Rigauku RSM Draft
- 1 XRD Rigaku Procedure 2017
- 2 Prep and Load
- 3 Normal Procedure
- 4 End Use
- 5 Optics Alignment
- 6 RSM Procedure
- 6.1 Analyzer Alignment
- 6.2 Goniometer Alignment
- 6.3 Rocking Curve Pre-Measurement – Phi (rough)
- 6.4 Rocking Curve Pre-Measurement – Multiple Angle Rough
- 6.5 Rocking Curve Pre-Measurement – Chi (rough)
- 6.6 Rocking Curve Pre-Measurement – Phi (fine)
- 6.7 Rocking Curve Pre-Measurement – Omega and 2-Theta
- 6.8 Rocking Curve Pre-Measurement – Chi (fine)
- 6.9 Rocking Curve Pre-Measurement – Omega and 2-Theta (refine)
- 6.10 RSM Measurement
- 7 Angles
XRD Rigaku Procedure 2017
Written by KMM from training and notes, September 2017. Updated NTS 20171126.
The generator for this XRD may be operated at conditions up to 45kV and 200mA. The normal operating conditions are 45kV/200mA. Aging of the anode takes 70 minutes and must be performed each time the X-ray source is to be used. By default, the instrument is configured for rocking curves and 2theta-omega diffraction scans. LabAccess is interlocked to the XRD doors.
Prep and Load
At the computer, open the Rigaku Smartlab Guidance application window and login.
Begin the aging process to reach the normal operating conditions for the x-ray anode at least 70 minutes before you plan to perform your experiment.
To begin the aging process, click the Startup button on the left side of the Rigaku Smartlab Guidance software window.
Click Execute in the popup dialog to initiate the aging process.
The Tube voltage and Tube current can be viewed on the bottom left Hardware Status window.
You can also set a tube aging timer, which will start the aging process when the time is reached. Choose a time and then click OK. The Startup button should be red.
Log in to LabAccess once the x-ray tube is aged and you are ready to begin.
Load your sample.
Press the DOOR LOCK button on the front of instrument. When the yellow lamp starts blinking and beeping, the door can be opened.
Place sample in the center of the cross hairs on the standard sample mounting plate.
For off-axis scans (scans with Chi translation, RSMs), use magnetic clips located in the XRD enclosure to hold the sample in place, or the classic backing wafer and tape method.
Close enclosure doors carefully, ensuring both sides of the sliding doors are in contact with each other. Press the DOOR LOCK button and the beeping should stop. If not, open and close the doors carefully again and press DOOR LOCK button
Normal Procedure
The package manager window on the right hand side of the screen lists the available measurements (if not visible, Tasks > Package/Macro/Package Bar). Users should only select measurements from the User defined package list. Other measurements require reconfiguration of the XRD system, which must be performed by the technical staff. If you’re unsure how to measure your sample always ask first!
To perform a rocking curve measurement, double click the measurement titled MER rocking curve HR PB-Ge(220)x2 in the User defined package list.
After you double click, the following steps will appear in the Package/Macro Measurement Window on the left side of the screen.
1 Sample Alignment
2 Rocking Curve Pre-Measurement
3 Rocking Curve Measurement
Rocking Curves can be performed by doing the three steps one-by-one, or by setting up each step at the beginning and then Clicking the big macro package Execute button (details below)
Sample Alignment
To begin your measurement, click on the box labeled 1 Sample Alignment, which opens the sample alignment window.
Enter your estimated sample thickness and sample width and sample height.
The sample width and height define the area of your sample, and can be left at the default 10.0 mm for samples larger than 1cm2.
Click the Execute button on the bottom left of the sample alignment window. A Hardware Control window will open in the corner.
A SmartMessage dialogue box will appear instructing you to place a sample spacer, wafer sample plate, and sample in the system. For samples less than 3 mm thick, no changes to the stage are necessary (i.e. spacer is already in use).
Click the Execute/OK button on the SmartMessage window, and the automated sample alignment process will begin.
When the alignment is complete, the Hardware Control window will close.
Close the Sample Alignment window by clicking the X in the top right corner.
Goniometer Alignment
After the sample alignment process is complete, you must align the goniometer to the reflection you want to measure using a rocking curve pre-measurment.
To align to the desired specific crystal reflection, you must first tell the XRD which crystal structure and reflection angle you want to measure.
Click the Process tab at the top of the screen and then click Crystal Information.
In the Crystal Information window, choose your sample material, or enter a new material by clicking the New button.
Click OK at the bottom of the Crystal Information window to load your crystal structure.
Click the Process tab and then click Diffraction Space Simulation (DSS). A map of the reciprocal space for your sample (selected crystal structure) is displayed in the DSS.
To find your reflection angles, enter the h k l values in the Reflections list fields on the right side of the DSS window, or click on the point on the DSS map. Check the Reflections fields are correct. (0 0 4) is very common.
