISO 14577 Berkovich or Vickers Test and analysis according to ISO 14577 Part 1 19 z xPFeatreShem Sd to detemine the latera force required to break a MEMS feature 4 To setup your tests simply click on the Batch Mode icon in the main menu and enter the Define page which will walk you through the setup 84 Loading Samples SER es ae 1 2 3 6 7 In the TestWorks program right click in the Tray Position panel and select Load Sample Tray Remove the
39. ion NA configurations Delete a Review Deletes a configuration of panels from the page Configuration NA Review Page Configuration Channel Data and Inputs Panel Right Most Panel Edit NA Allows the user to edit the values and formulas 31 of inputs formulas and channels Adjusts the ordering of the Reported Inputs into Input Results Order NA the method Formulas Results Adjusts the ordering of the Reported Formula Order NA values from the test Results NA Displays the results from the method Displays the data that corresponds to the Raw Channel Data NA selected points on the Graphical Display Required Inputs NA Displays all of the Inputs into the method Displays the Inputs that can be changed after testing has been completed After changing this Inputs Editable Post value the user must recalculate the entire Test NA sample to apply the change to all of the tests Statistics Channel Bottom Panel Allows the user to define the statistical analysis Configure Statistics performed on the data List the most commonly used menu items for indentation testing below and be aware of what they accomplish Menu Item Description What panel is it in and What does it Do 22 7 Ensurin uality Fused Silica Data Introduction The user should run fused silica data every time samples are ran using a Berkovich indenter tip
40. is already open and notice that the graph that was just created has been added to the project summary Return to the Analyst program 9 Create a bar graph that compares the Hardness of the two materials over the defined range this range was defined in TestWorks before exporting the data to Excel a Right click on the Word Projects in the left panel and select add Bar Chart Under the heading Results select H Average Over Defined Range Select both samples and click OK Notice that once again the graph is duplicated in the Excel file summarizing the results 10 Create a Sample level plot for the Load On Sample versus Displacement into Surface for each thin film sample a Right click on the sample Thin Film Sample 1 in the left panel and select add X Y Graph Choose the appropriate quantities for the X and Y axes and select all of the tests Choose Loading Segment for the Start Test Segment selection box in the lower right corner you are going to limit the graph only to the data in the loading segment Choose Loading Segment for the End Test Segment selection box in the lower right corner Click OK 43 f Notice that this plot is located in the Excel file Thin Film Sample 1 xls Since this is a sample level plot it is stored in the sample file it is not created in the project file Thin Film Summary 44 10 Introduction
41. l and choose Output to Excel This will automatically open Excel and export the results and some channel data to an Excel file 4 From the main menu select File and Open Sample Open the folder 1 TestWorks Training and select the file Thin Film Sample 2 Export this data to Excel 5 Launch Analyst from the Program File from the MTS TestWorks folder 6 Click on the Calculator icon across the top menu bar 7 Atthe prompt enter a project name Thin Film Summary and save the project in your folder After clicking Save Analyst will calculate the sample and create a new workbook that summarizes the samples 8 Create a Project level plot that compares the Moduli as a function of displacement into the surface of the sample a Right click on the word Project in the left window and choose add X Y Graph b In the pop up window set the X Axis to Displacement into the Surface and the Y1 Axis to Modulus c Highlight both Samples listed If no samples are highlighted Analyst assumes that the user wants to graph all of the samples Therefore it will 42 h not make a difference if you highlight the two samples or leave them both unhighlighted Click OK Right click on the graph and choose Edit Graph Notice the available options on the tabs Create a new title and format the axes if needed Change program windows to the Excel project file Thin Film Summary this file
