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SM Beamline Health and Safety Orientation (HSO) training

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1. 15 26 Kloor Cooler 15 15 2 8 CLS Beamline Staff Avallab lea m 17 3 0 Overview of the SM Beamline and STXM 19 4 0 PART A Enabling the SM 21 4 1 Starting the STXM Branch Graphical User Interface 2 21 4 2 Branch 21 4 3 Safety and Photon Shutters Access Control Information System Panel 21 44 Beamline Safety and SM Photon Shutfers an 25 4 5 Closing the SM Beamline at the end of the 51110 25 4 6 Enabling the SM Beamline Quick Guide nee 27 5 0 PART B STXM Microscope Set up 29 Zane Plate Selection 29 5 2 Grating 29 5 3 Energy Selection ae 33 54 Harmonie Selection we een 29 o Polarization Sekten 35 5 6 Constant of Fixed Focus CH ai rue uen tete iu OS 37 6 0 PART C STXM Microscope Optimization 2 2400 39 6 1 Verify that Beam is reaching the Detector us iieri en 39 6 2 Detector Bean ee cm 41 6 3 OSA ro
2. 43 64 Focusing Sean 43 OS EXIS tS ee 45 6 6 Hori_Defl M3STXM Mirror een a 45 PUL OPS 47 10 1 CLS SM STXM MANUAL 2 Version 24 October 2011 6 8 STXM Microscope Set up and Optimization Quick 49 7 0 SM Beamline STXM Energy Calibration 51 APPENDICES 53 Appendix A Selecting Parameters for Specific Elements 55 Appendix B Sample 1 ea a 56 Appendix Sample Prepara ai He 58 Appendix De Data Analysis inei dice ate ipea nigra 60 Appendix E SM Beamline Polarization 2a 62 Appendix F Zone Plate Order Sorting Aperture OSA Sample amp Detector Relationship 64 Appendix SM Data Access and Data Transfer 2 2 2 22 224 1 4 66 Appendix Connecting to the Printer in the STXM 70 Appendix I SM Beamline Computer s for Users esses 72 Appendix J Selecting the optimum Cff value ae nete 74 Appendix K References oco Siete el uated E eee ice 76 Filename 111024 SM STXM BeamlineManual doc Table of Acronyms Acronym Meaning CLS Canadian Light Source SM Spectromicroscopy STXM Scanning Transmissio
3. 000880 Ton EN ove OPEN CLOSE 2 0000 secs AE SM PSH 6898808 _BSH CLOSED Taper 0 0000 10 0115 Sec 10 ZR EM 6146 10 Open close beam Eed MONOCHROMATOR Sec 11 CEM 62616 10 36415 65 a 49705 86 Grating 4970559 Sec 13 EM 1 089 10 STXM Energy selection Sec 14 DA 51 1 095 09 ooo If you want the EPU or grating tracking OFF during a scan Please contact Sec 15 a 530 3370 0 the beamline staff Sec 16 EEN 521010 Pressure should be lt 5 9 before Opening any valve 1 Updated 26Jan2011 224977777 Epuoffset 0000000808 Contacts UsefulTools i mn En ingshen Lu 3743 Energy eV 320052 Jay Dynes 3940 Figure 4 1 STXM Branch Graphical User Interface accessed from the SM Beamline Control computer Peer 7 edm 1 10 Figure 4 2 STXM PEEM SM OTHER Button on the task bar located on SM Beamline Control Display 2 10ID 1 CLS SM STXM MANUAL 20 Version 24 October 2011 4 0 PART A Enabling the SM Beamline The SM Beamline Computer controls the beamline including the valves shutters EPU grating and mirrors The valves and shutters need to be opened before setting up and optimization of the STXM Microscope The following sections show in detail how to enable the beamline and is summarized in a Quick Guide Section 4 6 The sections are presented in the recom
4. 4 86576 ua cs 240 ss 25 4 86571 f E 4 866E 400 2 240 90 35 6 7916 3 240 is OSA to SAMPLE distance um NN Calculator Zone Plate Z um 1157 29 Max Ao for current energy estimation _ Calculated Zone Plate Pos tion MAO lt 90 40 7 8451 4 150 55 60 7 2692 308 _ 6 5 s Energy eV 320 051 J 240 4 8587 Expected positions for current energy m 5 Diameter mc Focal Length um 1557 29 amp 50 B C 2 40 m Sample 2 add sample m thickness um 400 3 60 5 m ar ee OK Current Zone Plate Figure 5 5 Zone Plate focus parameters and Ao OSA to Sample distance um 10ID 1 CLS SM STXM MANUAL 32 Version 24 October 2011 5 3 Energy Selection CAUTION There is a risk of crashing the zone plate into the Order Sorting Aperture OSA when going from HIGHER ENERGY to LOWER ENERGY The next couple of steps are to protect the zone plate from crashing into the OSA We will now use the STXM Control Graphical User Interface GUI Figure 5 4 to change the energy 3 Change the zone plate focus from AUTO to STATIC window bottom middle Fig 5 4 This is done by dragging from the AUTO to STATIC In the static mode the zone plate will not move when a new energy value is entered 4 Enter 395 eV in t
5. 600 400 BD AG for aaien x Destination Scan Controls _ Current Scan Status 1541 72 1473 Goll No Current Scan Image of START sample SENE Estimated Time Region of Hori_Defl_ urad 67 6 67 6 5 Elapsed Time ei TES Next Scan 4 Point of n Fe E r Exit Slits Dispersive um 380 38 Go 15 View Bea l NonDispersiveumf 1119 111 51 Current Destination Jog Setup Motors ERU Gap E TE nt Je 0 00 0 pl sl Er CUL pe 0 00 MC NN Mcossez 510019 51001 Gol 5 Step 5 eros EPU Folowing Scan aon EPU THAI Ist BL Feedback Rs Auto gt gt B ae mee Exit Slit Curr 9 000 Es OSA OUT Zone Plate OUT Sample OUT ui 0 000 0 000Fbk Offs amp oc ire ee se it Curr 0 000 0 000 Figure 5 6 STXM Control Graphical User Interface Codes for Polarization Setup for STXM Table 5 2 EPU Vertical Circular and Horizontal Polarizations Essen 294 029 sees 95506 6 E Data STXM data 2011 2011_01 110115 A110115007 hdr loaded success Actual Polarization IncVert 90 CirLeft LinHor CirRight IncVert 90 ST
6. Setaslo countero 17000 8000 L 670 Expected 688 0 eV Actual 688 6 eV Difference 0 6eV 1 710 720 A110115025 hdr Chart 1 scan Set 10 Expected 400 87 eV Actual 401 06 eV Difference 0 81 eV 40000 20000 oL 400 Energy 400 5 401 057 1 401 5 49076 5 1 401 counterO Al10115045 hdr crar a scan 15000 10000 Expected 867 12 eV Actual 867 06 eV Difference 0 06 eV 5000 L 866 866 5 Energy 867 057 867 1 867 5 Figure 7 2 Gas spectra used for calibrating at the and Ne 15 edges 10 1 CLS SM STXM MANUAL 22 Version 24 October 2011 APPENDICES 10 1 CLS SM STXM MANUAL 53 Version 24 October 2011 10 1 CLS SM STXM MANUAL 54 Version 24 October 2011 Appendix A Selecting Parameters for Specific Elements The table is incomplete consult with the Beamline Staff for elements not listed Range eV Dispersive Nondispersive B K 18520 LEG LH CRCL 13535 N 39040 LEG 500 MEG 1545 P 2135 2165 MEG 5 LH 4040 P 12555 LEG LH CRCL 400 S 2452007 6 3 75 2 35 35 3403600 LEG ee a eS UNE UN 12 32 EE El ee EN E Exit slits estimated always adjust so that maximum intensity lt 20 M
7. 7 8 Click Printer and Faxes 2 File click Add Printer 3 4 Select A network printer or a printer attached to another computer Click Next then click NEXT Select Connect to this printer or In box type vsrv print Ol prd cp3525n e O0 May actually give you list of printers before entering a printer name Then asks you if you want to set as default printer Click Finish Apple machines Must have internet connection to download drivers 1 System preferences 2 Print amp scan 3 Add printer 4 IP top 5 Select protocol as IP IP address 10 40 0 71 6 Add HP Color LaserJet CP3525 10 1 CLS SM STXM MANUAL 70 Version 24 October 2011 10 1 CLS SM STXM MANUAL 71 Version 24 October 2011 Appendix I SM Beamline Computer s for Users Users cannot install any software on any SM beamline computer without prior permission from the Beamline Staff The program available for image and spectral analysis is aXis2000 IDL Language and it is loaded on the STXM Control Computer and the VLM computer At the time of data collection 1 during your shift the STXM Control computer can be used for data analysis using aXis2000 Outside of a User s shift the SM beamline has one computer VLM optical microscope that may be available to Users for data analysis however its availability cannot be guaranteed and thus Users are encouraged to bring their own laptop computers for dat
8. b Enter Energy c Change Ao click on S to open new screen d Change zone plate focus from STATIC to AUTO e Click Energy Go button 5 4 Select Harmonic 5 5 Select Polarization STXM Optimization 6 1 Verify the Beam is reaching the Detector Change AUTO to OPEN to open the shutter If no beam check that a PMT detector is turned on b You are in an open hole on the sample plate c All valves are open d OSA is aligned see below e Detector is aligned see below 6 2 Detector Scan 6 3 OSA Scan 6 4 OSA Focus Scan 6 5 Adjust Exit Slits lt 20 MHZ s counts 2 x 10 on display 6 6 Adjust Hori Defl urad 1 M3STXM Mirror Pitch 6 7 Adjust EPU Offset 10 1 CLS SM STXM MANUAL 49 Version 24 October 2011 Digital Pressure Analogue Pressure STXM pump valve Tank Valve i Figure 7 1 A Gas Cylinders at the SM entrance B Vacuum pump switch and gas inlet values for He C Analogy Gas gauge for measuring He level in the STXM Tank D Digital gauge for measuring gases pressure for calibration and E Vacuum pump value Table 7 1 Gas Calibration Lines for STXM Aig 1 2 Hudson et al Phys Rev A 47 1993 361 4s Ryd 3 2 To 1 2 Ma et al Phys Rev A 44 1991 1848 400 87 Chen et al Phys Rev A 40 1989 6737 406 150 407 115 n v 3 Prince et al J Elec Spect 42 1999 141 Rydberg et al Phys
9. gt Spectrum and Counts Displayed Here A Reading file 110301026 1 Loading scan A110301027 hdr Reading file A110301027 a xim Loading scan A101114046 hdr Reading file A101114046 a xim Current Scan Status Scan Controls No Current Scan Image of sample Estimated Time Region of START sample scan Elapsed Time tine of Next Scan 4 Point of Miernsenpe Control Motor Current Destination Jog Setup Motors e 600000000000000 coarsex 0 00 0 Go 5 sl coarsez o 5100 19 5100 Go step sl det off cff 21 Auto gt X Je eel _OSAIN Grating e 09 zone Plate s 9 008 AUX4 0 0 Figure 6 2 STXM Control Graphical User Interface 10ID 1 CLS SM STXM MANUAL 38 Version 24 October 2011 6 0 PART C STXM Microscope Optimization The STXM Microscope is optimized by maximizing the flux for a particular set up 6 1 Verify that Beam is reaching the Detector It is assumed that the beamline has been enabled that is all valves and shutters are open including the variable aperture The STXM microscope is routinely optimized at 395 eV as there is lots of flux and the amount of flux expected is well known Thus to verify that the detector is respon
