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STANDARD OPERATING PROCEDURE:

PANALYTICAL X’PERT PRO XRD

Purpose of this Instrument: Identification of signal-phase materials and multi-phase mixture; Quantitative determination of amounts of different phases in multi-phase mixture.

Location: Room B-61D Engineering Sciences Building

Primary Staff Contact: Weiqiang Ding (304) 685-1938 cell weding@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. NOTE: The purpose of this manual is for general measurements with the PANalytical X’Pert Pro XRD. For more advanced measurements or measurements with certain accessories, please contact SRF staff members for assistance.

START UP

1. Log in your session on the FOM on the log-in computer on the workbench.

2. Sign in on the logbook located on the workbench next to the log-in computer.

3. Check the X-ray generator display on the XRD instrument display panel (Figure 1). The Voltage should be 45 kV and the Current should be 20 mA. The Shutter should be closed (no display under Shutter open). Contact MCF staff if the XRD is not in the stated idle condition. NOTE: If Shutter open display shows “1” (open) but the XRD is not scanning (angle values do not change),

press the “Shutter close” button to close the shutter. If shutter display shows “”, the doors are not fully closed. Close the doors tight and the display will disappear.

Figure 1. XRD idle state status display

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4. Check the cooling water temperature reading on the chiller next to the XRD. The temperature should be 70 - 74 oF. Contact MCF staff if the temperature is out of the range.

5. On XRD computer desktop, double click “X’Pert Data Collector” icon to start the program.

6. Log in to the X’Pert Data Collector program.

7. In software top menu, select “Instrument > Connect”. A dialog will come up for stage configuration selection (Figure 2). Select “Sample Spinner” from the list and click OK. Contact MCF staff for assistance if you need to use other stages.

8. A dialog window will show up showing the current instrument configuration. Click OK to continue.

Figure 2. Select stage configuration while connecting to the instrument.

POWDER SAMPLE PREPARATION

The following procedure is for preparing powder samples only. If you have other types of samples for measurement, please contact MCF staff for assistance.

1. Follow the Stand Sample Preparation procedure on the workbench to load powder sample with the Powder Sample Preparation Kit (Figure 3).

(a) (b)

Figure 3. (a) Empty holder; (b) Holder filled with powder.

2. If you only have small amount of powder sample (not enough to fill the holder), you may put a small piece of glass in the holder and then load powder on top.

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SAMPLE LOADING (FOR AUTOLOADER)

The following procedure is for performing measurements with Sample Spinner and Autoloader only on powder samples. If you need to use the universal stage or bracket stage, please contact MCF staff for assistance.

1. Check to ensure that shutter is closed. Open the enclosure doors.

2. If you only have one sample loaded in the sample holder, mount it at the A1 position on top of the A sample column.

3. If you have less than 15 samples, mount them in the A column from top down. Use B & C column positions if you have more than 15 samples (Figure 4).

4. Close the enclosure doors and make sure they are fully closed.

Figure 4. Five samples loaded in autoloader column from A1 to A5.

BUILD ABSOLUTE SCAN PROGRAM

Use the following procedure to create a new Absolute scan program. If you already have a program created, use “File > Open Program” to open the existing program and edit it for current session.

1. In top menu, click “File > New Program”. A dialog window will pop up (Figure 5).

2. Select “Absolute scan” in the Program type drop down box and click OK. The Prepare Absolute Scan window will appear (Figure 6).

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Figure 5. Create an absolute scan.

3. In Configuration section, select “Sample spinner” in the drop down box.

4. In Scan Axis section, select “Gonio”.

5. In Scanning mode section, select “Continuous”.

6. Input the proper Start angle, End angle, Step size and Time per step.

7. Click “Settings” button on the right to open the “Settings” window (Figure 6).

8. In Settings window, click “Sample Stage” in the window. Then check “Spinning” at the bottom of the window and select the proper Revolution time from the drop down box.

9. Click “Apply” and then “OK” to close the Settings window.

10. Save the program by click “File > Save” and give the program an easily identifiable name.

Figure 6. Absolute scan set up interface.