42. l load equal to Load Applied during profiling 100 uN to measure the residual deformation in the groove Finally a cross profile gives the shape of the section of the groove and helps evaluating the plastic deformation The cross profile is done along the scratch at the point that experienced a load equal to Cross profile location for example 5mN during the scratch Sequence of the Scratch Test 46 Surface profile 20uN Position 0 700um Normal load pied Ru Max profile 20 uN Position Pre scratch 0 100 600 700um profile Normal load Residual profile 20uN Position 0 700um Cross sectional profile Tangential E Force 47 Cross Profile Scratch direction A Cross profile on a scratch realized with a Berkovich indenter face forward The cross profiles are done to estimate the plastic deformation 48 Steps in a Standard Scratch Test Surface Find Original Morphology Profile Scratch with Ramp Loading Post Profile Cross Profile Reviewing Scratch Data on the TestWorks Review Page All of the options that are related to the review screen after an indentation test are the same options that are available in all of the other test methods After a scratch test there are a few options that make reviewing the data a bit easier which should be listed below To export the results and other testing parameters to Excel select Excel from the top men
43. le Summary report with any edits Setting up Users in TestWorks O O O Add a new user to TestWorks that requires an entry password Limit the accessibility of a user Change the Access level of a method Specify new directories for data storage Limit the functions available to the user Method Selection o Usethe PDF file associated with the method to investigate the purpose input requirements and the applicable materials for the method o Usea list of descriptions for test methods to determine which might best fit their testing needs Running Tests and Setting up Batches o Setup batches of tests o Save standard batch formats for quick test set up o Recall batches for quick test set up The Review Page o Navigate the review page o Change the graphical display options o Review two different samples in one TestWorks file o Change input values for a sample that has already run Using Analyst to Review Indentation Data o Import samples into Analyst by creating a summary workbook o Understand the structural levels of the Analyst program by creating sample level and project level graphs o Generate graphs using different formats Using Analyst to Perform a Tip Calibration o Complete a tip calibration using fused silica as a reference material o Compare the tip area coefficients to the ideal area required for a modulus of 72GPA by using the Fractional Difference function in Analyst o Usethe advanced options in the tip calibra
44. like 3 groups of dog bone specimens in a folder 5 Click the Define tab This brings you to the batch wizard 6 Read the blue prompt before the Next Step button Click Next Step to initiate the wizard 7 Read the blue prompt Click Next Step 8 Read the blue prompt Ensure that the option Start A New Batch is selected Click Next Step 9 Read the blue prompt Select the first two options Click Next Step 10 Read the blue prompt Click Next Step 11 Under sample name enter Test Sample Remember you will have the option to modify this name before running the batch Click Next Step 12 Read the blue prompt Leave all values at default Click Next Step 13 Read the blue prompt Leave all values at default Click Next Step 14 Read the blue prompt Edit the required inputs as follows Set Depth Limit to 750 nm Set Poissons Ratio to 0 25 Click Next Step 23 15 16 17 18 19 20 Read the blue prompt Click on the center of the center circle Click Define array of tests beginning at this location Enter 5 indents in the X direction and 2 indents in the Y direction for a total of 10 indents Use an indent spacing of 30 microns in both directions To save this configuration so it is assessable for future indents click Save As and save the array as 5 X 2 30um Spacing For future indents of this configuration simply select this op
45. located in the same directory as the method itself See Above answer the following questions e What is the basic purpose of the method e What hardware is required e Are there any types of materials for which this method is not appropriate Now we will use information within the method itself to learn more First do the following 2 Launch TestWorks and login 3 Open the method XP Basic Hardness Modulus at a Depth and click OK 4 Click on Method in the main menu bar select Edit Method and then select Configuration Items Note that there are formulas inputs and channels then many other selections Click on input on the right hand side of the screen Then select one of the Display Names Use the tabs in the bottom window to explore the input Click on the Description tab to view a text description 19 5 Using the text descriptions answer the following questions e What do the inputs Delta X For Finding Surface and Delta Y For Finding Surface mean How do they affect the test e What does the input Perform Drift Test Segment do e What does the formula Drift Correction mean e What is in the channels Displacement Into Surface and Load on Sample 6 When you have finished close TestWorks Note All released methods have an associated pdf file and internal text descriptions to help you learn when and how to use the method Table 1 lists the available methods along
