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STANDARD OPERATING PROCEDURE:

BRUKER D8 DISCOVER XRD (THIN FILM SAMPLES)

Purpose of this Instrument: The Bruker D8 Discover XRD is used for phase analysis of polycrystalline films,

characterizing single crystal and epitaxial films, and powders.

Location: 211 ERB

Primary Staff Contact: Weiqiang Ding (304) 685-1938 cell weiqiang.ding@mail.wvu.edu

Secondary Staff Contact: Harley Hart (412) 443-1514 cell harley.hart@mail.wvu.edu

The Shared Research Facilities are operated for the benefit of all researchers. If you encounter any problems with

this piece of equipment, please contact the staff member listed above immediately. There is never a penalty for

asking questions. If the equipment is not behaving exactly the way it should, contact a staff member.

WARNING: This system generates x-rays. Radiation is monitored by a room dosimeter as specified by WVU

Radiation Safety.

START-UP

1. Sign-in on the FOM and the system log book – see Figure 1.

Figure 1: Screenshot of WVU FOM website at http://fom.wvu.edu/fom.

2. Verify the water recirculator tank is full. This is done by checking that the FULL light is illuminated on the water chiller panel - see Figure 2.

FULL Light Indicator

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Figure 2: FULL light indicator on XRD water recirculator.

3. Open the XRD Commander software on the computer desktop.

4. The idle power state of the tool is 20 kV / 5 mA (Figure 3a). Incrementally increase the HV generator power by setting the voltage and current to the following settings and pressing the SET icon (Figure 3a):

20 kV / 10mA – wait 5 minutes

20kV / 20 mA – wait 5 minutes

30kV – 20 mA – wait 5 minutes

30kV – 30mA – wait 5 minutes

40kV – 30 mA – wait 5 minutes

40kV – 40 mA – wait 5 minutes (this is final set-point)

5. Press the green DOOR button on the side of the tool to unlock the radiation enclosure doors. Listen for the safety latches to release and then open the doors by pulling outwards on the handles and sliding the doors to the side – see Figure 3b.

(a) (b)

Figure 3: (a) Commander program window; (b) System side panel showing OPEN DOOR LOCATION

6. Attach the desired stage and shims to the system. The z-scan will determine if shims need to be added or removed. Shims need to be added if the detector records excessive counts and shims will need to be removed if the detector records zero counts.

Vacuum Stage: This stage uses backside vacuum to hold the sample in place – see Figure 4.

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Figure 4: Image of Vacuum stage.

Goniometer Stage: This stage requires adhesive on the backside of the sample to hold the sample in place – see Figure 5.

Figure 5: Image of Goniometer stage.

Clip Stage: This is ideal for samples on glass slide. This stage uses side clips to hold the sample in place – see Figure 6.

Figure 6: Image of Clip stage.

Hot Stage: This stage uses clips over the sample to hold the sample in place – see Figure 7.

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Figure 7: Image of Hot Stage.

NOTE: If the Hot Stage is to be used, a Shared Facilities staff member needs to be contacted so that the system configuration can be changed.

7. Place the sample on the center of the stage and gently close the system doors. – see Figure 8. Verify that the doors are properly closed (cannot pull open, no red alarm on side panel Figure 3).

Figure 8: Image of a sample placed at the center of the Vacuum Stage.

Warning: If the doors are not closed properly before operating the tool, the system safety interlock will fail and the tool will shut-down the x-ray source. If this occurs, contact a Shared Research Facilities staff member immediately.

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SILICON 111 STANDARD SAMPLE CALIBRATION PROCEDURE

NOTE: Use stage shims #1 and #3 for the calibration.

1. Insert the proper monochromator slits (1.0mm, 0.8mm, NO DETECTOR SLIT) – see Figure 9 below.

Figure 9: Monochromator slit set-up for alignment.

2. Set the Chi drive to 0° and select the MOVE ALL DRIVES icon . The Chi drive will move into a vertical position on the diffractometer.