10. For FC assistance call 657 3639 2 7 Invoice In your yellow experimental folder there is an invoice for your shifts We encourage you to pay while at the CLS Remit payment at the CLS Reception 1 306 657 3500 during normal office hours 8am to 4 30pm or to the Floor Coordinator outside of normal office hours Payment methods include Cash Cheque USASK CFOAPAL Credit Card Visa Mastercard Make cheques payable to Canadian Light Source Inc If you have any questions please contact the CLS User Services at 1 306 657 3700 or clsuo lightsource ca 10 1 CLS SM STXM MANUAL 15 Version 24 October 2011 10 1 CLS SM STXM MANUAL 16 Version 24 October 2011 2 8 CLS Beamline Staff Availability This page was taken from document 6 7 1 1 Rev B dated 2009 02 03 Please see the complete document for more information Role of the beamline staff Beamline staff will set up the beamline They will be present at the scheduled start of the experiment to complete the necessary paperwork and provide any required safety training They will train the users to operate the beamline and will assist new user groups through the first few hours of their experiment The beamline staff will assist users with their experiments However it is not their role to perform experiments for users including Beam Team members except by special arrangement It is the users responsibility to provide enough qualified individuals to run the experiment for the dur
11. U D Urquhart S G Obst M Hitchcock 2007 Soft X ray spectromicroscopy beamline at the CLS Commissioning results Nuclear Instruments amp Methods in Physics Research A 582 96 99 10 1 CLS SM STXM MANUAL 76 Version 24 October 2011
12. 6 2 the counts from the detector are displayed If you see a spectrum on a yellow background it means that the detector counts are not being displayed Click on the CHART button very top right to get the count screen If the detector is connected to the STXM computer and the HV is turned on there should be counts around 400 in the display even if the SM PSH and BSH shutters are closed If the counts are reading 0 i e flat line as shown it means that the 10 1 CLS SM STXM MANUAL 39 Version 24 October 2011 counterO 5149 29 ro Loading scan A110301026 hdr Reading file A110301026 a xim Loading scan A110301027 hdr Reading file A110301027_a xim Loading scan A101114046 hdr Reading file A101114046_a xim Current Scan Status Scan Controls No Current Scan image START Sample Scan Estimated Time Region of Elapsed Time Line of Next Scan 4 Point View Beam Micraccope Control Current FE stination Jog Setup Motors je 0 00 0 5 sl coarsez 1 1 5100 S100 Go 5 Stop 5 decor Focus Auto vj Ao 400 0 8000000000000866 0 000 Figure 6 3 STXM Control Graphical Usef Interface ES Det Scan Estimated Time 20s Centre Pos Range Points Step pm Dwel Timem 0 Load S to 20 Cancel Defin
13. For the connection and the Folder that you want to connect to Drive v Z Drive v Folder Browse Folder Browse Example server share Reconnect at logon Example server share Connect using different credentials Reconnect at logon i Connect to a Web site that you can use to store your documents and pictures Connect using a different user name Sign up for online storage or connect to a network server lt Back Finish station8107 sm_stxm File Edit View Favorites Tools Help ay Q pack 2 Search Folders ES 97 i m Address station107 sm_stm Figure G2 Windows address window in Explorer 10ID 1 CLS SM STXM MANUAL 65 Version 24 October 2011 Appendix G SM Data Access and Data Transfer The raw data files are archived and saved indefinitely STXM Data is stored on Drive E All STXM data is stored by date and the order of collection For example the first scan on February 9 2011 would be stored as 110209000 the next as 110209001 and so forth Users can copy their data i e Optical Microscope VLM Data or the STXM Control STXM Data while at the CLS over the internet or can access the data after they leave the CLS via ftp Accessing Data while at the CLS Laptops connected to any CLS network port VLANIIO or 110 can access the internet Wireless is also available ask the Beamline Staff
14. To Cursor and Sample to Cursor Coarse buttons Fig 6 3 Click on the OSA to Cursor Set to 0 0 button to mark the centre of the OSA as 0 OSA X 0 OSA Y If the OSA is not found within the usual 70 x 70 um scan size the likely reason is that it was bumped during sample loading increase the size to 300 x 300 um and do another OSA Scan Centre the OSA as outlined above The accuracy of centering the OSA is better at 70 x 70 um than 300 x 300 um so repeat at 70 x 70 um If the OSA is still not found contact the Beamline staff for assistance To check the size of the OSA hole check the ZP in focus box and repeat the OSA scan at 70 x 70 um The expected result is shown in Figure 6 5C The size of the OSA can be determined by clicking on the left and right edges of the OSA Generally the 50 um OSA hole is used DO NOT Align the OSA now just for reference To see the OSA and Zone plate the range is increased to 300 x 300 um Figure 6 5D DO NOT Align on the 300 x 300 image just for reference uniformity of the zone plate Note the OSA scan should be done whenever loading a sample to verify that it was not bumped during the sample change Also an OSA scan could be done when changing to different edges particularly if there was a large energy change e g 500 eV 6 4 OSA Focusing Scan The OSA Focus Scan is done to calibrate the Zone Plate scale using the OSA as the reference point The OSA Focus Scan is done right
15. are closed by the Control Room during an injection when there is a beam dump or for planned maintenance These shutters must be opened before beam can come down the beamline The SSH indicator light button and the PSH indicator light are located on the Access Control Information System ACIS Panel Fig 4 3 Permission to open the SSH shutter is given by the Control Room and is indicated when all the lights before the SSH shutter are green Open the SSH by pushing the LARGE GREEN BUTTON at which time the LARGE RED BUTTON will go off and the GREEN BUTTON on The PSH shutter can only be opened after the SSH shutter is opened and is opened from the STXM Branch GUI Fig 4 4 Note that the SSH and PSH shutters also control the beam access to the REIXS beamline and may be opened by their Users Staff If you cannot open the SSH or PSH shutters after the injection is complete contact the floor coordinator for assistance Note also that the SSH and PSH shutters cannot be closed from the STXM CONTROL computer once they are opened 10ID 1 CLS SM STXM MANUAL 23 Version 24 October 2011 a SM Beamline Control System 0x SM PSH 1 PGM M3PEEM M3STXM STXM ES St SS SH 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 Branch amp Grating Selection EPU Monochromator Valves amp Vacuum Note To change branch or grating the SM photon EPU CA 1 166e 10 0 shutter SM PSH has to b
16. change grating first click HOME HOME when itis done then select grating 2 OpenBeamline SSH GLOSED PSH CLOSED OPEN CLOSE SM PSH 005808 BSH CLOSED open close bear GE 3 GoseBeamline 4 Energy Selection If you want the EPU or grating trackin OFF during a scan Please e the beamline staff Q1 00035 Q2 0 0025 Harmonic Mode Ange 0 0020 9 aa 443 T 0 0345 cit 2149 Epu offset 01000 9 7 UsefulTools Figure 4 4 STXM Branch Graphical User Interface Energy eV 320 052 10 1 CLS SM STXM MANUAL 22 Valves amp Vacuum Sec 1 Sec 2 Sec 4 Sec 6 Sec 7 Sec 8 Sec 9 Sec 10 Sec 11 Sec 12 1166e 10 OP 9 829e 11 1 367 09 e o 21 6 674e 10 000 E 1 48076 10 E 51 3 885e 10 ooo ICL 51 61486 10 ooo 51 6 761 10 000 2 4 1 50261 10 ooo 51 1 089 10 ooo 1 095 09 254 91 3970e 10 21 5 210 10 ooo Pressure should lt 5 9 before opening any valve Updated 26Jan2011 Contacts Jian Wang 3546 Yingshen Lu 3743 Jay Dynes 3840 Version 24 October 2011 The sample can be loaded prior to opening the shutters and enabling the beamline and or STXM microscope The SAMPLE LOADING UNLOADING procedure is shown in Appendix B The Safety SSH and Photon PSH shutters
17. file 110301027_ Aut Loading scan A101114046 hdr m 1 uto m 200 Reading file A101114046_a xim a 138 Citeo Beamline Control 2 Microscope Status Energy Reading Destination Current Scan Status Scan Controls SampleX 00009 9 ev 9 320 043 BME No Current Scan Image of START SampleScan SampleY 9 5000 8809 ev Estimated Time Region of SampleFinez 9 25 009 Hori_Defl_ urad 76 67 5 elapsed Time pe Ne coarse er gt Pause CoarseY e Exit Slits e Next Scan 4 Point of HEBES TUS Dispersive um 38 G a ispersive um 5 ZonePlatez o b Microscope Control ng EEE fe m NonDispersive umf 11 Im Motor Current Destination Jog Setup Motors ae 4 Gap mm 0 000 Coarsex e 0 00 0 Go 5 Stop 5 PES DetectorX BE All ON D Y 0 00 0 00 0 Sea PT are O s1001 5100 eol 5 stop 5 geor DetectorZ DINE Focus cff 5 BL Feedback 6 auto 8 ed Sample _OSA IN Zone Plate IN Sample IN Grating Slit Curr Exit Slit d Ao Mover OSA OUT Zone Plate OUT Sample OUT aux3 e 0 000 lock AUX4 0 000 0 000 A Focus amp Zone Plates Parameters Focal Length Function J NEN NELLE LILLE miS E d Central 1 Diameter stop Outer zone Al z
18. harmonic and polarization for a particular element is shown in Appendix A The table is incomplete so if you do not see the element or edge of interest contact the Beamline Staff to determine whether the element can be run at the SM beamline Table 3 1 Summary of SM beamline important parameters Source Apple II type Elliptically Polarizing Undulator period 75mm End Stations STXM PEEM Energy Range 130 to 2500 eV Flux STXM 10 ph s for a resolving power of R 3000 PEEM 10 ph s for a resolving power of R 3000 Spatial Resolution STXM 30 nm PEEM 50 nm Resolving Power E AE Nominal 3000 can reach gt 10 10ID 1 CLS SM STXM MANUAL 19 Version 24 October 2011 a SM Beamline Control System 0 M3PEEM M3STXM 5 5 1 2 3 4 5 6 8 9 10 11 12 13 14 15 16 a Branch amp GratingSelection 5 EPU Monochromator Valves amp Vacuum Note change branch or grating the SM photon EPU DA 1166e 10 6 shutter SM PSH has to be closed Feier step EPR BRR RRR eee eee Gap 200 0000 40 2995 Sec 2 9 829e 11 SelectBranch PEEM O EEE Q1 9 00 000 CAM 1367e 09 e first olok HOME a Sec 6 JJ 230 6 674 10 grating first F b A eoo when it is done then select gratin Q2 m Sec 7 4 807e 10 2 OpenBeamline Q3 9 0000 9 0025 a SSH CLOSED
19. image which will activate the Focus to Cursor Set ZP calibration button not shown appears in place of the Sample To Cursor and Sample to Cursor Coarse buttons Fig 6 3 Click on the Focus to Cursor Set ZP calibration If it was not possible to see the focal point it may be because the zone plate was way out of focus Consult the Beamline Staff for assistance Usually the OSA Focus Scan needs to be conducted only when initially setting up the microscope at 395 eV The OSA Focus Scan can be done after every OSA Scan usually not necessary however above 1000 eV there can be problems Ask the Beamline staff for details 6 5 Exit Slits The exit slit controls the beam size in both the vertical and horizontal directions that hits the zone plate While the flux is determined by both the Dispersive vertical and Nondispersive horizontal exit slits Fig 6 7 only the Dispersive slit influences the spectral resolution Hence the nondispersive exit slit can be opened larger than the dispersive exit slit to increase the flux but maintain the desired spectral resolution The exit slits are usually selected so that the maximum flux is lt 20 MHz The exit slit size is often displayed as the Dispersive Nondispersive slits e g 20 20 The size of the exit slits are adjusted to prevent saturation of the PMT detector as a linear response is necessary for quantification and good image quality The PMT saturates when the