46. mined Complete Unload and Start the Next Test The indenter is completely unloaded and the next test is started If the next test site is less then 100um away the surface find will not be completed again Comments on how the hardness and modulus are calculated for the CSM method Modulus The displacement oscillation during the loading segment is used to monitor the phase shift and amplitude difference between the excitation force and the material response In 73 the figure below the applied oscillation is shown imposed over the loading curve this is an example loading curve used to emphasize the oscillation Loading Curve Displacement Oscillation Nominal Force Nominal Force r Excitation Force 80 60 40 va 20 P can i Dr 0 40 60 80 100 Time seconds Time seconds The excitation force and the displace response are shown for elastic and viscoelastic materials below Elastic Material Viscoelastic Material 2 1 zu pul D oO 27 A M uy zt N Saat le N loss me 3 8 o D a o A Oo i 0 os x O f o 9 E amp 5 amp 4 E ES 3 5 E 2 1 1 1 1 E 3 1 1 1 1 3 0 10 20 30 40 50 10 20 30 40 d Time milliseconds Time milliseconds Using the phase shift and the material response the stiffness of the material is determined from the following Equation 5 S 5 F 4 cos K mo amp 74
47. n Analyst After generating the tip area coefficients in the Analyst program a new entry shows up in the Y Axis field when the add Y X Graph is selected under Projects this new entry is fractional differences When plotted against Displacement into Surface this provides the user with the fractional difference between the tip area required for a modulus of 72GPa at the given depth and the tip area function generated by the curve fit For more information on fractional differences see the section Performing a Tip Calibration in the Analyst program Help files B oe VU oq Entering the New Tip Area Coefficients into TestWorks Select the opened TestWorks program Select Tip in the main menu and choose Configure Tip At the Configure Tip Parameters dialog box click the Add button Name the tip using the Tip Number and Current Date Then click OK 38 In the parameters section enter the modulus for the tip material the default value for modulus is the modulus for diamond Enter in all of the tip area coefficients from the print out and press OK Let the sample recalculate and save your sample 39 Advanced Options During a Tip Calibration Fixed Values Min Max Depths Modulus Cal Function Cal Number of Coefficients Load Frame Stiffness Parameters Analytical Model Constants Curve Fit Weighting The modulus or the tip Lead Term
48. n Table 4 correspond to measurements made at the critical point marker C on previous plot for each scratch test These results help to understand at what load the fracture occurs in the material and at penetration fracture happens During a Scratch Segment the load is ramped up to a maximum load 50mN in this example over a specified distance from point b to point d 500microns in this example The Critical Load column in the table refers to the normal load applied to the surface at which fracture occurs the position of the critical load is marked C in the above penetration curve In addition the penetration depth is provided in Table 4 at the critical load Fracture occurs when the material starts cracking or tearing Optical images can be reviewed to verify the position of fracture After the Scratch Segment is completed an additional profile is taken to determine the Residual Deformation left by the Scratch Segment both the Scratch Segment and the Residual Deformation curves are plotted on the same graph for ease of comparison Fracture is usually determined graphically by small jumps in the penetration curve Blue Parameters Scratch Width Total Height of the Groove Residual Scratch Depth and Pile Up Height Table 5 shows a list of only the parameters in Table 3 that are circled in blue these parameters are the measurements taken after the scratch segment is complete and refer to the cross profile provided above
49. nd quickly recalculate the data 1 In the review page ensure that the fused silica data looks clean and tag any outlying tests 2 Check that the results for the elastic modulus and hardness of the fused silica sample are between 69 74GPa and 8 5 10 5GPa respectively 3 Right click in the Graphical Display Panel and change the Y Axis channel to Load over Stiffness Squared Ensure that the data flattens out to a value between 0 00135 and 0 00152 the tail of the data should not trail up or down 87 88 Document History Version Effective Date Supersedes Change Date Release 11 06 2006 Release N A 89