GaAs [0 0 4] – 2theta = 66.0445; omega = 33.0222
Click the Move gonio button to move the goniometer to your desired reflection.
Substrate Angles are listed in a section below
Rocking Curve Pre-Measurement
Click the 2 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The RCPM step (now) aligns the sample for the Rocking Curve (next).
This step is the most likely to fail and need to be redone or tweaked.
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the alignment scan.
Enter your sample name in the Sample name: field.
Click the Read current positions button to load your diffraction angle into the scan parameters. The Move origin check box is checked by default.
Click the Execute button to run the alignment scan.
When the alignment is complete, the Hardware Control window will close.
Close the RCPM window by clicking the X in the top right corner.
Rocking Curve Measurement
After the RCPM, the system is ready to perform a rocking curve measurement.
Click the 3 Rocking Curve Measurement (RCM) button in the measurement process flow chart. The RCM window will open.
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the measurement scan.
Enter your sample name in the Sample name: field.
To perform a 2-theta/omega scan (normal), check the 2-theta/omega scan conditions check box (checked by default) and enter your desired scan range. To perform an Omega scan, check the Omega scan conditions check box and enter your desired scan range.
Remember to double the range as compared to the old XRD due to the angle relationship.
Click the Execute button to perform your rocking curve measurement.
When the measurement is complete, the Hardware Control window and shutter will close.
Check the saved file to make sure it looks OK.
To run another RCM on the same sample, modify your RCM parameters and re-run.
If there were alignment or scan issues, redo alignment or troubleshoot.
When done with this sample, close the RCM window by clicking the X in the top right corner.
Swap Samples, or remove final sample for the day.
Repeat from Rocking Curve Pre-Measurement for additional samples that are similar thickness and size.
Otherwise, for samples that are different, go back to Sample Alignment.
Or proceed to do a RSM on the sample next if needed.
Note that one should probably do all of the RCMs for a set of samples, then all of the RSMs. This will avoid doing extra part swapping, and extra optics alignment scans.
Rocking Curve Macro
Setup the Macro to run all three steps for a RCM.
Setup each step as if you are performing it, but do not move the goniometer nor click execute in the window for each.
Click OK as you fill at each one so the program remembers what you enter.
The File name: and Sample name: fields are almost the half the changes.
Enter the angles for the material you want to scan into the RCPM window with the Move origin check box checked (checked by default).
It will move the Gonio to those angles when the RCPM starts.
You must setup your 2-theta/omega scan conditions at this time.
Setup 1 Sample Alignment: Sample dimensions.
Setup 2 Rocking Curve Pre-Measurement: File and Sample Name fields, enter the necessary angles.
Step 2 is the most likely to fail, so it is good to make sure this step works.
Setup 3 Rocking Curve Measurement: File and Sample Name fields, Scan Parameters.
Press the large execute button in the Package/Macro Measurement Window on the left side of the screen.
Make sure the scan starts correctly (may need to swap slits or confirm the stage is correct).
End Use
When you are finished with the tool for the day, follow these steps.
Reset the goniometer position.
Double click the measurement titled Shut down in the User defined package list.
This will load a single MOVE flowchart that can be executed by clicking the big Execute button in the Package/Macro Measurement window on the left hand side.
If this doesn’t work, click MOVE to open the Move window, and go through each tool setting to set it to 0 by clicking Execute
Typically 2-Theta, Omega, Z, Rx, and Ry need to be set to 0. Alpha stays at 90 deg.
Chi and Phi have to be set to 0 after a RSM.
If you did a RSM, run a high res optics alignment, procedure is below.
Check Sedona to see if anyone else is scheduled to use the tool today. The X-ray source takes over an hour to turn on, so please check to make sure that no one else is using the tool later.
If no one is scheduled after you, idle the X-ray source.
Click the Shutdown button in the Package/Macro Measurement window.
Click the Execute button in the Shutdown window that opens.
Note that the Soller slit and normal sample stage must be loaded into the XRD.
Copy saved files to a flash drive.
Cleanup work space.
Close the SmartGuidance software.
Log out of LabAccess.
Optics Alignment
Soller slit must be installed on the detector arm, swap it in if necessary.
Remove the sample stage (flat disk with crosshairs) and spacer together using notch lock (2 o’ clock position of stage mount).
Install the standard reference plate (looks like a diving board). No sample is loaded.
Put in 10 mm source slit.
Double click the package titled high resolution PB-Ge(220)x2) optics alignment in the User defined package list.
After you double click, the following steps will appear in the Package/Macro Measurement Window on the left side of the screen.
1 Optics Alignment
Click on the box labeled 1 Optics Alignment, which opens the optics alignment window.