20. is closed 5 Turn on the vacuum pump using the switch on the wall 6 Open the vacuum pump valve 7 Pump until pressure is less than 200 mTorr bottom scale on the digital gauge 8 Close the vacuum pump valve 9 Turn off the vacuum pump 10 Open the Helium valve on the wall Make sure there is He in the tank located outside the SM entrance way 11 If Helium was not the gas previously used open the release valve to flush the gas line 12 Open the gas valve on the STXM tank and allow Helium to fill the tank to 1 6 atmosphere red line marked on the analog gauge 13 Turn off the Helium valve on the wall 14 Turn on the Detector 10 1 CLS SM STXM MANUAL 56 Version 24 October 2011 Figure C1 A Sample Plate in storage case with samples Si3N4windows and labeling information B Sample Holder inside STXM Tank Si3N4 windows fastened with double sided tape and epoxy and D FIB samples fastened to sample plate Sample Plate Coordination System 5000 0 5000 Coarse X Coarse X Coarse Y 5000 5000 0 5000 5000 5000 5000 0 0 0 5000 0 au gt Figure C2 Sample plate coordination system Note for ALS 5 3 2 Hole 1 and for 11 02 Holes 1 2 and 3 are not accessible 10ID 1 CLS SM STXM MANUAL 57 Version 24 October 2011 Appendix C Sample Preparation Sample preparation is briefly discussed here for more detailed information and for information on alternative experiment
21. that detailed above may be available by prior agreement between the users and the beamline staff As much as possible arrangements will be make to provide the highest level of assistance for new user groups If significant assistance with experimental planning data acquisition and interpretation is required it is normally expected that the users will treat the beamline staff as collaborators with appropriate recognition given e g co authorship Where practical additional assistance should be solicited ahead of the user s experiment 10 1 CLS SM STXM MANUAL 17 Version 24 October 2011 EPU PCM M3PEEM ES STXM STXM ecc M3STXM M4PEEM A ES PEEM 49 1 8 1 5 1 5 3 0 1 5 3 3 0 16 2m 21 0m 22 5m 24 0m 25 5m 29 9m 33 7m x M2 M3PEEM M3STXM B uut PGM Figure 3 2 STXM Hutch A STXM End Station Tank and B STXM Control Computer work area Figure 3 3 A Sample Mounting area amp Optical Microscope B User work area and C SM Beamline Control Computer work area 10ID 1 CLS SM STXM MANUAL 18 Version 24 October 2011 3 0 Overview of the SM Beamline and STXM Microscope The SM beamline consists of an elliptically polarizing undulator EPU located inside the storage ring the M1 mirror inside the SM hutch and a plane grating monochromator PGM Fig 3 1 There are two branches on the SM beamline with dedicated end stations the scanning transmission X ray microscope STXM Fig 3 2 and ph
22. then increase When optimized close the Hori_Defl S display You may need to readjust the exit slits so that the Io signal maximum is lt 20 MHZ s 6 7 EPU Offset The position of the beam relative to the EPU Gap changes slightly with a change in energy That is the beam may be off centre of the EPU Gap resulting in a reduction in the intensity of the beam The loss in intensity can be corrected for by adjusting the EPU Offset Fig 6 8 Adjust the EPU Offset by 0 05 to 0 1 units negative or positive until the maximum signal is realized Note you must click on the SET button to implement the change Confirm that the change was made by comparing that the actual and input values are the same Clear the display Clear button top left of display to make it easier to see small changes The EPU Offset is usually between 0 3 and 0 3 You may need to readjust the exit slits so that the Io signal maximum is lt 20 MHz s 10 1 CLS SM STXM MANUAL 47 Version 24 October 2011 10 1 CLS SM STXM MANUAL 48 Version 24 October 2011 6 8 STXM Microscope Set up and Optimization Quick Guide STXM Microscope Set up and Optimization Quick Guide Use STXM Control GUI Consult the manual for complete details STXM Set Up 5 1 Select Zone Plate Discuss options with Beamline Staff 5 2 Select Grating 5 3 Select Energy CAUTION Changing from High to Low Energy a Change zone plate focus from AUTO to STATIC
23. usually sends out a remainder to Users of their upcoming beam time one week prior to beam time The most current beamline schedule for all beamlines is available on the CLS website http www lightsource ca operations schedule php A printable copy of the SM beamline schedule disseminated previously by the SM Beamline Scientist can be obtained via the SM website http exshare lightsource ca sm or ask the beamline Staff for a copy If you have any questions please do not hesitate to contact the beamline staff or the CLS User Services office 1 2 Perform Proposal Amendment if Required Proposals must be up to date with regards to the samples the Users intend to run during their shifts at the SM beamline and the samples must receive CLS Health Safety amp Environment HSE approval prior to the commencement of the shifts Changes to on site personnel should also be updated prior to the commencement of the shifts Note it is the responsibility of Users to ensure that their proposal is up to date The amendments must be done on line editing their previously submitted proposal In order to ensure that HSE gives their approval the changes should be made at least 4 weeks prior to their beam time Samples not approved by HSE will not be allowed to be run at the SM Beamline Contact the CLS User Services office if you have any questions regarding proposal amendments 1 3 CLS Safety Training and New User Registration All new Users must Comp
24. 4 S fr 1 52 d eo amp amp lt 6 lt lt 4 11 S So E Q 2 Q E Z 6 2 cm B 4 E E a ia 2 1019 1 1079 1 1 200 220 240 260 280 300 300 350 400 450 50C 400 450 500 550 600 Energy eV Energy eV Energy eV Figure J1 Peak photon flux in the first order near the carbon nitrogen and oxygen K edges in circular polarization measured using the LEG at STXM exit slit Second order contribution near the Carbon K edge for the LEG and MEG Fig J2 1 Second order contribution increases with an increase in the cff value 2 Second order contribution is higher at LinHor polarization than at CirRight polarization 3 Use cff values of 2 0 to 2 5 at the Carbon K edge for both the LEG and MEG Second order suppression Second order suppression STXM Exit Slit 250 I mm grating STXM Exit Slit 500 I mm grating O CircularRight 200eV CircularRight 265eV Linear Hor 200eV Linear Hor 28peV CircularRight 200eV CircularRight 265eV LinearHor 200eV LinearHor 265eV e Second order contribution 96 Second order contribution 96 1 5 2 0 2 5 3 0 3 5 4 0 1 5 2 0 2 5 3 0 3 5 4 0 Figure J2 Second order contribution as a function of value near the Carbon K edge for the LEG 250 l mm and MEG 500 l mm 10 1 CLS SM STXM MANUAL 74 Version 24 October 2011 10 1 CLS SM STXM MANUAL 75 Version 24 October 2011 Appendix K References 1 Kaznatcheev K V Karunakaran Ch Lanke
25. 50 mm 7th Harmonics 10 10 500 100 150 200 2500 200 400 ev 800 1000 Energy eV Figure 5 2 Photon flux as a function of energy at the STXM exit slits for A First order light using circular polarization and B First third and fifth order light using linear horizontal polarization 10ID 1 CLS SM STXM MANUAL 28 Version 24 October 2011 5 0 PART B STXM Microscope Set up The following assumes that the SM beamline has been enabled The STXM computer controls the microscope set up and optimization and data acquisition See STXM User Manual for details on data acquisition and is located inside the STXM hutch Fig 3 2A Sometimes it is necessary to restart the computer which is done through the Windows software or by rebooting the STXM computer button located on the front of the computer Fig 3 2A If the STXM computer is restarted the User must log back on and the screen opens to Figure Fig 5 1 login selection and password PW are found on the bottom left of the STXM Control computer screen monitor and the PW is case sensitive Note usually the sample is loaded previous to setting up and optimizing the STXM Microscope To see the loading procedure as well as the sample plate design and numbering system see Appendix B Also Users need to understand the relationship between the zone plate order sorting aperture OSA Sample and Detector which is discussed in Appendix D We encourage new Users to l
26. Hz 10 1 CLS SM STXM MANUAL 55 Version 24 October 2011 Appendix B Sample Loading Unloading Appendix B Sample Loading Unloading Recommend that gloves be worn when loading unloading samples Before opening the STXM Tank the following is required 1 Turn OFF the Detector extents the life of the detector 2 Move the sample holder away from the OSA and Zone Plate by moving Coarse 7 to 5000 STXM_CONTROL_GUI 3 Close the BSH shutter on STXM Branch GUI protects User from X rays 4 Open the vent valve on the STXM tank to break the vacuum may already be at atmosphere 5 Record the sample information sample position and the empty hole positions Figs B2 in your logbook Open the STXM Tank by removing the left front plate 1 Remove the sample plate if applicable which is held by clips on the Sample Holder Fig B1B by gently lifting it straight up being careful to avoid hitting the OSA Zone Plate detector and mirrors 2 Load the sample plate again being careful to AVOID hitting the components in the STXM End Station 3 Look inside the STXM End Station to make sure the sample plate was correctly mounted and the sample holder is about 5000 um back from the OSA Use a flashlight if necessary CAUTION For WET CELLS pumping may cause the windows to break thus flushing with Helium may be preferred In this case do not pump Ask the Beamline Staff for assistance 4 Make sure that the vacuum pump valve