50. nd select Load Batch When the selection dialogue box opens find the TestWorks Samples file and open the folder labeled 1 TestWorks Training the flow for finding this folder is below Local Disk C Program Files MTS Systems TestWorks Samples TestWorks Training Select either Standard CSM Test Batch bch select this one if the instrument configuration has the CSM option or the Basic XP Test Batch bch Press the Play Big Green Arrow button and at the dialogue box replace Sample 1 with the sample name and press OK Right click in the Video Image box that appeared and select Nano Handset this allows fast positioning of the sample stage Click on the sample puck that corresponds to the sample location so an outline of the microscope cone is located over the position Right click again and select Move to Target this will move the selected position under the microscope Right click in the Video Image box and select Nano Video Handset Use the up and down arrows in the lower left of the video image to adjust the focus of the microscope the large arrows focus fast while the small arrows focus slowly The Microscope Light Source is externally located usually in close proximity to the keyboard Using the mouse place the red crosshairs over a clean part of the sample and click OK Now the tests are running 11 Functions on the Test P
51. nels exceeds the minimum or maximum value that you have preset Common limits are low high load limits and low high extension limits Sample Report There are two Report configuration items one for samples and one for specimens Your settings control how the report will be printed once you have selected either Print Sample or Print Specimen respectively Tag Limits The Tag Limits dialog establishes limits on the value of the specimen data or results The specimen will be tagged if the specimen data or results exceed one of the limits Tagging a specimen means that the specimen will be marked with a yellow tag icon and its data will not be used in statistical comparisons Units The Units dialog allows you to customize the Units category such as SI MKS or English that will be used for all channels formulas and inputs within a test method Create Formula Formula Builder The Formula Builder provides a quick and easy way to create formulas for use in your TestWorks methods To use the Formula Builder select the type of formula you wish to create in the Choose a Formula Type list box 78 Creating New Formulas for Analysis In this exercise several formulas will be explored The objective of this exercise is to use formulas to provide new results First the minimum value of hardness over the calculation range will be determined Following the determination of the minimum
52. ntroduction During the standard indentation processes there are several basic actions that take place These steps differ between the load unload method and the CSM method because of fundamental differences in obtaining the stiffness of the material This section will explain the basic indentation process Objectives The user will be able to o Understand the Surface Find and Surface Approach test segments along with the required inputs associated with this integral part of the test o Create a flow diagram of the processes involved in the standard Load Unload and CSM methods o Describe the two techniques used for determining stiffness during an indentation test 67 Surface Find Test Segment Surface find test segment a proper surface find is critical for accurate data The surface find test segment is completed during the first test on a sample or when the tests are located over 100um apart not all tests require a surface find Both methods with or without CSM start with a surface find in which the indenter approaches the surface of the sample at a high rate of speed well removed from the actual test location the default value for the approach location is 50um in the x and y directions from the testing location The second part of the surface find is a slower approach in which the system better characterizes the surface location This second surface find is completed at a location that 1s 5096 closer to the actual test site than
53. ose Properties Examine the available options available on this screen Notice that meters can be added or deleted for display and the appearance of the meters can be changed 12 Reviewing the Indentation Data 1 When the one or more tests have completed click on the Review tab located under the main menu icons 2 On this page the user can review the indentation data as other tests are being conducted Select one of the tests in the left window Click on the number to highlight it in blue this allows tracking and cross hairs display of the highlighted graph 3 Ifthere are any tests that are outliers right click on the test number and select Tag Test this option eliminates the from the statistical calculations Tagging a test does not eliminate the data 4 On the Graphical Display panel right click and choose line display Notice that there are three choices in for displaying the lines change this selection to lines and points when examining lots of data and the computer is moving very slow the lines only selection will produce faster graphs 5 Display the graph Load on Sample vs Displacement into Surface 6 Examine the Editable Inputs in the right most panel These inputs can be changed and the sample can be recalculated to reflect the updated information to recalculate the sample click on Tools in the main menu and select Recalculate Sample 7 Inthe far right panel right click and choose Raw