If the system is a little off for a Sample Alignment, or you just did a successful RSM, check the Change Optics (quick alignment only) check box.
Do not check if the quick align fails twice, or a RCPM/RCM or RSM fails and you suspect optics alignment issues.
Click the Execute button to run the alignment scan.
When the alignment is complete, the Hardware Control window will close.
If it fails, check all the angles are set to 0 and run again.
If it fails again, do not check the quick align check box and do a full alignment.
Close the Analyzer Alignment window by clicking the X in the top right corner.
Replace the normal sample stage and spacer.
RSM Procedure
To perform a Reciprocal Space Map (RSM) measurement, double click the measurement titled MER Reciprocal Space Mapping (RSM) high resolution PB-Ge(220)x2 in the User defined package list.
After you double click, the following steps will appear in the Package/Macro Measurement Window on the left side of the screen.
1 Optics Alignment (PB-Ge(220)x2)
2 Sample Alignment
3 Analyzer Alignment
4 Rocking Curve Pre-Measurement
5 Rocking Curve Pre-Measurement
6 Rocking Curve Pre-Measurement
7 Rocking Curve Pre-Measurement
8 Rocking Curve Pre-Measurement
9 RSM Measurement(0D)
RSMs can be performed by doing the nine steps one-by-one, or by setting up each step at the beginning and then Clicking the big macro package Execute button, but this is NOT recommended due to more complicated setup, the likelihood of one or more step failing in the middle, and the step order being off!
The order of steps is NOT the above order. It is: 1, 2, 3, 6, 4, 5, 6, 8, 7, 8, 9.
Most of the steps are quick, with 9 and 4 being the longest.
Step 4 is the most likely to fail.
Optics Alignment is just like the Optics Alignment section above, and can be skipped if the optics are aligned.
Sample Alignment is just like a sample alignment for a RCM.
You can skip if you just did an aligned RCM for the sample, or you are putting in a very similar sample: similar thickness and size, and the same material and desired reflection angle. For long scans or sensitive samples, it may be worth doing a sample alignment for each sample.
The RSM RCPM/alignment steps written here have ranges that have worked for normal epitaxial samples so far. For odd or sensitive samples, you may need to adjust scan parameters, keep an eye on each scan, manually adjust the position of angles (Using Shutdown > Move, which will reset the File and Sample name fields, and do certain Steps, or sets of Steps, multiple times.
Analyzer Alignment
Set 2-Theta and Omega to 0 to lower the arms for system modification if needed.
Swap in the 2 bounce monochromator Ge(220)x2
Unplug the Soller slit on the detector arm. Unhook RPS cable first from base, it has a locking mechanism, so you must pull the plastic back at the plug base.
Remove the Soller slit on detector arm using the allen key to unlock it. It has an optical tag near the top of the backside, so be careful where you grab it.
Put in the 2 bounce monochromator, lock it in place, and plug in the ROD cable.
Click the 3 Analyzer Alignment button in the measurement process flow chart. The Analyzer Alignment window will open.
Analyzer name should be Ge(220)x2 by default.
Check align at 2-Theta = 0 deg check box (not checked by default).
Click the Execute button to run the alignment scan.
When the alignment is complete, the Hardware Control window will close.
Close the Analyzer Alignment window by clicking the X in the top right corner.
Goniometer Alignment
After the analyzer alignment process is complete, you must align the goniometer to the
desired specific crystal reflection, so you must first tell the XRD which crystal structure and reflection angle you want to measure.
Click the Process tab at the top of the screen and then click Crystal Information.
In the Crystal Information window, choose your sample material, or enter a new material by clicking the New button.
Click OK at the bottom of the Crystal Information window to load your crystal structure.
Click the Process tab and then click Diffraction Space Simulation (DSS). A map of the reciprocal space for your sample (selected crystal structure) is displayed in the DSS.
To find your reflection angles, enter the h k l values in the Reflections list fields on the right side of the DSS window, or click on the point on the DSS map. (2 2 4) is common.
Click the Symmetric geometry button at DSS window top. The window should change and show your desired h k l centered in the map.
You can see a preview of the scan by clicking the Show RSM measurement area button at DSS window top.
Control the area shown with the RSM measurement area ranges on the right.
This is a preview, not a command.
Set Phi to 0.
Click the Move gonio button to move the goniometer to your desired reflection.
Substrate Angles are listed in a section below
Rocking Curve Pre-Measurement – Phi (rough)
Click the 6 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The 6 RCPM step (now) aligns the sample in Phi (rough)
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the scan.
Typically mention what type of alignment it is, e.g. 224 Phi Alignment.
Enter your sample name in the Sample name: field.
Click the Customize… button to setup the scan.
Scan Parameters: -10, 10; 0.020; 20.0.
Alignment method is Quick axis by default; Scanning Sequence is Only Chi(Phi) by default.