27. Io signal intensity is above 20 MHz s Click on the CHART button very top right to get the count screen The chart units are Hz s The PMT is usually set to PMT 10 So a chart reading of 2 x 10 Hz s is equal to 20 MHz multiply by 10 for the PMT and 1 MHz 10 Hz On your image for 2000 Hz ms maximum 20 MHz s for a dwell time of 1 ms 2000 Hz ms x 10 PMT 10 x 1000 ms s So when counts 2000 on an image may indicate that your detector is saturated if your frame is in the image counts may be 2000 Since the signal intensity is a function of the energy the selection of the energy at which the exit slit size is adjusted to keep the intensity 20 MHZ s is usually done at the lowest energy of the edge that you will collect a stack line scan as generally the Io signal intensity decreases with increasing energy Figure 5 2 For example at the Fe L edge use 695 700 eV For the C K edge we generally set up at 300 eV because of the big dip in the C K edge Io signal due to C contamination on the optics and windows the flux at 300 eV is usually around 10 MHz with slits 35 35 and the Ti filter in but above 20 MHz at 320 eV which is OK 6 6 Hori Defl M3STXM Mirror Pitch The position of the beam on the M3STXM mirror changes slightly with a change in energy That is the beam moves off of the best spot on the M3STXM mirror resulting in a reduction in 10 1 CLS SM STXM MANUAL 45 Version 24 October 2011 z Loa
28. Rev A 44 1991 1848 0 Hitchcock et al J Elec Spect 42 1987 11 3s Ryd Francis et al Phys Rev A 52 1995 4665 Coreno et al Phys Rev A 59 1999 2494 10 1 CLS SM STXM MANUAL 50 Version 24 October 2011 7 0 SM Beamline STXM Energy Calibration The energy scale of the beamline is calibrated generally about 3 or 4 times a year by the Beamline Staff taking about 4 hours to complete However for many reasons the energy scale may change after the calibration procedure Thus Users are recommended to use reference compounds with known peak positions and or compressed gases to accurately adjust the energy scale of their collected data Compressed gases available for calibration at the beamline include carbon dioxide nitrogen neon and SF check for availability The carbon dioxide and nitrogen are outside the STXM hutch near the entrance to the SM beamline while Ne is in a small cylinder inside the STXM hutch Fig 7 1 Gas Calibration Procedure Note only Beamline Staff are permitted to change the gas cylinders 1 Identify the gas that is closest to your energy of interest Table 7 1 2 Remove the sample or move to a hole in the sample plate Gas calibration can be done with your sample inside the STXM Tank 3 Pump the STXM Tank to below 200 mTorr making sure that the pump value is closed when the pump is first started then open the value after the pump is started Note
29. STXM Manual SM 10ID 1 Beamline Canadian Light Source Inc CLS University of Saskatchewan 101 Perimeter Road Saskatoon Saskatchewan Canada S7N 0X4 SM beamline Phone 1 306 657 3609 CLS Main Receptionist Phone 1 306 657 3500 CLS User Services Phone 1 306 657 3700 Fax 1 306 657 3535 CLS website http www lightsource ca SM beamline website http exshare lightsource ca sm Table of Contents Tabl of NCFORVITIS aas chus esas Eten 3 the Document ua s ote qb ee 5 SM Beamline Staff and Beam Team Leaders ccsscssscsssssscsssecseesssceestssansscsssanconseascacetseaccenseese 7 Past SM Beamline Staff senad eaeoe nee 8 1 0 Checklist before your Arrival oiv ee 9 1 1 Confirm SM beamline time u nern 9 1 2 Perform Proposal Amendment if Required u 9 1 3 CLS Safety Training and New User 4 9 1 4 Sending Samples and Equipment to the 5 11 ca een desde 11 1 6 Remote PCS I 11 2 0 AL the SM Beamline natste delden ennen eed 13 2 1 Meeting with Beamline Staff prior to Starting your Experiment aen 13 2 2 SM Beamline Specific Orientation aa 13 23 Laboratory nnee nee cadena 13 24 Permit amp Pink Sheet senken aa en 13 2 3 Food and Drink
30. XM value 2 1 0 1 2 Table 5 3 EPU Inclined Polarizations Actual 80 70 60 50 40 30 20 10 10 20 30 40 50 60 Angle 70 80 STXM 20 30 40 50 60 70 80 90 110 120 130 140 150 160 value 170 180 1 Add 100 to the actual angle required 80 Actual Angle 100 20 STXM value entered 10ID 1 CLS SM STXM MANUAL 34 Version 24 October 2011 5 4 Harmonic Selection The harmonic determines the EPU gap settings which influences the flux The recommended harmonic for each energy range is displayed in Table 5 1 or for each element in Appendix A 1 To change the harmonic drag down to the desired harmonic using the EPU Harmonic box on the STXM Control GUI Fig 5 6 or click on the HARMONIC button on the STXM Branch GUI Fig 4 1 It is preferable to use the STXM Control GUI as the parameters file is updated whereas making the change in the STXM Branch GUI does not update the parameter file Note initial optimization of the microscope is usually done at 395 eV just below N K edge so initially use the values for K edge 1 harmonic 1 5 5 Polarization Selection The SM beamline is designed to produce plane horizontal LinHor or vertical IntVert 90 IntVert 90 circular left CirLeft or right CirRight and linear polarized light LinInc with the pola
31. a analysis If you use the SM beamline computers for data analysis save your work under the folder C Users and copy onto a memory stick or transfer through the CLS ftp data server site see Appendix F before leaving the CLS as folders older than 1 month will be deleted 1 Optical Microscope VLM Computer only available when not required for previewing samples Username Posted on Monitor or Keyboard Password Posted on Monitor or Keyboard aXis2000 Spectral and image analysis of STXM and PEEM data Microsoft office suite Word Excel PowerPoint 10 1 CLS SM STXM MANUAL 72 Version 24 October 2011 10 1 CLS SM STXM MANUAL 73 Version 24 October 2011 Appendix J Selecting the optimum Cff value The constant of fixed focus Cff value controls the angles for the mirror and the grating of the PGM Usually the Cff value is set at 2 15 To change the Cff values consult with the Beamline Staff One can select different Cff values in order to trade off intensity for increased spectral resolution This section gives information on how these quantities change as a function of the Cff value for the LEG 250 l mm and MEG 500 I mm Fig J1 e Use Cff values between 1 75 to 2 5 for better intensity and to reduce second order light e Intensity at CirRight polarization is higher than at LinHor polarization 10 12 0 E 1 5 1 92 2 45 3 13 4 0 ee E 20 S o 8 S 21 Mar 2007
32. addressed to a permanent staff member of the CLS preferably to the beamline scientist or science associate responsible for the beamline that you will be using e To expedite outgoing shipments you can make round trip shipping arrangements from your home institution Please advise Shipping amp Receiving if you have made these arrangements Please notify the CLSI Receiving stores lightsource ca at least 1 week prior to arrival to advise of any shipments that will arrive before or during your stay This is especially important if you intend to ship hazardous materials where storage of the shipment may require advance planning if there are any special handling instructions or if shipment will require a forklift or crane Users are responsible for Canada customs clearance and any charges incurred If they do not have a Canadian Customs Broker they can ship via Fedex or UPS and complete a One Time Agency Agreement which is available from Fedex or UPS 1 5 Manuals The SM beamline and microscope STXM operational manuals are available on line on the SM beamline website at http exshare lightsource ca sm Read them before your arrival at the CLS so that you can use your beam time more efficiently 1 6 Remote Access Remote access to the SM STXM computer is available Contact the CLS SM staff for details 10 1 CLS SM STXM MANUAL 11 Version 24 October 2011 Spectromicroscopy Beamline Quality Assurance Checklist Zone Plate OSA Hole Siz
33. aff and a User listed on the permit Make sure that all the samples that are going to be examined are listed and that all approvals have been signed off e g BSO 10 1 CLS SM STXM MANUAL 13 Version 24 October 2011 10 1 CLS SM STXM MANUAL 14 Version 24 October 2011 If you leave the beamline for more than 30 minutes during your beamtime you must fill out the HSE form BEAMLINE UNATTENDED BEAMLINE NOT IN USE pink sheet Figure 2 2 and place it with your permit The purpose of the pink sheet is so that the CLS Emergency Response Team is made aware of who is on site in case of an Emergency e g fire 2 5 Food and Drink Food and drink are allowed at the SM beamline in the User work area No food or drinks can be taken into the STXM hutch or past the doors to the Beamline Control Computer area PEEM end station 2 6 Floor Coordinator The Floor Coordinator s FC roles are to communicate CLS Policies Procedures to Users monitor compliance with those policies procedures including inspection of the Experimental Permit and perform periodic inspections of all experimental areas When the SM beamline staff is unavailable the FC will act as liaison between the Users and the Controls Operator and HSE personnel They provide first response in the event of accidents incidents on the experimental floor They can disable the SM beamline if CLS policies procedures are not adhered to They have access to the on site food and accept payments
34. after the OSA Scan The OSA Focus Scan menu can be accessed from the Scan Control by dragging down to the OSA Focus Scan Fig 6 3 The usual parameters for an OSA focus scan are shown in Figure 6 6A Note a Green Line appeared onto the OSA image when the OSA focus scan was opened Figure 6 6B Usually it is not necessary 10 1 CLS SM STXM MANUAL 43 Version 24 October 2011 I Control Program 28 Feb 20 File Setup Window Help View Be Slit Curr imc Figure 6 7 STXM Control Graphical User Interface 10 1 CLS SM STXM MANUAL Microscope Control Motor Loading scan A110301026 hdr Reading file A110301026_a xim Loading scan A110301027 hdr Reading file A110301027_a xim Loading scan A101114046 hdr Current Scan Status No Current Scan Image Estimated Time Region Elapsed Time Line Next Scan 4 Point u F scan Controls Reading file A101114046_a xim START Sample Scan Current je 0 00 2223 Je 5100 1 cor wo Destination Jog Setup Motors roms 5100 5 Stop S decor OSA OUT Zone Plate OUT Sample OUT 00600000000 44 Version 24 October 2011 PMT 10 to move the Green line Click Begin Scan and expected image of a calibrated zone plate is shown in Figure 6 6C Move the cursor to the focused position by clicking on the OSA focus scan