54. preferred cleaning process Put a couple of inches of water in the ultra sonic cleaner then place the tip in a coffee mug with enough MEK to cover it then place the coffee mug into the water Let the cleaner work for about 10 min Load the tip retaining nut into the tip change tool Place the tip into the tip retaining nut using a pair of tweezers and holding it by the Indenter Tip Tab The beveled edge of the tip holder indicates the front edge of a pyramidal tip a pyramidal tip can be positioned edge or face forward Using the tip change tool carefully align the Indenter Tip Tab into the Indenter Shaft Slot Align the threads and tighten the collar clock wise back into the XP head Ensure a snug fit but do not over tighten 61 Performing a Microscope to Indenter Calibration The microscope to indenter calibration is used to establish the relative positioning between the microscope and indenter so that when properly calibrated the indentation will be performed at the site chosen while the sample was under the microscope and after the indentation is performed under the tip the site of the indentation will be returned to a point directly under the microscope Different versions of the software allow different options for the microscope to indenter calibration To perform a microscope to indenter calibration l 2 Ensure that the single crystal aluminum is correctly loaded into the sample tray per the
55. r is determined after the critical load The user should also examine the scratches optically to help clarify what type of fracture simple cracks delamination might have occurred The parameters circled in red on Table 2 show the values of the Critical Load and the Penetration Depth when fracture occurs It should be noted that scratch testing is used only for comparative results In addition the parameters used for scratch testing are very sensitive to change therefore the user must ensure that testing parameters remain consistent For more information on scratch testing see section 8 Scratch Testing in the user s manual 56 11 Commonly Used Procedures Introduction This section introduces the procedures for common operations of the instrument hardware If there are any questions on these procedures please contact NanoTech before trying to complete the task Objectives After reading this section the user will understand how to Mount and load Samples Change and clean XP indentation tips Perform a Microscope to indenter calibration Change the microscope objective Change the indentation workspace OO0o00 0 57 Mounting and Loading Samples l 2 3 On the Test page in the TestWorks program right click in the Sample Tray Position panel and select Load Sample Tray Remove the Sample Tray Mount your sample onto a Sample Disk It is recommended that a cut microscope slide be affixed to
56. rr model and is 0 72 for conical tips 1 for flat punches and 0 75 for a Berkovich tip This slide bar allows the user to weight the area function for smaller or larger depths 40 9 Using Analyst to Review Indentation Data Introduction This section of the tutorial demonstrates how to export data to Excel and compare sample using Analyst Analyst is a program developed by MTS Nano Instruments that acts as a front end interface allowing easy creation of graphs and comparison analysis of samples With every workbook creation in Analyst the user creates an Excel workbook that contains all averaged data for each sample and the comparison graphs that are created Objectives At the end of this section the user will be able to o Import samples into Analyst by creating a summary workbook o Understand the structural levels of the Analyst program by creating sample level and project level graphs o Generate graphs using different formats 41 Creating a Report to Compare Multiple Samples The following exercise demonstrates the comparison of two thin film samples using the Analyst program The files used from the TestWorks Training folder in this exercise are Thin Film Sample 1 mss Thin Film Sample 2 mss 1 Close all open programs 2 Open TestWorks and login From the File menu choose Open Sample and select Thin Film Sample 1 mss from the 1 TestWorks Training folder 3 In the main menu select Exce
57. s fracturing This marker can be moved e Move the C marker and look at the results change at the bottom of the review page e Look at the residual penetration and the maximum penetration during the scratch e These channels can be plotted on their own Try to look at the original shape of the sample by plotting original morphology vs scratch distance e Plot the cross profile contours cross profile topography vs cross profile distance 51 Cross Profile Topography nm Cross Profile Distance um Markers used on the plot 1 Beginning of the cross profile 2 End of the cross profile O Top left pile up P Top right pile up G Bottom of the groove 52 Reading Scratch Results in Excel Table 3 shows the standard tabular results from a scratch test after exporting the data to Excel Each column of data will be described individually Table 3 An Example of Scratch Results Exported to Excel ul ro nad f Penetrat Critical dani Scraten Total Height Of Residual Tom Load M 9 Width the Groove Scratch Depth nm 3761 66 3565 371 23 061 3777 928 nm nm nm 1022 487 707 45 315 037 Y 1011 799 681 098 330 701 11 756 1028344 708966 319378 23 115 3848 831 11 184 1019878 684457 335422 21 506 3639 657 DEM EUN EE 22 202 3718 689 A Nas 1019941 694 831 325 191 Std Dev 0 973 114 067 6 142 12 867 COV C 3 07 T 1 85 In Ta