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BUILD BATCH SCAN PROGRAM

1. In top menu, click “File > New Program”. A dialog window will appear (Figure 7).

2. Select “General batch” in the Program type drop down box. Then select “sample spinner” in the Configuration drop down box. Click OK to open the Prepare batch window (Figure 7).

Figure 7. Select proper stage for new general batch program.

3. Click to highlight the first line in the program window.

4. Click “Insert Batch Settings” button at the bottom of the window.

5. Click the “X-ray/PHD” tab in General Batch Settings window (Figure 8). Check the “Set” box and input 45 kV and 40 mA. Click “OK” to close the window.

Figure 8. Set the X-ray power setting for measurement.

6. Click to highlight the second line in the program. Then click the “Insert Batch Settings” button.

7. Click the “Changer/Non-ambient” tab in the General Batch Settings window.

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8. Check the “Sample position” box and then the “Set” box. Then check the “Magazine” box and input the sample location in column (e.g., A1). Each column can hold 15 samples and the positions are numbered 1 to 15 from top down (Figure 9).

Figure 9. Sample position set up

9. Click to highlight the third line and then click “Insert Measurement Program” button.

10. In the Open Program window, select “Absolute scan” in the drop down box and then select the desired Absolute Scan program from the list. Click OK to continue (Figure 10).

11. Select the Folder where the data file will be stored.

Figure 10. Select the desired absolute scan program from list.

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12. To run same type of tests on multiple samples loaded consecutively on the same sample column, use the following procedure to program cycle measurements:

Click to highlight the next blank line in the program.

Click the “Insert Batch Settings” button at the bottom of the window.

Click “Changer/Non-ambient” Tab.

Check the “Sample position” box and the “Increment” box (Figure 11).

Check “Magazine” box and input 1 in the box under the Increment. Click OK to continue.

Figure 11. Set the sample auto-loading

Click to highlight the next blank line in the program.

Click “Insert Measurement Program” button.

Select the desired Absolution Scan program and set the folder for data storage.

Press “Shift” key on keyboard and click to highlight the last two lines in the program (Figure 12).

Click “Cycles” button and type in the proper cycle number (Figure 12), which should be one less than the total sample number.

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Figure 12. Set cycles to repeat measurement steps.

13. Click to highlight the next blank line in the program and then click the “Insert Batch Settings” button to set the idle state of the instrument at the end of the session.

14. Click the “X-ray/PHD” tab in General Batch Settings window. Check the “Set” box and input 45 kV and 20 mA.

15. Click the “Position” tab. Select the check box for “2 Theta” and input 40. Select the check box for “Omega” and input 20 (Figure 13). Click OK to continue.

Figure 13. Set the tool to idle state

16. Click “Check” button at the bottom of the window to check any error in the program (Figure 14).

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17. Save the new general batch scan program by click “File > Save” and give the program an easily identifiable name.

Figure 14. Use Check function to check the general batch program.

DATA ACQUISITION

1. Check to ensure that the samples are loaded at the locations specified in the general batch program.

2. Check the beam mask installed. Select the proper size copper mask to limit the lateral divergence of the beam for your application. (Use 20 mm size mask for powder samples). Close the enclosure doors.

3. Click on “Incident Beam Optics” tab on the left side column of the software interface. Check the Angle value of the “Divergent slit: Prog. Div. Slit”. A slit size of ½o or 1o are recommended for normal operation.

4. To change the divergent slit size, double click on the “Prefix Module: Progr. Div. Slit Module” to open the “Incident Beam Optics” configuration window.

5. In the “Divergent Slit” tab, select the proper “Aperture” size in the drop-down menu. Larger divergent slit size results in broader beam and increased signal intensity but also stronger background at <10o range. Click “OK” to exit.

6. If you need to install Incident Beam Anti-Scatter Slit (rectangular shaped metal piece with a slit in the middle), make sure it is twice the size of the incident divergence slit.

7. Click on “Diffracted Beam Optics” tab on the left side column of the software interface. Check the value of the “Anti-scatter slit” within the “PreFIX module: X’Celerator Module” section. It should be twice the size of the divergent slit set in the “Incident Beam Optics” tab.