3. Enter the DETAILS screen (Figure 10). Change the detector setting to 0D and set the opening to 0.075mm. Press the SET DETECTOR icon to change the opening size. NOTE: Alignment can only be done in 0D mode.

Figure 10: Screenshot of Details Screen.

NO DETECTOR SLIT 1.0 mm monochromator slit

0.8 mm monochromator slit

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4. Click the ADJUST tab. Run a DETECTOR (2Θ) scan in Scantype using the following settings:

Scan type: Detector

Z: - 0.9 mm

Absorber: 10

Scan Start: - 0.5o

Scan Stop: 0.5o

Increment: 0.001o

Scan speed: 0.1 sec/step

Mode: Continuous

Figure 11. Scantype selection in ADJUST tab.

5. Zoom-in over the peak and select the mid-point of the peak. This value will automatically be entered into the 2Θ Requested Position. Use the MOVE ALL DRIVES icon to move the 2Θ -drive to this position –see Figure 12.

Figure 12: Screenshot of Detector scan

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6. Run a Z scan using the following settings:

Scan type: Z

Absorber: 10

Scan Start: - 0.9 mm

Scan Stop: 1.9 mm

Increment: 0.01 mm

Scan speed: 0.5 sec/step

Mode: Continuous

Once the scan is complete, ZOOM in over the sloped area. Select the USE ZOOM icon which will adjust the scan range (start/stop) to the range of zoom. Change the increment to 0.001 and then repeat. After the second scan, select the mid-point of the sloped area. This value will automatically be entered into the Z Requested Position. Use the MOVE ALL DRIVES icon to move the z-drive to this position. This will move the sample halfway into the x-ray beam – see Figure 13.

NOTE: The range of the Z-drive is limited from - 0.9 to 1.9. If the sloped graph is not seen, then shims will need to be added/removed to allow the sample to be properly aligned.

Figure 13: Screenshot of Z-scan.

7. Run a Rocking Curve (Θ) scan using the following settings:

Scan type: Rocking Curve

Absorber: 10

Scan Start: - 1o

Scan Stop: 1o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

Use the MOVE ALL DRIVES icon to move the Θ-drive to this position. This will adjust the sample surface so that it is parallel to the x-ray beam – see Figure 14.

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Figure 14: Screenshot of Rocking Curve

8. Repeat steps 5 and 6 until a less than 1% change is verified on both the Z and Θ drives.

9. Enter 28.443 into the 2Θ Requested Position. Check the 2Θ box and select the MOVE ALL DRIVES icon.

10. Run a Rocking Curve scan using the following settings:

Scan type: Rocking Curve

Absorber: 1

Scan Start: 14o

Scan Stop: 15o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

Zoom-in over the peak and select the mid-point of the peak. This value will automatically be entered into the Θ Requested Position. Use the MOVE ALL DRIVES icon to move the 2Θ drive to this position.

11. Run a Chi scan using the following settings:

Scan type: Chi

Absorber: 1

Scan Start: - 3o

Scan Stop: 3o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

Note: If a dip is observed as that shown in Figure 15 in the peak of the Chi scan, then the Chi-scan will need to be manually adjusted. This is done by entering changing the Chi-scan requested position by increments of 0.1 and repeating the rocking curve until a Rocking Curve with maximum intensity is observed. Then repeat the Chi-scan – see Figure 16.

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Figure 15: Screenshot of Chi-scan with a dip in the peak.

Figure 16: Screenshot of Chi-scan after manually adjusting the Chi by increments of 0.1.

12. Run a Rocking Curve scan using the following parameters – see Figure 17:

Scan type: Rocking Curve

Absorber: 1

Scan Start: 14o

Scan Stop: 15o

Increment: 0.0005o

Scan speed: 0.1 sec/step

Mode: Continuous

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Figure 17: Screenshot of Final Rocking Curve

13. Save the scan file as .raw file and open the EVA analysis software. The FWHM should be 0.0035. In the XRD Commander software, double-click over the peak and select the mid-point of the peak. This value will automatically be entered into the Θ Requested Position. Use the MOVE ALL DRIVES icon to move the Θ-drive to this position.