58. sts NA sample Tags the test and keeps the data from entering Tag Test NA into the calculation for the statically data Recalculates the test based on new values entered into the Editable Post Test Inputs or calculated formulas and software channels Recalculate Test NA entered into the method definition Recalculates the all of the tests based on new values entered into the Editable Post Test Inputs or calculated formulas and software Recalculate Sample NA channels entered into the method definition Displays warnings taken during testing and View Warnings NA review Displays the time data and user information about the sample setup In addition this shows the method information and the time individual Properties NA tests were started Clears all of the channel data for that specific Delete Curve Data NA test Delete Test NA Deletes the test from the sample Delete All Tests NA Deletes all of the tests from the sample Delete All Tagged Tests NA Deletes only the tests that are tagged Graphical Display Panel Center Panel Resets the graph to the setting defined by the Reset NA Properties menu Crosshairs NA Displays Crosshairs on the graph Allows the crosshairs to move with the arrow Tracking NA keys or mouse over data points Adds test to the graph The user can click and Add Text drag the text to a new location Adds an arrow with text to the graph The user Arrow can click and drag the arrow to
59. sult complete the following selections i Select Method from the main menu ii Select Edit Method iii Select Configuration Items 80 iv Vi vii viii ix Select Channels Click on Reduced Modulus under Display Names In the lower portion of the dialog box click on the button Units Class Select Stress for the Class Under Type select GPa Click OK in each dialog box to exit Average Load during Thermal Drift Correction 19 Under the Method menu in the top bar select Edit Method and select 20 21 22 23 24 Create Formula Choose Average Value Function enter the display name Average Load During Thermal Drift Correction and click Create Make the following selections in the Formula Builder i il iii iv Click OK Result Channel Load on Sample Select Use Index Points Markers Point 1 Start Drift Marker Point 2 End Drift Marker Notice that the Average Load During Thermal Drift Correction has now been added as a result Change the default value of the input Do Drift Hold When Load Below so that the method always completes a thermal drift correction The steps for completing this change are below i ii iii iv v vl Select Method from the main menu Select Edit Method Select Configure Items Select Inp
60. t the sample file labeled Sample 3 mss After the sample loads open the Review Page Right click in the Test panel the left most panel and choose Select all Tests Review this data as you like and then go onto step 5 to import another sample for comparison Select File from the main menu and choose Import then choose From TestWorks 4 Sample Click the Advanced button and open the 1 TestWorks Training folder from the Samples folder the flow for finding this folder is listed below Local Disk C Program Files MTS Systems TestWorks Samples 1 TestWorks Training Select the file labeled Sample 4 mss and click Open Notice that all of the tests in Sample 4 appeared in the Test column Take a moment to look over all of the buttoned options Click the button Select All and press OK Wait a moment for the calculations to finish and right click in the Test Panel the left most panel to select all tests Changing Inputs Post Test l 2 Login to TestWorks From the File menu choose Open Sample and open Sample 4 mss that is located in the folder labeled 1 TestWorks Training Go to the review page 28 10 11 In the panel with the test numbers right click and select Select All Tests Note the value of the average modulus In the Editable Inputs panel change the Poisson s ratio to
61. the fast surface find When the second approach detects the surface the system then waits for the thermal drift to stabilize below a given value the default thermal drift is 0 05nm s Then the Surface Approach Test Segment starts and the final approach takes place at the test site at a rate designated by the Surface Approach Velocity From this point on the two indentation processes differ The diagram below shows the Surface Approach Segment Surface AX for Surface PUDE NN Surface find Asproadiadd pproach Tes Test Location Segment AY for Surface Slow surface find and hold find for thermal stability Surface Find ex Fast Surface Find Test Segment Surface Find Test Segment 68 Surface Approach Inputs in Test Methods When setting up a test after the sample name has been entered a section of questions will appear relating to the surface find The following table should clarify the elements of the surface find Surface Find Inputs Description Delta X for finding the Surface um Delta Y for finding the Surface um The X distance away from the indent location where a surface find is conducted The Y distance away from the indent location where a surface find is conducted Allowable Drift Rate nm s The acceptable drift rate for conducting the indentation test Surface Approach Distance The distance above the reference surface location in which the instrument will start to look for th