The Move origin check box should NOT be checked by default, for this and most RCPMs
Click the Close button to return to the RCPM window.
Click the Execute button to run the scan.
When the alignment is complete, the Hardware Control window will close.
Close the RCPM window by clicking the X in the top right corner.
Rocking Curve Pre-Measurement – Multiple Angle Rough
Click the 4 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The 4 RCPM step (now) aligns the sample in Rx, Ry, Omega-s, then Omega and 2-Theta.
This step is the most likely to fail and need to be redone or tweaked.
This scan sets Phi to 0, does an Omega scan, sets Phi to 180, does and Omega scan, guesses Ry, Sets Phi to 90, does an Rx scan, and repeats. When it’s happy, it does an Omega scan, 2-Theta scan, and an Omega scan.
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the scan, e.g. 224 Rough Alignment.
Enter your sample name in the Sample name: field.
Click the Customize… button to setup the scan .
Alignment method: Precise axis alignment (default).
Optimize 2-Theta checked by default.
Click the Read current positions button to load your diffraction angle into the scan parameters. The Move origin check box is checked by default.
Chi is unchecked because it tends to mess up your scan.
The Change Omega position to half of 2-Theta position check box is checked by default.
Rx,Ry: -3, 3; 0.010; 9.9; Sequential (default)
Omega: -2, 2; 0.005; 5.0; Sequential.
2-Theta: -1, 1; 0.005; 2.0; FWHM.
Click the Close button to return to the RCPM window.
Click the Execute button to run the scan.
When the alignment is complete, the Hardware Control window will close.
If the scan fails, re-run it but be sure not to check Previous alignment (default unchecked).
If it fails again, decrease Omega and 2-Theta range by 80% (-1.6,1.6; -0.8, 0.8) and decrease the scan speeds to 1.0. Re-run.
If it fails again, ?
Close the RCPM window by clicking the X in the top right corner.
Rocking Curve Pre-Measurement – Chi (rough)
Click the 5 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The 5 RCPM step (now) aligns the sample in Chi (rough)
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the scan, e.g. 224 Chi Alignment
Enter your sample name in the Sample name: field.
Click the Customize… button to setup the scan.
Chi: -3, 3; 0.020; 10.0.
Alignment method is Quick axis by default; Scanning Sequence is Only Chi(Phi) by default.
Click the Close button to return to the RCPM window.
Click the Execute button to run the alignment scan.
When the alignment is complete, the Hardware Control window will close.
Close the RCPM window.
Rocking Curve Pre-Measurement – Phi (fine)
Click the 6 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The 6 RCPM step (now) aligns the sample in Phi (fine)
Phi changes Chi, always do a Chi again (eventually) after Phi
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the scan. Overwrite the previous Phi.
Enter your sample name in the Sample name: field.
Click the Customize… button to setup the scan.
Phi: -0.2, 0.2; 0.020; 1.0.
Click the Close button to return to the RCPM window.
Click the Execute button to run the scan.
Click Yes to overwrite the Phi (rough) alignment data file in the popup window.
When the alignment is complete, the Hardware Control window will close.
Close the RCPM window.
Rocking Curve Pre-Measurement – Omega and 2-Theta
Click the 8 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The 8 RCPM step (now) aligns the sample in Omega and 2-Theta (sort of again)
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the scan. Overwrite the previous Rough.
Enter your sample name in the Sample name: field.
Click the Customize… button to setup the scan.
Alignment method: Quick axis alignment (select from pull down).
Scanning Sequence: Only Omega (select from pull down).
Optimize 2-Theta checked by default.
Rx, Ry grayed out, as is Chi.
Click the Read current positions button to load your diffraction angle into the scan parameters. The Move origin check box is checked by default.
Check the Change Omega position to half of 2-Theta position check box.
Omega: -0.5, 0.5; 0.002; 1.0; Sequential. (default)
2-Theta: -0.19, 0.19; 0.0019; 0.76; FWHM. (default)
Click the Close button to return to the RCPM window.
Click the Execute button to run the scan.
Click Yes to overwrite the Rough alignment data file in the popup window.
When the alignment is complete, the Hardware Control window will close.
Close the RCPM window.
Rocking Curve Pre-Measurement – Chi (fine)
Click the 7 Rocking Curve Pre-Measurement (RCPM) button in the measurement process flow chart. The RCPM window will open.
The 7 RCPM step (now) aligns the sample in Chi (fine)
Click the button next to the File name: field to navigate to your save folder (e.g. C:\User Data\User Name), and enter a file name for the scan. Overwrite the previous Chi.
Enter your sample name in the Sample name: field.
Click the Customize… button to setup the scan.
Chi: -0.5, 0.5; 0.010; 1.0. (default).
Click the Close button to return to the RCPM window.
Click the Execute button to run the scan.