35. al set ups e g humidity chamber see the SM website http exshare lightsource ca sm Pages SM Home aspx Samples are mounted on samples plates specifically designed to fit into the STXM sample Holder Fig C1 The SM beamline will supply the User with sample plates and plastic storage cases Samples can be mounted on Si3N4 windows or TEM grids For other materials consult with the Beamline staff Si3N4 windows grids are usually fastened to the sample plate using double sided tape Fig We also recommend that the windows grids be fastened down with epoxy for added stability Fig The SM beamline can supply the User with a small number of Si3N4 windows otherwise the User is asked to purchase the windows directly from the suppliers Two known suppliers of silicon nitride windows are Silson Ltd in Northampton England http www silson com Norcada in Edmonton Canada http www norcada com products php There are a number of different sizes of silicon nitride windows generally we find that a window thickness of 75 or 100 nm and a window size of 0 5 x 0 5 mm on a 200 um thick frame are suitable for most applications The windows can be purchased in large sheets where the User has to break them apart or already separated and put into a gel case the sheets are considerably cheaper TEM grids can be purchased from any TEM supplier Both formvar coated and lacey carbon grids have been found to be sui
36. ank is moving and back to green when the tank has stopped moving Note it may be necessary to click the HOME again as sometimes the move is not completed as evident by DONE not appearing and the not in position stops flashing 2 Then click on the desired grating 1 LEG MEG Fig 5 3 and while the grating is moving the display will show not in position and will display the numbers 250 LEG 500 MEG or 1250 HEG when complete Following this procedure ensures that the energy calibration is more reproducible If the grating is selected without pushing the HOME button the energy scale may change by up to 0 3 eV from its previous setting when changing gratings 10 1 CLS SM STXM MANUAL 31 Version 24 October 2011 Storage Ring Current counter0 px Scan ren Clear interval ms 500 Signals WS 477 14 08 121 Cursor 0 En k 04 10 02 lt 9 301 5 0 7 OX mi esr 02 x ag b 24 A y 7 06 Ll 138 08 EST x 5149 29 Sample 86 Abs gt 340 11 28 19 11 23 46 11 31 12 11 32 38 _ Sample To Cursor EDEN Loading scan A110301026 hdr El pm Sample To Cursor Reading file A110301026 um Coarse Loading scan Al 1050202 7 hdr Shutter Reading
37. ation of the beamtime note that the CLS has 24 hour operation Normal working hours During normal working hours 9am 5pm Mon Fri the beamline staff will be present at the CLS or able to respond at short notice Note that under the present schedule only three or four user shifts per week fall within these times Outside normal working hours Up to 10pm Mon Fri and 10am to 10pm weekends and holidays users may contact the beamline staff for assistance using the contact details provided If telephoning is indicated users should use the beamline phone so that staff can identify that this is likely to be a request for user assistance A response is not guaranteed but beamline staff will endeavour to inform users in advance of times when no coverage is available Staff may attempt to solve problems remotely but may come in to the lab at their discretion Outside these hours we request that users do not attempt to contact the beamline staff unless prior arrangements have been made for additional support In the event that the Floor Coordinator FC is familiar with the beamline they may be able to offer assistance However in general the FC is not authorized to perform technical fixes and users should not expect the FC to solve technical problems Since 24 hour support cannot be provided users should be prepared that on occasion no help will be available until the start of normal working hours Additional support Support beyond
38. ding scan A110301026 hdr Reading file A110301026_a xim Loading scan A110301027 hdr Reading file A110301027 a xim Loading scan A101114046 hdr Reading file A101114046_a xim F Current Scan Status F Scan Controls Sean Image START samplescan gt Estimated Time Region Elapsed Time Line m Next Scan 4 Point port Control Motor Current Destination Jog CoarseX je 0 009 0 5 Stop CoarseZ 0000000000000866 Entrance Slit ol Em T E C c Figure 6 9 Defl urad 35 pitch window opens icking on 5 10ID 1 CLS SM STXM MANUAL 46 Version 24 October 2011 the intensity of the beam The loss in intensity can be corrected for by adjusting the pitch of the M3STXM Mirror M3STXM pitch is shown on the STXM CONTROL GUI as the Hori_Defl_ urad box Fig 6 8 Click on the 5 button beside the Hori_Defl box opening to Figure 6 9 Under the JOG enter 1 if not already entered sometimes 0 if STXM Control program was restarted Clear the Chart display Clear button top left of display to make it easier to see small changes Use the red arrows left and right of the JOG box to maximize the intensity If the signal is going down use the other arrow Be patient between each movement as there is a backlash sometimes and the signal may actually decrease initially
39. ding to the beam we will use the set up conditions for 395 eV See Section 5 for details Grating MEG Harmonic 1 Polarization CirLeft or CirRight Energy 395 eV Exit Slits 20 20 Dispersive Nondispersive see below for details Also it is assumed that a sample plate with samples has been loaded See Appendix B for the procedure for Loading Unloading a sample and that the STXM tank has been pumped and filled with 1 6 atmosphere of He 1 Turn on the PMT detector by turning on the high voltage controller which is usually sitting on top of the STXM chamber Fig 6 1 The voltage should be around 1050 V 2 Move to an open hole on your sample plate assumes a sample is loaded See Appendix B for the sample plate coordination system 3 Move the sample holder to 3000 um using Z the distance can visually confirmed This distance is just to ensure that the sample holder is not blocking the beam For looking at actual samples the expected position between the sample holder and OSA is about 300 um larger than the Ao value e g Ao 300 expect Coarse Z about 700 for Si3N4 window CAUTION is advised though as sometimes the calibration of the Coarse Z scale goes off Thus it is usually better to gradually move e g starting position Ao 1000 um the Coarse Z closer i e sample holder and use the focus as the guide 4 On the spectral display window top right corner on the STXM Control GUI Fig
40. e um 40 50 60 70 80 Detector Scan Completed OSA Scan Completed OSA Focus Scan Completed Exit Slits Counts at 395 eV Hz s Other Comments Beamline Staff that set up and optimized the STXM Microscope Print Name Signature Date Figure 2 1 Spectromicroscopy Beamline Quality Assurance Checklist Figure 2 2 Information sheet pink sheet to be left with the permit when the User is away from the beamline for more than 30 mins 10ID 1 CLS SM STXM MANUAL 12 Version 24 October 2011 2 0 At the SM Beamline 2 1 Meeting with Beamline Staff prior to Starting your Experiment The beamline staff wants to meet with your group at least 30 mins prior to the commencement of your beamtime to discuss your experiment and the operation of the SM beamline and STXM microscope and go over and sign the Experimental Permit Note Users will not be allowed to run without an Experimental Permit signed by both the User and beamline staff For complicated non routine STXM experiments additional time may be required to discuss your experiment please make arrangements with the beamline staff well in advance of your beamtime to ensure that your beamtime is efficiently used Note if you need help to prepare your samples prior to your beamtime please make arrangements with the beamline staff well in advance of your beamtime The Beamline Staff will ensure that the STXM microscope is set up initially for the Users first shift For first time Us
41. e Plate Detector Diameter D TITEL 0 S Diameter 240 um 600 um Focal Length f Monochromator i Refocusing Optics lii i Zone Plate 7 M EN i Zone Plate i CoarseZ DetectorZ i lt 0 0 0 Detector 0 0 0 1 m Focal Length f a Maximum A Distance A Sf rin Resolution 1 22Ar Detector Position L M Figure F1 Relationship between the position of the zone plate OSA sample and detector in the Z direction e g Coarse Z Zone Plate at Zone Plate at E OSA STXM Sample Plate Detector E gt E FocalLength at E f l l l Zone Plate Z i Ao Focal Length at E f Zone Plate Z j CoarseZ Figure F2 Zone plate position as a function of energy E2 gt El zone plate moves further away from the OSA 10ID 1 CLS SM STXM MANUAL 63 Version 24 October 2011 Appendix F Zone Plate Order Sorting Aperture OSA Sample amp Detector Relationship The spatial relationship between the zone plate OSA Sample holder and detector are shown in Figures Fl F2 and OSA is assigned the coordinates 0 0 0 left of the OSA is the zone plate and it is negative while right of the OSA where the sample holder is is positive The OSA and Detector do not move during data acquisition whereas the zone plate and sample holde
42. e closed Beier step 2 G 2 402995 200 0000 Sec 2 9 829e 11 SelectBranch BRANCH 2 STXM as Q1 0 0000 0000 5 Sec 4 2 51 1 367 09 e SelectGrating tee wea O 250 m To change grating first click HOME Y Sec 6 21 6 674 10 when itis done then select grating Q2 90000 aes O AEM 4807e 10 Q3 9 0000 0 0025 Sec 8 3 885 10 OPEN CLOSE pooo BMO secs SEN Taper 2 0000 aus Sec 10 6 148e 10 ooo Kost MONOCHROMATOR Sec 11 MJ El 6 761 10 ooo 36415 65 Mirror 3641929 Sec 12 jai 814 5 026e 10 ooo ing 49705 86 Grating 4970559 Sec 13 1089 10 ooo STXM EnergySelection Sec 14 1 095 09 ooo If you want the EPU or grating tracking OFF during a scan Please contact Sec 15 ul 3370 10 the beamline staff Sec 16 or rcr 5 210e 10 H x Mode Ange Pressure should be SE 9 before opening any valve Updated 26Jan2011 214977777 Epu offset 0000008 Contacts Wang 3546 Yingshen Lu 3743 Jay Dynes 3840 Energy eV 220052088 Figure 4 5 STXM Branch Graphical User Interface 10ID 1 CLS SM STXM MANUAL 24 Version 24 October 2011 4 4 Beamline Safety and SM Photon Shutters The SM PSH shutter is to be closed whenever there is a grating or branch change to protect the PGM The BSH shutter is to be closed whenever there is a sample change or the STXM E