62. the mounds under points O and P The Residual Scratch Depth refers to the depth of the scratch into the surface This parameter differs from the previous Total Height of the Groove because it does not include the height of the Pile Up The residual scratch depth is measured by the vertical distance between the surface and point G Pile Up Height refers to the height of the mounds at the edge of the scratch with reference to the surface This parameter is determined by the average distance between the surface and point O and the surface and point P 55 Summary for Reviewing Scratch Data The goal in scratch testing a set of samples is to compare their elastic plastic and fracture behaviors Elastic and plastic behaviors are determined before the critical load is reached and one of the ways to characterize these behaviors is through cross profiling the scratch Using the results of the cross profile blue circled parameters in Table 1 the user can compare the deformation of each sample caused by a set normal load The normal load used for cross profiling is set by the user and the load should be less then the critical load The other way to characterize the elastic and plastic behaviors is to examine the difference in the Scratch Segment and the Residual Deformation curves prior to the critical load While elastic and plastic behaviors are determined before the critical load the fracture behavio
63. tion dialog box to tailor the tip area function to their testing needs Ensuring Quality Silica Data o Identify problems in fused silica data o Troubleshoot problems that might be causing poor results on fused silica Scratch Testing o Understand the parameters involved in scratch testing o Chartthe test flow process of the scratch test o Review scratch data using standard review channels O O Understand the makers associated with scratch testing Output the data to Excel Commonly Used Procedures O O O O O Mount and load Samples Change and clean XP indentation tip Perform a Microscope to indenter calibration Change the microscope objective Change the indentation workspace Basic Indentation Process o Understand the Surface Find and Surface Approach test segments along with the required inputs associated with this integral part of the test o Create a flow diagram of the processes involved in the standard Load Unload and CSM methods o Describe the two techniques used for determining stiffness during an indentation test Method Modification o Create formulas that determine the maximum or minimum values for a given channel o Create a function that determines the Load Applied on Sample at a penetration depth of 200nm o Create a formula that averages the load applied to the sample during the Thermal Drift Correction segment o Create a formula that determines the value of a channel at a given marker
64. tion from the drop down menu Click OK Click Next Step and respond No to the prompt Click the Test tab All of the defined tests are summarized in the panel on the right hand side of the screen In this panel right click and select Save Batch At the prompt use the filename StandardBatch and click Save Close TestWorks You have now saved a batch that can be run at any time in the future Recalling and Running a Predefined Batch Launch TestWorks 1 Login and select Batch Mode 2 Inthe panel on the right hand side of the screen right click and select Load Batch 3 Select the batch StandardBatch created in another example and click Open 4 Click the Go button the green cone 5 Name the sample and select the starting location as prompted 24 6 The Review Page Introduction There are many options available in the review page Therefore the review page will be introduced through a few exercises The first exercise will simply introduce many of the options The second will show the user how to compare two or more samples in TestWorks Finally the third exercise will walk the user through changing Inputs Editable Post Test to see how these options change the data At the end of the exercises a table summarizing the review page options along with a description is provided Objectives Upon completion of this section the user w