14. Insert a 0.1 mm detector slit. Enter the DETAILS screen (Figure 10). Set the opening to 14.025mm Change the detector setting to 1D. Press the SET DETECTOR icon to change the opening size.

15. Run a 2Theta/Omega Scan using the following parameters – see Figure 18:

Absorber: 1

Scan Start: 28o

Scan Stop: 29o

Increment: 0.0005o

Scan speed: 0.1 sec/step

Mode: Continuous

Figure 18: Screenshot of 2Θ-Omega scan.

16. Once the scan is complete, save the data by selecting FILE SAVE AS .RAW. Saving the information as a .raw file will enables the user to import the information into EVA or LEPTOS.

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17. To remove the sample, first move the Θ-drive back to home position by entering zero in Θ-Requested drive position. Uncheck all DRIVE boxes except for the Θ-drive before selecting the MOVE ALL DRIVES icon.

Warning: Failure to move the Θ- drive back to the home position first can result in the crashing of the 2Θ- Θ drive. This will cause the tool to shut-down and needed to be reset. Furthermore, serious damage can occur to the tool detector and drives.

18. Check all drive boxes and set the drives to the following positions:

2 Θ: 0o

Phi: 0o

Chi: 90o

X: 0

Y: 0

Z: 0

19. Once all drives have reached the home positions, press the green DOOR button on the side of the tool to unlock the radiation enclosure doors. Listen for the safety latches to release and then open the doors. Remove you sample from the stage.

Note: If a stage other than the vacuum has been used, first remove the stage and then install vacuum stage.

20. Close the radiation enclosure doors and verify that the doors are properly closed (cannot pull open).

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THIN FILM SAMPLE SOP

1. Insert the proper monochromator slits (0.1mm, 0.8mm, 1.0mm) – see Figure 19.

2. Close the radiation enclosure doors and verify that the doors are properly closed (will not open when you pull).

Figure 19: Image of monochromator slit locations.

Warning: When inserting the monochromator slits, be sure to insert the slits in a vertical direction and verify that the slits are securely in place. Failure to do this can result in damage to the tool.

3. In the XRD Commander software, set Chi to 0° and select the MOVE DRIVES icon . The Chi drive will move into a vertical position on the diffractometer – see Figure 20 below.

Figure 20: Image of diffractometer with Chi at 0°

4. Enter the DETAILS screen in the XRD Commander software (Figure 21). Change the detector to 0D mode and set the opening to 0.075mm. Then press the SET DETECTOR icon to change the size of the opening – see Figure 21.

0.1mm monochromator slit

1.0 mm monochromator slit

0.8 mm monochromator slit

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Figure 21: Screenshot of Details Screen.

5. Select Adjust tab (Figure 22a) at the bottom left corner of the program window. In the Scantype pull-down menu, choose DETECTOR (2Θ) scan. Set the following scan settings and then click Start icon to start the scan:

Scan type: Detector

Z: - 0.9 mm

Absorber: 10

Scan Start: - 0.5o

Scan Stop: 0.5o

Increment: 0.001o

Scan speed: 0.1 sec/step

Mode: Continuous

Zoom-in over the peak and select the mid-point of the peak. This value will automatically be entered into

the 2Θ Requested Position. Press the MOVE ALL DRIVES icon to move the 2Θ -drive to this position –see Figure 22b.

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Figure 22: (a) Scan type selection; (b) Screenshot of an example of a final Detector Scan.

6. Run a Z scan (from Scantype menu) using the following settings:

Scan type: Z

Absorber: 10

Scan Start: - 0.9 mm

Scan Stop: 1.9 mm

Increment: 0.01 mm

Scan speed: 0.5 sec/step

Mode: Continuous

Once the scan is complete, ZOOM in over the sloped area. Select the USE ZOOM icon which will adjust the scan range (start/stop) to the range of zoom. Change the increment to 0.001 and then repeat. After

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the second scan, select the mid-point of the sloped area. This value will automatically be entered into the Z Requested Position. Use the MOVE ALL DRIVES icon to move the z-drive to this position. This will move the sample halfway into the x-ray beam – see Figure 23.