43. ers for a detector scan are shown in Figure 6 4A Click Begin Scan and the expected result of a well centered detector is shown in Figure 6 4B To align the detector move the cursor to the centre of the Detector image by clicking on the detector image which will activate the Detector to Cursor Set to 0 0 button on the left hand side under the image display window Click on the Detector to Cursor Set to 0 0 button If the detector is not found there are likely three reasons First you may not be in a hole and the sample sample plate is blocking the beam make sure you are in a hole Secondly the OSA may not be aligned and is blocking the beam Move the OSA out of way by clicking on the OSA Out button Do another detector scan Remember to put the OSA back by clicking the OSA In button Finally the detector may not be aligned increase the scan size from the usual 1000 x 1000 um to 2500 x 2500 um Do another detector scan If the detector is still not found contact the Beamline staff for assistance Note that the detector scan usually only needs to be done once at the beginning of the shift to confirm that the detector is well aligned 10 1 CLS SM STXM MANUAL 41 Version 24 October 2011 Gran Estimated Time 475 Centre Pos um mRange um Points Step um aS eV 32 30 2 333 ray Dwell Time ms 3 30 2 333 ZP Focus OSA X 0 70 OSA Y 0 70 F
44. ers or those needing a refresher the Beamline Staff will go through all the steps for enabling the beamline and setting up and optimizing the microscope during the first shift and any subsequent shifts as needed The SM Beamline Staff will provide the User with a Quality assurance checklist that shows that the STXM microscope is performing as expected Figure 2 1 2 2 SM Beamline Specific Orientation BSO After successfully completing the CLS safety training the User must also complete the SM Beamline Specific Orientation BSO given by the SM beamline staff The BSO training takes about 20 min and we ask that you show up at least 20 mins prior to the start of your shift to complete the BSO if possible For other times make arrangements with the beamline staff Note to validate the Experimental permit requires that both the staff and User sign the BSO document only with both parties signature on the permit will the User be permitted to operate the beamline The BSO must be completed every 2 years 2 3 Laboratory Permits Laboratory permits are required to use the wet laboratories Rm 1071 amp 1080 and must be posted in the laboratories at all times during the beamline shift All persons listed on the Laboratory permit must have completed the laboratory safety module and the date on which it was completed must also be on the permit 2 4 Permit amp Pink Sheet Prior to using the beamline the permit must be signed by both a beamline St
45. for the information To set up your laptop requires that you map your network drive and select the appropriate computer and folders 1 Map the Network Drive For Windows 7 computers Click START COMPUTER then Map Network Drive opening to another screen Figure For XP computers Right Click START then select Explore then Right Click Network Places and select Map Network Drive opening to another screen Figure G1B 2 In the FOLDER option For the STXM Control computer enter station8 107 sm_stxm click Finish For the Optical Microscope computer enter WKS W0000120540 VLM data click Finish Note that this only needs to be done once on your computer Alternatively can access the data on the STXM Control computer using the Windows Map_Network_Drive feature by entering station8107 sm_stxm in the address window of Explorer Fig G2 10 1 CLS SM STXM MANUAL 66 Version 24 October 2011 10 1 CLS SM STXM MANUAL 67 Version 24 October 2011 Accessing data from outside the CLS using an ftp program In order to access your CLS SM experimental data from outside the CLS it is necessary that the data be copied to the ftp data server which can only be done from the STXM computer at the CLS If your data is not in the ftp data server 1 not copied yet and you are no longer at the SM beamline email the Beamline staff to complete the ftp data transfer Data transfer to
46. he Destination box or the Energy for your experiment and either press the button or Enter This will calculate the position that the zone plate should move to using the current Ao value Note that the Ao value is the expected sample position relative to the OSA Thus the focal length f is calculated based on the distance of the zone plate from the OSA Z and the distance from the OSA to the Sample Ao f Z Ao Ao increases with increasing energy The reason that we change the Ao instead of just moving the zone plate further back from the OSA is due to alignment issues and physical constraints So if we move from higher energy to lower energy the calculation of the new focal length is based on the Ao from the higher energy subsequently the zone plate position is moved closer to the OSA to satisfy f Z Ao Consequently the zone plate may crash into the OSA when moving from higher energy to lower energy 5 Change Ao to the recommended value To see the recommended Ao value click on the S box next to the box AUTO or STATIC displayed Fig 5 4 which opens into a new window Figure 5 5 The maximum Ao for the current energy estimation is shown on the bottom right Select an Ao value less than the maximum usually within about 50 um of the Ao maximum The exact Ao value is not that critical as the zone plate position will adjust accordingly Input the new Ao top left and click OK Also notice the zone plate tha
47. igure 6 5 A OSA scan parameters OSA scan at 300 eV 70 x 70 um OSA scan at 300 eV of the OSA and ZP 300 x 300 um and when ZP in focus is checked Begin Scan 30 000 50 0 30 1 667 Dwell ms E pum v 0000 000 gt peon 4 gt z Centre Pos um Range Points Step um A Sta is 2 1557 3 200 0 30 1 6 66667 Recorded Load Sean Channels Definition 05 maim 1t Points Step lim Energy eV Theta Figure 6 6 A Normal OSA focus scan parameters B Green line on OSA image C OSA focus scan 10ID 1 CLS SM STXM MANUAL 42 Version 24 October 2011 6 3 OSA Scan The purpose of the OSA is to filter out zero order light Appendix F requiring that the OSA be well aligned with the beam The OSA Scan menu can be accessed from the Scan Control by dragging down to the OSA Scan Fig 6 3 The usual parameters for an OSA scan are shown in Figure 6 5A Make sure that the ZP in focus box is not checked at this time Click Begin Scan and the expected result of a well centered OSA at 395 eV is shown in Figure 6 5B To align the OSA estimate the centre of the OSA 1 bright circle and move the cursor to the centre of the OSA by clicking on the OSA image which will activate the OSA to Cursor Set to 0 0 button on the left hand side under the image display window not shown appears in place of the Sample
48. ition Variable dwell time A Variable Dwell Time Read File Energy eV Figure 6 4 A Detector scan parameters detector scan image 10ID 1 CLS SM STXM MANUAL 40 Version 24 October 2011 detector is probably not connected to the STXM computer Consult with the Beamline Staff for possible solutions 5 Open the shutter on the STXM Control GUI by changing the AUTO to OPEN Fig 6 3 There should be an increase in the number of counts Usually we expect around 800 000 counts at 395 eV depends on exit slit size zone plate and whether the microscope has been optimized Nevertheless as long as the counts were observed to increase e g 2000 when the shutter was opened it should be possible to optimize the microscope using the procedures outlined below Note the shutter is usually left in the AUTO position opening automatically when acquiring data 6 If there was no increase in the counts it indicates that the beam is possibly being blocked To trouble shoot consider the following a PMT detector is turned on b You are in an open hole on the sample plate c Valves are opened d OSA is aligned see below e Detector is aligned see below 6 2 Detector Scan For the best sensitivity the detector needs to be aligned with the beam The Detector Scan menu can be accessed from the Scan Control by dragging down to the Detector Scan Fig 6 3 usual paramet
49. larization Setup The helical APPLE II type undulator for 10ID 1 Spectromicroscopy beamline is designed to produce plane Horizontal and vertical circular and linear polarized lights with the polarization planes inclined at any angle It consists of four magnet assemblies that are designed to move longitudinally relative to each other as shown in Figure 7 1 The top and bottom girders can be moved vertically to change the gap and the four assemblies or rails in the longitudinal direction to change the phase lt 2 7 pp he Au Following S Sasak Figure El Schematic of the elliptically polarizing undulator Attwood 2005 The following list describes the positions of the magnet assemblies in relation to the operating parameters 1 Circular polarization Two assemblies on the extreme opposite sides are moved in the same direction Parallel mode 2 Plane polarization a Horizontal Four assemblies are at the same position longitudinally b Vertical Like case 1 for circular polarization but the longitudinal movement length is equal to the undulator period length c Inclined Like case 1 but the assemblies are moved in the opposite directions to each other antiparallel mode 1 upper left moved forward and the lower right moved backward 10 1 CLS SM STXM MANUAL 62 Version 24 October 2011 Zone Plate OSA STXM Sample Plate Detector Zon
50. lete New Users Registration and users with expired badges must complete update their mandatory training prior to access to the experimental floor and laboratories Please login and view your Experimental Permit at Proposals to identify any additional training or controls to be followed prior to the start of your experiment These training modules can be completed online prior to arrival at the CLS This is strongly recommended since it saves a considerable amount of time during the check in process at the User Services Office Note the training database is currently housed on a separate server therefore if you have not received login details specifically for the training database please contact mailto clsuo lightsource ca for details The CLS User Services office hours are Monday to Friday from 8 00 a m to 4 30 p m 10 1 CLS SM STXM MANUAL 9 Version 24 October 2011 10 1 CLS SM STXM MANUAL 10 Version 24 October 2011 1 4 Sending Samples and Equipment to the CLS To ensure the safe and timely delivery of all packages shipped To and From the CLS please follow the instructions detailed on http www lightsource ca uso shipping php for labeling packing and shipping e Due to lack of storage space we request that your equipment arrive no more than one week before your beamtime e Users are responsible for the cost of transportation and customs clearance for shipments C O D packages will not be accepted e All packages must be