65. u and choose Output to Excel Note that the program Analyst does not handle scratch data 49 List the most commonly used menu items for scratch testing below and be aware of what they accomplish Menu Item Description What panel is it in and What does it Do Exercise Review some scratch results We will use a sample data file included in the training materials Scratch PMMA The file used from the TestWorks Training folder in this Exercise is Scratch PMMA mss Launch TestWorks At the User Login prompt select MTS and then click OK At the next prompt click cancel and click on the open sample button At the next prompt click the advanced button and open the training data file UA eee Bac uses Go to the review page the following discussions are based on this data Graph area e Plot the following channels penetration curves with roughness vs scratch distance you should obtained a plot similar to the following 50 Penetration Curves With Roughness nm AOOO te LEER E iat oe re Gt ee I p Spes 3000 Residual l i deformation 2000F iere ae D F 10007 Scratch Distance um Markers used on the plot a Beginning of the scratch b End of the pre scratch profile c Critical point start of fracture d End of Scratch e End of post scratch profile e Notice the C marker that shows where the sample start
66. uts Highlight the Display Name Do Drift Hold When Load Below In the lower portion of the dialog box change the Default Value to 600 The maximum load of the XP is 500mN this will 81 ensure that the correction for thermal drift segment is always completed vii Click on another input to confirm the changes The value of the load at the start of the hold for thermal drift 25 26 27 28 29 30 Under the Method menu in the top bar select Edit Method and select Create Formula Choose Average Value Function enter the display name Load at Start of Thermal Drift Segment and click Create Make the following selections in the Formula Builder i Channel Load On Sample ii Index Point Start Drift Marker Click OK Notice that the Load at Start of Thermal Drift Segment has been added as a result Save your method Run Data to Examine the New Results 82 Commonly Used Procedure Posters 83 Selecting a Method 1 Use the chart below to determine which method might best fit your needs 2 Use the pdf file associated with the method to investigate the method process and the reported results further 3 Open the test method in TestWorks and examine the test flow 1f needed methods that By te yous Method Title Des on facility Uses our patented Continuous Suffnass Measurement CSM opbon to return hardness H
67. waters 4 XP CSM Hand E using Const Disp Rate Similar to 1 but loading occurs at a constant displacemert rete With nanapositioning accuracy method automatically indants scans tha SXP CSM NP Auto hdent and Scan impression then repeats for the nat test No user interacton raqured from test to test Indentation is performad using the same algorithm es for 1 With nanopasitioning accuracy 3D surface imaging C 8 XP CSM NP Fteractive Scan scans Usad to tune scan settings before using 7 XP CSM NP teractive hdert papse method RE enindentation using the XP 2DProflomay o Similar to ib bat alos imagng of much larger areas a Hand E vs penetration depth using a series of test in which paak force is raraduced at each new test site Constant bading rete force application User sets loading time max loads and hold times Orignaly for bp calibration use has broadened Returns H and E vs penetration depth using mubple badunbad cycles at 10 XP Basic Hardness Modulus T ip Cal Load Control gach test site Constant loading rate force application Usar sets load time max load end number of cycles M xPBasicCrmep Returns the stress exponent for creep using a long hold segment 12 xP Basic HandE et a Senes of Displacements Apples a pre load full load than ratums to pre loed post load Returns 13 XP Edga Deformation Test Step Load the difference in penetration between pre end post4oad Popular for testing razor blad
68. with a brief description Use this table to start your search for a method that applies to your testing plan Indentation Methods Indentation methods are in both the XP and DCM folders and there are several options depending on the material being tested There are commonly subtle differences between Surface Approach Sensitivities range of calculations and rates at which the indention takes place The largest difference between indentation methods is between the Basic and CSM methods These two methods use fundamentally different techniques to attain the stiffness of the material this difference is described above However there is surprisingly little difference in the setup of the two methods only a short list of inputs differs in the process 20 Table 1 Available Methods and Descriptions Check all enorm Method Title Description Taciley Uses our patented Continuous Suffnass Measurement CSM option to return hardness H and elastic modus E as a continuous function of 1 XP CSM Standard Hardness Modulus and T ip Cal penatration into the test surface Load using a conetant strain rate User specifies dynemic fraquency amplitude strain rate and maximum 2 XP CSM Easy Hardness Modus end T ip Cal Similar to 1 vith fewer seri puts Good for first bme users Similar to 1 vath defaut inputs optimized for testing thin films especialy JIXP CSM Hardness Modulus for Thin Films good for tasting dieletric materials on Si

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