Figure 23: Screenshot of an example of a final Z-scan.

Notice: The range of the z-drive is limited to -0.9-1.9. If the sloped graph is not seen, then shims will need to be added/removed to allow the sample to be properly aligned.

7. Run a Rocking Curve (Θ) scan (from Scantype menu) using the following settings:

Scan type: Rocking

Absorber: 10

Scan Start: -1o

Scan Stop: 1o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

Once the scan is complete, ZOOM in over the sloped area. Select the USE ZOOM icon which will adjust the scan range (start/stop) to the range of zoom. Change the increment to 0.001 and then repeat. After the second scan, select the mid-point of the peak. This value will automatically be entered into the Θ-drive Requested Position. Use the MOVE ALL DRIVES icon to move the Θ-drive to this position. This will adjust the sample surface so that it is parallel to the x-ray beam – see Figure 24.

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Figure 24: Screenshot of an example of a final Rocking Curve.

8. Repeat steps 6 and 7 until a less than 1% change in position is verified on both the Z and Θ drives.

9. Run an X scan (from Scantype menu) using the following settings:

Scan type: X

Absorber: 10

Scan Start: -20 mm

Scan Stop: 20 mm

Increment: 0.01 mm

Scan speed: 0.1 sec/step

Mode: Continuous

Zoom-in over the peak and select the mid-point of the peak. This value will automatically be entered into the X-drive Requested Position. Use the MOVE ALL DRIVES icon to move the X-drive to this position – see Figure 25.

Figure 25: Screenshot of an example of a final X-scan.

10. Go to the DETAILS tab and set the 0D opening to 10 mm.

NOTE: Steps 10 – 21 are for aligning to the Symmetric Substrate Peak

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11. Move 2Θ drive to a theoretical symmetric Bragg peak position of your sample by entering the value into the 2Θ Requested Position. Verify the drive box is checked and press the MOVE ALL DRIVES icon.

12. Run a Rocking Curve scan using the following settings:

Scan type: Rocking Curve

Absorber: 1

Scan Start: (½ of 2Θ value) – 1o

Scan Stop: (½ of 2Θ value) + 1o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

Once the scan is complete, ZOOM in over the parabola. Select the USE ZOOM icon which will adjust the san range (start/stop) to the range of zoom. Change the increment to 0.001 and then repeat. After the second scan, select the mid-point of the peak. This value will automatically be entered into the Θ-drive Requested Position. Use the MOVE ALL DRIVES icon to move the Θ-drive to this position.

13. Perform a Chi scan using the following parameters:

Scan type: Chi

Absorber: 1

Scan Start: -2o

Scan Stop: 2o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

Once the scan is complete, ZOOM in over the parabola. Select the USE ZOOM icon which will adjust the san range (start/stop) to the range of zoom. Change the increment to 0.001 and then repeat. After the second scan, select the mid-point of the peak. This value will automatically be entered into the Chi Requested Position. Use the MOVE ALL DRIVES icon to move the Chi-drive to this position.

14. Repeat step 12 and 13 until the Rocking Curve intensity is optimized for intensity

Note: It is not necessary to revert back to the faster scan values or scan lengths. Use the same scan parameters as those obtained identified in the high resolution scans of the alignment.

15. Run a Detector (2Θ) scan using the following parameters:

Scan type: Detector

Absorber: 1

Scan Start: (2Θ value) – 0.5o

Scan Stop: (2Θ value) – 0.5o

Increment: 0.01o

Scan speed: 0.1 sec/step

Mode: Continuous

0D Opening: 0.225 mm

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Once the scan is complete, ZOOM in over the parabola. Select the USE ZOOM icon which will adjust the san range (start/stop) to the range of zoom. Change the increment to 0.001 and then repeat. After the second scan, select the mid-point of the peak. This value will automatically be entered into the 2Θ Requested Position. Use the MOVE ALL DRIVES icon to move the 2Θ -drive to this position.