51. mended order for enabling the beamline 4 1 Starting the STXM Branch Graphical User Interface Usually the STXM Branch Graphical User Interface GUI Fig 4 1 is already running and is visible on the SM Beamline Control monitor Display 3 located in the STXM hutch left of the STXM Control Monitor Fig 3 2B If the STXM Branch GUI is already running proceed to Section 4 2 otherwise The STXM Branch GUI can be accessed from the SM beamline Control Computer located outside of the STXM hutch Fig 3 3C 1 Make sure you are on the STXM display window and not the SM PEEM or OTHER window Fig 4 2 button located on the task bar displayed on SM Beamline Control Computer monitor Display 2 This may be the problem if you are not seeing the STXM Branch GUI 2 To access the STXM Branch GUI click on the runSTXM shortcut on the desktop display Display 2 which opens to the SM Beamline Control monitor Display 1 Drag the STXM Branch GUI onto the SM Beamline Control monitor Display 2 which will also be displayed on the SM Beamline Control Display 3 in the STXM hutch next to the STXM Control computer monitor 4 2 Branch Selection Ensure that the STXM branch is selected which is indicated in the Branch amp Grating Selection section of the STXM Branch GUI Fig 4 1 Change from the PEEM branch to the STXM branch by clicking on the PEEM icon and dragging down to the STXM icon The changeover is c
52. n X ray Microscope PEEM X ray Photoemission Electron Microscope ACIS Access Control Information System STXM Branch GUI STXM Branch Graphical User Interface SM BEAMLINE GUI SM Beamline Graphical User Interface STXM Control Name of STXM control program STXM_CONTROL_GUI STXM Control Graphical User Interface cff Constant of fixed focus 10 1 CLS SM STXM MANUAL 3 Version 24 October 2011 10 1 CLS SM STXM MANUAL 4 Version 24 October 2011 Scope of the Document The purpose of this manual is to help novice and less experienced Users to set up the SM beamline and set up and optimize the STXM End station i e the microscope in a step by step procedure including snap shots of the actual buttons to push Many of the steps are discussed in detail giving the User some insight into what they are doing and what the expected outcome should be After following the steps in this manual the User will be able to enable the SM beamline Part A and set up Part B and optimized Part C the STXM Microscope setting the stage for Data Acquisition For detailed discussion on Data Acquisition see the STXM USER MANUAL Note that the SM Beamline needs to be enabled first prior to setting up the STXM microscope Also included is a section on gas calibration There is also an Appendix section that deals with Sample Preparation Sample analysis Sample Loading Unloading Zone plate and sample relationship data transfer data analysis etc This manual als
53. n to LinInc and enter the appropriate value for the angle To obtain the actual angle required a value needs to be entered into the ANGLE box The value to enter is determined by adding 100 to the angle required For example for an actual angle of 80 enter the value 20 80 100 See Table 5 3 for the values for angles for every 10 starting at 80 10 1 CLS SM STXM MANUAL 35 Version 24 October 2011 10 1 CLS SM STXM MANUAL 36 Version 24 October 2011 5 6 Constant of Fixed Focus Cff The constant of fixed focus Cff value controls the angles for the M1 mirror and the grating of the PGM which determines the amount of the reflected and diffracted light hitting the M3STXM mirror Generally the higher the reflected light the better the spectral resolution while the higher the diffracted lighted the higher the flux Usually the Cff value is set at 2 15 a value that gives a resolving power over 3000 and good flux By increasing the Cff value the resolving power will increase at the expense of the flux Appendix J The Cff value is displayed on the STXM BRANCH GUI but can only be changed from the SM Beamline Control GUI not shown To change the Cff value consult with Beamline Staff 10 1 CLS SM STXM MANUAL 37 Version 24 October 2011 Figure 6 1 Photomultiplier Tube PMT High Voltage Controller on top of the STXM Tank Remember to turn off the High Voltage when opening the STXM Tank to light HE counterO 28
54. ndstation is being accessed thereby protecting the User from the X rays 1 To Open Close the SM PSH or BSH shutters click on the OPEN or CLOSED buttons Fig 4 5 2 Click the OpenBM button There should now be beam to the STXM End Station Follow the procedures in Section 5 to verify that there is beam to the STXM Microscope 4 5 Closing the SM Beamline at the end of the shift At the end of the shift we want to prevent beam from hitting the mirrors particularly the M1 and silicon nitride window on the zone plate snout as this will extend their life and cut down on carbon contamination This is accomplished by closing the shutters and variable aperture Fig 4 5 1 Close the SM PSH shutter 2 Close the BSH shutter 3 Click the CloseBM button 4 Turn OFF the detector 10 1 CLS SM STXM MANUAL 25 Version 24 October 2011 10 1 CLS SM STXM MANUAL 26 Version 24 October 2011 4 6 Enabling the SM Beamline Quick Guide Enabling the SM Beamline Quick Guide STXM Branch GUI unless otherwise stated 4 0 Enabling the SM Beamline Samples can be loaded at any time 4 1 Start STXM Branch GUI usually already displayed 4 2 Branch Selection Close SM PSH shutter Select STXM branch if on PEEM Branch 4 3 Open safety shutter only after injection Green button on ACIS panel and Open PSH shutter 4 4 Open SM PSH and BSH shutters 4 2 Grating or Branch Change 1 Close SM PSH shutter Branch change onl
55. o provides Users with some useful information including the SM Beamline staff contact information what a User needs to check before their arrival and what the User can expect upon their arrival at the SM Beamline 10 1 CLS SM STXM MANUAL 5 Version 24 October 2011 10 1 CLS SM STXM MANUAL 6 Version 24 October 2011 SM Beamline Staff and Beam Team Leaders Chithra Karunakaran Jian Wang Staff Scientist Staff Scientist Tel 1 306 657 3749 Tel 1 306 657 3546 chithra karunakaran lightsource ca jian wang lightsource ca Yingshen Lu James Dynes Science Associate STXM Research Associate Tel 1 306 657 3743 Tel 1 306 657 3840 Yingshen lu lightsource ca james dynes lightsource ca Adam Hitchcock Stephen Urquhart Beam Team Leader McMaster University PEEM Leader University of Saskatchewan Tel 1 905 525 9140 Ext 24749 Tel 1 306 966 4657 aph mcmaster ca stephen urquhart usask ca web http unicorn memaster ca web http homepage usask ca sgu703 index html 10ID 1 CLS SM STXM MANUAL 7 Version 24 October 2011 Past SM Beamline Staff Uday Lanke Martin Obst PEEM Research Associate STXM Research Associate Martin obst uni tuebingen de Drew Bertwistle Kon Kaznatcheev Science Associate Staff Scientist drew bertwistle lightsource ca kaznatch bnl gov 10ID 1 CLS SM STXM MANUAL 8 Version 24 October 2011 1 0 Checklist before your Arrival 1 1 Confirm SM beamline time The CLS User Services office
56. omplete when the yellow not in position disappears and is replaced by Branch 2 STXM 4 3 Safety and Photon Shutters Access Control Information System Panel To protect the SM beamline each section is separated by valves that can isolate each section automatically in the case of a sudden pressure increase or are used to isolate sections during scheduled maintenance beamline development Shutters are located in various spots on the beamline to block X rays from going further downstream in the beamline 10 1 CLS SM STXM MANUAL 21 Version 24 October 2011 Figure 4 3 A Safety SSH and Photon PSH Shutters Access Control Information System Panel located on the wall outside the SM hutch at the start of the SM beamline and B a close up of the panel indicator lights and safety shutter button m SM Beamline Control System 10ID 1 SM Beamline Control STXM branch RingStatus 0 001 Spring Shutdown PSH1 Val PSH SSH F Val 1 SM PSH 1 PGM M3PEEM M3STXM 5 5 EPU Monochromator EPU Gap zooo 40 2995 pomo 8090108 Q2 am nem 9495 Q4 Eoo Taper pooo 0015 MONOCHROMATOR Mirror 36415 65 36419 39 Grating 49705 86 49705 99 6 REIXS EPU 1 Branch amp Grating Selection Mote To change branch or grating the SM photon shutter SM PSH has to be closed Beier step SelectBranch BRANCH 2 STXM SelectGrating Les mes To
57. ook at Appendix D before proceeding 5 1 Zone Plate Selection There are a number of Zone Plates that can be used defined by their spatial resolution mainly 25 35 and 40 nm For energies before 280 eV the 40 nm zone plate must be used as the focal length of the 25 and 35 nm prevent their use due to physical constraints Only Beamline Staff can change zone plates It takes about 20 30 mins to change a zone plate and set up the microscope again Experiments should be planned so that the changing of zone plates is kept to a minimum 5 2 Grating Selection The SM beamline has 3 gratings the low energy grating LEG 250 l mm the medium energy grating MEG 500 I mm and the high energy grating 1250 l mm The flux of the gratings is energy dependent thus choosing the appropriate grating depends on the element of interest Table 5 1 shows the photon energy range of each grating and the photon flux as a function of energy Fig 5 2 10 1 CLS SM STXM MANUAL 29 Version 24 October 2011 SM Beamline Control System 1 Branch amp GratingSelection Mote To change branch or grating the SM photon shutter SM PSH has to be closed Beier step 2 SelectBranch SelectGrating See To change grati 3 when it is done then select grating OpenBeamline SSH GLOSED OpenBM PSH 020508 OPEN CLOSE SM PSH GioSED BSH CIOSED Openvetose beam CEE Energy Selection If you want
58. otoemission electron microscope PEEM Fig 3 1 The STXM branch has 1 mirror M3STXM and the PEEM branch has 2 mirrors M3PEEM M4PEEM Fig 3 1 Note that only 1 branch is operational at any one time since the M3PEEM mirror must move in front of the M3STXM mirror in order for the PEEM end station to receive beam There are 2 separate computers one for operating the SM Beamline 1 SM Beamline CONTROL and one for the STXM i e STXM CONTROL The User is not permitted to use the SM Beamline Control computer unless otherwise directed by the SM Beamline staff The STXM hutch consists of the STXM endstation Tank and the STXM CONTROL Computer and display 3 for the SM Beamline CONTROL computer Fig 3 2 The SM Beamline work area is located outside the STXM Hutch consisting of an area for mounting samples along with an Optical Microscope VLM for previewing the samples Fig 3 3A For more detailed sample preparations such as those involving a reaction the User is to use the wet labs 1071 1080 There is also a User Work area available for data analysis with space enough for 3 computers Fig 3 3B The SM Beamline Control computer work area is shown in Fig 3 3C Table 3 1 summarizes the important parameters of the SM beamline The energy range of the SM beamline is from 130 to 2500 eV soft X ray A table of the elements accessible in the energy range of the SM beamline as well as the specific edge energy range grating