8. To change the anti-scatter slit size, double click on the “Anti-scatter slit” section to open the “Diffracted Beam Optics” configuration window.

9. In “Type” drop down menu, select the desired anti-scatter slit size. The anti-scatter slit size should be twice the size of the divergent slit of the Incident beam optics. Click “OK” to exit.

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10. Click on the “Detector” tab. Set the detector to “Scanning mode in Usage field. Set the Active Length to 2.122.

11. In the top menu, select “Measure > Program …”

12. Select “General Batch” in the drop down box. Then select the desired general batch program from the list. Click OK to continue (Figure 15).

13. In the Start window, select each sample from the list in the middle of the window and input a Sample ID for each of them at the bottom (Figure 16).

14. Click “OK” and the instrument will start the measurement.

Figure 15. Select the desired general batch program to run.

Figure 16. Set up Sample IDs for each sample.

15. The measurement can be stopped anytime by pressing the red “Stop” button on the top menu.

16. Upon completion each measurement, the program will automatically save the data to the folder specified in the batch program.

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DATA ANALYSIS

1. Click the X’Pert HighScore Plus icon on the desktop to start the program.

2. Click “File > Open” to open the XRD data file to be analyzed.

3. Click on the IdeAll button at the bottom of the window to start automatic identification process.

Figure 17. X’Pert HighScore Plus interface

4. If the automatic identification process fails to find any match, try the manual pattern matching

procedure as follow:

Select “Treatment > Determine Background” in the top menu.

Select “Accept”

Select “Treatment > Search Peaks” in the top menu.

Select “Accept”

Select “Analysis > Search & Match> Execute Search & Match” from top menu (Figure 18).

Select the “Chemistry” tab.

Set element restrictions based on your best knowledge of the sample then close the window (Figure 19).

Select “Parameter” tab to change the scoring scheme or allow pattern shift.

Select “Automatic” tab to set up filter to accept phases that match.

Press “Search” button and then click OK.

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Figure 18. Search and Match menu

Figure 19. Search and Match settings

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SHUT DOWN

1. Check the XRD status display reading to ensure that the XRD is at idle state (45 kV 20 mA, shutter closed). If the shutter is still open (display “1”), press the “Shutter close” button on the display to close the shutter. If the X-ray power is not at idle state, click the X-ray in the Instrument Settings tab (Figure 20) and set the X-ray generator power to 45 kV 20 mA.

2. Disconnect the instrument by selecting “Instrument > Disconnect” in top menu.

3. In the Close Control Form window, select “Close control window and go off-line” option. Click OK (Figure 20).

Figure 20. Disconnect the instrument from software

4. Close the X’Pert Data Collector program.

5. Open the front doors and unload samples from the sample loader. Close the doors.

6. Sign out on the FOM and sign out on the logbook. Report any problem in the FOM log off window and in the note section of the log book.

7. Clean up the work area before leaving the room.

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EMERGENCY PROCEDURES

If a user ever has a problem or an uncertainty should ASK someone who knows and can help. There are no penalties for asking for help but there may be for not reporting damage to the equipment that may delay or prevent others from working. If, at any time, the user needs to contact someone for help, call or locate the following staff of the Materials Characterization Facility (MCF):

Weiqiang Ding Office: ESB G75D Phone: (304) 685-1938 cell

Harley Hart Office: White Hall 409 Phone: (412) 443-1545

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

Shut down the XRD power by pressing the Standby button on control panel

Shut down the computer Then, if possible, the user should stay with the optical profiler while trying to contact the above individuals. If it becomes necessary to leave the instrument then the user should leave a large, legible note on both the optical profiler and at least one of the above individuals’ offices, stating:

The problem, describing what happened and steps taken

When it occurred date and time

User name and phone number

If a dangerous situation is evident (smoke, fire, sparks, etc.), the user should press the Emergency power off button to turn OFF power to the entire system and notify the proper emergency personnel. If turning off the power would be unsafe in the user’s estimation, the user should leave the facility and contact emergency personnel immediately.