16. Run a Rocking Curve and Chi Scans to optimize the intensity of the Rocking Curve. Repeat until a change of less than 1% is seen on the Θ and Chi drives.

17. Run a 2 Theta/Omega scan using the following settings:

Scan type: 2Theta/Omega

Absorber: 1

Scan Start: User Defined (degree)

Scan Stop: User Defined (degree)

Increment: User Defined (degree)

Scan speed: User Defined (sec/step)

Mode: Continuous

0D Opening: User Defined

Make sure you have enough time reserved to finish the scan. Calculate the scan time as follow:

Scan time = ((scan stop – scan start)/increment) x scan speed/3600 ( hr)

18. Once the scan is complete, save the data by selecting FILE SAVE AS .RAW. Saving the information as a .raw file will enables the user to import the information into EVA or LEPTOS.

19. To remove the sample, first move the Θ-drive back to home position by entering zero in Θ-Requested drive position. Uncheck all DRIVE boxes except for the Θ- drive before selecting the MOVE ALL DRIVES icon.

Warning: Failure to move the Θ- drive back to the home position first can result in the crashing of the 2Θ- Θ drivse. This will cause the tool to shut-down and it will need to be reset. Furthermore, serious damage can occur to the tool detector and drives.

20. Check all drive boxes and set the drives to the following the home positions:

2 Θ: 0o

Phi: 0o

Chi: 90o

X: 0

Y: 0

Z: 0

21. Once all drives have reached the home positions, press the green DOOR button on the side of the tool to unlock the radiation enclosure doors. Listen for the safety latches to release and then open the doors. Remove you sample from the stage.

NOTE: If a stage other than the vacuum has been used, then remove stage and install vacuum stage.

22. Close the radiation enclosure doors and verify that the doors are properly closed (cannot pull open).

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SHUT DOWN

1. Using the XRD Commander software, set the HV generator power to 20 kV and 5 mA (idle state) and press

the SET icon – see Figure 26.

Figure 26: Screenshot of idle parameters.

2. Check that all required parameters are recorded in the log book.

3. Clean up the work area by doing the following: a. Clean the zero reflective piece of fused silica with isoprpoanol if it was used b. Place all tools into the storage box

Notice: If the powder has fallen off of your sample into the Chi drive gears, a Shared Facilities staff member MUST be notified so that it can be cleaned and the gears can be properly greased.

4. Properly dispose of any used materials – i.e. alpha wipes, glass slides, etc.

5. Sign out on the log book and sign out of the FOM. Report any problem in the log book and in the problem

report section of the FOM sign out window.

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EMERGENCY PROCEDURES

If no one is available and the machine is not acting as expected, the user should do the following:

Press STOP in the XRD Commander software.

Set the voltage to 20kV and 5mA.

Do not leave the machine running in an abnormal state. If the machine cannot be placed in the default state, immediately contact:

Primary Staff Contact: Weiqiang Ding (304) 685-1938 or Weiqiang.ding@mail.wvu.edu

Secondary Staff Contact: Harley Hart (412) 443-1514 or harley.hart@mail.wvu.edu

The user should then complete a Tool Issue Report form and submit this form to ESB G75D. The user should also

add comment using the FOM software as to tool status.

Then, if possible, the user should stay by the tool while trying to contact a Shared Facilities staff member. If it

becomes necessary to leave the tool then the user should leave a large, legible note at the XRD stating the tool is

DOWN.

If a dangerous situation is evident (smoke, fire, sparks, etc.), ONLY if it is safe to do so, the user should press the

EMO (EMERGENCY OFF) button on the right or left side of the tool and turn off the electrical breaker switch on

wall. The user should then notify all other lab persons within the ERB 211 to evacuate and leave the lab

immediately. The user should then contact proper emergency personnel from a safe place.

Weiqiang Ding (304) 685-1938 (cell)

Shared Research Facilities Manager (304) 293-9683

Harley Hart (412) 443-1514 (cell)

Shared Research Facilities Manager (304) 293-3422 x1460

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