59. r i e sample do move during data acquisition The zone plate will change position as it is a function of the energy The Ao value is the expected sample position relative to the OSA The zone plate uses the Ao in its calculation to determine its relative position to the OSA Thus the focal length f is calculated based on the distance of the zone plate from the OSA Z and the distance from the OSA to the Sample Ao f Z Ao increases with increasing energy The reason that we change the Ao instead of just moving the zone plate further back from the OSA is due to alignment issues and physical constraints So if we move from higher energy to lower energy the calculation of the new focal length is based on the Ao from the higher energy subsequently the zone plate position is moved closer to the OSA to satisfy f Z Ao Consequently the zone plate may crash into the OSA when moving from higher energy to lower energy gt T 1 Sample Holder Figure F3 Layout of zone plate ZP OSA Sample Holder and detector 10 1 CLS SM STXM MANUAL 64 Version 24 October 2011 Map Network Drive Map Network Drive Windows can help you connect to shared network folder and assign a drive letter to the connection so that you can What network folder would you like to map access the folder using My Computer Specify the drive letter for the connection and the folder that you want to connect to Specify the drive letter
60. rization planes inclined at any angle see Appendix C for more details For nonmagnetic samples where no change in polarization is required 3 settings are available LinHor CirLeft or CirRight The polarization influences the flux at a selected energy thus the polarization selection depends on the element of interest The recommended polarization for each energy range is shown in Table 5 1 or for each element in Appendix A Note initial optimization of the microscope is usually done at 395 eV just below the N K edge so initially use the values for K edge 1 polarization either CirLeft or CirRight la To change polarization enter the appropriate value in the EPU Polarization box CirLeft 1 CirRight 1 LinHor 0 IntVert 90 2 and IntVert 90 2 Table 5 2 on the STXM Control GUI see Fig 5 6 or click on the MODE button in the STXM Branch GUI Fig 4 1 and drag down to the appropriate polarization The advantage of making the change in the STXM Control GUI is that the polarization used is recorded with the data otherwise the previous polarization is recorded with the data For magnetic samples where a change in polarization is required e g X ray magnetic circular dichroism XMCD studies the angle can be varied from 20 to 180 degrees 1b To change polarization enter the appropriate value in the EPU Polarization box Table 5 3 on the STXM Control GUI or click on the MODE button and drag dow
61. t is currently being used indicated by the round circle being filled 6 Change the zone plate focus back from STATIC to AUTO If this is not done the zone plate position will not change with a change in energy 7 Click on the energy button Observe that the Zone Plate position changes At this time it would be advantageous to look through the STXM Tank viewport and estimate the distance between the zone plate and the OAS The expected value is that shown by the ZonePlate box If you think the zone plate and OSA are touching you may need to open the STXM Tank Note if the zone plate and OSA are touching and you continue to acquire data irreversible damage may result to the zone plate and or the OSA Call the Beamline Staff to assist you before damaging that 10 000 zone plate 10 1 CLS SM STXM MANUAL 33 Version 24 October 2011 STXM Control Program 28 Feb 2011 le Setup Window Help orage Ring Current Boe setas to countero lS A110211021 hdr A110115007 hdr chart 7 Scan 111000 110000 108000 106000 104000 un J TT 255 Loading scan A110115022 hdr Alf PMT 10 Reading file A110115022_0 xsp 2 E Data STXM data 2011 2011_01 110115 A110115022 hdr loaded success Shutter Loading scan A110115007 hdr e m ll Auto Reading file A110115007_0 xsp sampev J o Sample To Cursor 1055 Sample To Cursor 800 Coarse
62. table for STXM measurements Consult with the Beamline staff for more information Samples can also be prepared using Focused ion beam FIB milling Fig C1D Radiation damage is a possibility consult with the Beamline staff for more information 10 1 CLS SM STXM MANUAL 58 Version 24 October 2011 10 1 CLS SM STXM MANUAL 59 Version 24 October 2011 Appendix D Data Analysis The data is routinely analyzed using the aXis2000 software The Beamline staff is familiar with aXis2000 and can assist Users in using it for data analysis aXis2000 is freeware and is maintained by Adam Hitchcock The aXis2000 program and the IDL virtual machine package from ITT Visual Information can be downloaded from http unicorn mcmaster ca Users that do not have an IDL License must use the IDL Virtual Machine Version If you have trouble getting the aXis2000 program to run prior to your arrival at the SM beamline the Beamline staff will be able to help you install it at the time of your arrival There are some aXis2000 manuals tutorials available that can help New Users at http exshare lightsource ca sm Documents axis2000 pdf http unicorn mcmaster ca aXis2000 html Note however the manuals are dated and significant changes have been made to the aXis2000 program and some routines may no longer be applicable 10 1 CLS SM STXM MANUAL 60 Version 24 October 2011 10 1 CLS SM STXM MANUAL 61 Version 24 October 2011 Appendix E SM Beamline Po
63. the CLS ftp data server is done from the STXM Control computer 1 Double click the copy STXM data icon on the desktop This will copy the data files from STXM Control to the ftp data server Note the VLM data is also accessible provided that it was copied previously from the Optical Microscope using the copy VLM data icon on the desktop 2 Use your ftp program to connect to the CLS ftp data server Port 21 Hostname ask the Beamline Staff or look in the Manual at the SM beamline Username ask the Beamline Staff or look in the Manual at the SM beamline Password ask the Beamline Staff or look in the Manual at the SM beamline 3 Your data is in the sm user STXM data folder 10ID 1 CLS SM STXM MANUAL 68 Version 24 October 2011 10 1 CLS SM STXM MANUAL 69 Version 24 October 2011 Appendix H Connecting to the Printer in the STXM hutch Printer name prd cp3525n e 0 Windows 7 machines CA B WN ON N Click Devices amp Printers Click Add Printer Click Add Network wireless or Bluetooth printer Click The printer that I want wasn t listed Click NEXT Select Select a shared printer by name Enter in box vsrv print 01 prd cp3525n e 0 May actually give you list of printers before entering a printer name Click Next Should indicate you have been successful Click next 0 Click finish XP machines 1 5 6
64. the EPU or grating tracking OFF during a scan Please contact the beamline staff Harmonic __ Mode Ange 22407777 Epu oftset Energy eV 30087 1 SM PSH 4 M3STXM STXM ES E 8 8 10 12 13 14 15 16 EPU Monochromator Valves amp Vacuum EPU CA 1 166e 10 Gap 200 0000 40295 Sec2 Gal 3 829 11 Qi 0 0000 000 Sec 4 Gal 9 1367 09 Q2 0000 400025 Sec 6 MJ 1 6674 10 900 AEM 48076 10 Q3 9 0000 19 0025 Sec 8 DJ EE 3 885 10 04 0 0000 i memo oes Taper 2 0000 aus Sec 10 6 148e 10 ooo MONOCHROMATOR Sec 11 21 EM 6 761 10 36415 65 Mirror 3641929 Sec 12 DJ 514 5 026e 10 ooo 49705 86 Grating 9705 99 Sec 13 1089 10 ooo STXM Sec 14 10956 09 Sec 15 jai 51 3 970 10 Sec 16 21 5 210 10 Pressure should be lt 5E 9 before opening any valve Updated 26Jan2011 Contacts Jian Wang 3546 Yingshen Lu 3743 Jay Dynes 3840 Figure 5 3 STXM Branch Graphical User Interface 10 1 CLS SM STXM MANUAL 30 Version 24 October 2011 Note changing the grating will result in the energy being changed 1 To change gratings first click on the HOME button on the STXM Branch GUI Fig 5 3 this moves the tank to a set position The green button will change to yellow when the t
65. the End Station should be opened to atmosphere if it was filled with He as He is very difficult to pump 4 Fill the STXM Tank with the recommended pressure of gas Table 7 2 using the digital gauge If too much gas is allowed into the Tank pump the excess gas out until the desired pressure is reached 5 Select the size of the Exit Slits Table 7 2 6 Collect a Point Scan through an empty hole The calibration parameters are found in the Folder Gas Calibration 7 Examples of the spectra are shown in Figure 7 2 next page Table 7 2 Parameters used for the Compressed Gases Edge Gas Pressure Torr Exit Slit Size um Carbon 3 30 30 Nitrogen 2 30x30 Oxygen Air or T 30x30 Neon Ne 20 10x10 Fluorine SF 3 15x15 Sulfur SF The gauge has trouble reading the Neon so fill to 10 Torr and it will continue to increase 10 1 CLS SM STXM MANUAL 51 Version 24 October 2011 A110115007 hdr Chart 1 Scan B Belt Serasio countero 111000 Cls 106000 104000 Expected 294 96 eV 294 03 eV Actual Difference 0 93 eV 2935 294 029 Al 294 2945 95506 6 counter0 suse 120000 Expected 539 0 eV Actual 538 95 eV Difference 0 05eV 90000 85000 E 1 537 5 538 538 5 539 539 5 540 5404 538 95 85277 A110603090 hdr Chart scan 2
66. y necessary if on PEEM branch a Click on PEEM icon and drag down to STXM icon Grating change a Click when complete indicates DONE b Click the appropriate grating e g LEG MEG HEG when complete a number is indicated 250 LEG 500 MEG 1250 HEG 2 Open SM PSH shutter Sample Change Appendix B 1 Close SM PSH and BSH shutters 2 Turn OFF the Detector 3 Move Coarse 7 to 5000 um 4 Open vent valve to let air into the STXM End Station 4 5 Closing the Beamline at the end of the shift 1 Close SM PSH and BSH shutters 2 CloseBM 3 Turn OFF the Detector 10 1 CLS SM STXM MANUAL 27 Version 24 October 2011 Windows To begin click your user name stxm_admin Figure 5 1 STXM Control window when the computer restarts Table 5 1 Preferred grating and harmonic settings as a function of photon energy i ud Grating Hamont Polarization 1 LinHor CirRight 130 to 750 LEG CirLeft st LinHor CirRight 330 to 1000 MEG 1 CirLeft 1000 to 1800 MEG 3 LinHor 1800 to 2500 MEG LinHor gt 2200 HEG 5 or 7 not well characterized LinHor cff 2 0 for all cod except 3rd Sth 7th cff 2 5 S 510 Il 11 o a 6 Zi 2 4 v 1 st Harmonics 2 10 LEG MEG HEG 10 3rd Harmonics im B MEG x LEG 250 I mm 3 408 Pth Harmonics 3 MEG 500 I mm m MEG HEG E p 12

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