XRD - Main Campus Rigaku Ultima IV

Main Campus Rigaku Ultima IV

Webpage: http://tmi.utexas.edu/core-facilities/equipment/rigaku-ultima-iv/
Location: EER 6.604
Contact for training: Dr. Steve Swinnea (swinnea@che.utexas.edu) During training, you should bring a representative sample that can be used to compare again what you know is a known-good scan of your sample. This will help figure out what kind of scan parameters you need and to debug if there are any alignment issues.

The Main Campus XRD is a convenient backup when the MER XRD breaks. It is less automated and has slightly lower resolution than the Rigaku SmartLab at MER, but still very useful for a majority of our scans. For those who are interested, Professor Swinnea teaches an X-ray scattering theory course in the fall and a hands-on lab in the spring. The spring course can be taken without the theory course. Ask Swinnea for more details.

XRD Operating Procedure -- SDM Summer 2020, updated SDM Spring 2022

1. Make reservation to use the equipment. As of Spring 2022 this was done using TMI's FBS system (requires EID or UT email authentication)

   1. Likely need to request access for FBS from Prof. Swinnea

   2. Make sure you have an updated UT account number from Christine to bill the group for equipment use

   3. Check that you have lab access, e.g. you know the door code to get into the lab and you have elevator access to the 6th floor of EER

      1. (as of Feb 2022) Door code to EER 6.604 is 9810*

   4. https://fbs.research.utexas.edu/Anon/Logon.aspx?ReturnUrl=/

2. Set up hardware for your scan

   1. Digital alloy hardware configurations:

      1. Sending Optics:

         1. Install 2-bounce monochromator (make sure cable is plugged in) this filters out the copper k-beta and tungsten lines, which leaves only the k-alpha line. Change the software to register the 2-bounce installation

         2. ('Rigaku Control Pannel' --> (yellow icon) 'RINT 2200 Right system'), update the incident monochromator to 'CBO + 2-bounce' (the picture will change) and update the Geometry system tab to 'Thin film (highly resolution)'

         3. Change incident slit to be approx same size as your sample, e.g. 10x10 mm should be good for LM or full device scans

      2. Receiving Optics:

         1. Install PB 0.5 deg on receiving side (open the silver housing unit, slide in 0.5 deg PB element, close silver housing unit).

3. Warm up the X-ray tube

   1. in the XG Operation application window

      1. Idle conditions - 20 kV / 2 mA

      2. Normal operating conditions - 40kV / 44 mA

      3. Use green 'Set' button to change to the

      4. The tube takes 5-ish minutes to reach operating conditions from idle. Let it settle for 5-10 minutes before your first use so the tube power is stable

4. Put sample on the sample stage

5. Align and measure sample

   1. Open the Profile measurement software and load your settings

      1. (if it is not already open) go to 'Desktop/Rigaku/Not sure which folder/Thin Film Measurement'

      2. 'Thin Film Measurement' --> 'Profile'

      3. Load your MCD file (file/open, D drive/MCD/your_name.MCD)

   2. Name your scan and save it to the correct folder within the Profile Measurement window, e.g. change the File and Folder Name

   3. Perform specimen alignment (~10 min)

      1. double click on condition 1 within the Profile Measurement window, which should bring up the conditions window

      2. Parameters to use for scan:

         1. check the box 'Delete Previous setting results'

         2. check the box 'Specimen Alignment'

         3. uncheck 'Precise Alignment' and 'Profile Measurement'

         4. Sequence --> Z->Omega

         5. Repeat --> 2

         6. ATT --> 1/100

         7. DS --> 0.1 mm

         8. SS and RS --> 0.2 mm

         9. Specimen thickness --> 0.5 mm

      3. Exit the condition window

      4. In the Profile measurement window, click 'execute scan' icon on the left side

      5. The Profile measurement window will disappear when the scan starts. Once the scan is over, the profile measurement window will reappear

   4. Perform Precise Alignment

      1. From the Profile measurement window, double click on Condition 1

      2. Check the box for Precise alignment

      3. Digital alloy Precise alignment parameters (on GaSb)

         1. Sequence --> Omega->Z->Rx

         2. Repeat --> 2

         3. ATT --> 1/10

         4. DS --> 0.1 mm

         5. SS and RS --> 0.2 mm

         6. Specimen thickness --> 0.5 mm

         7. Peak Search Method --> Peak-top

   5. Perform Profile Measurement w-2t scan

      1. From the Profile measurement window, double click on Condition 1

      2. Uncheck Precise Alignment and check Profile Measurement

      3. Digital alloy Profile parameters (on GaSb)

         1. Typically scan from 48 to 72 degrees

         2. Sampling step ~0.002 and scan speed 1.5 deg/min (similar to scans at MER)

         3. ATT setting depends strongly on what you want to measure. Likely you need to set up different scan ranges by checking/unchecking different range options in the software. The detector saturates >1E6 CPS so adjust the ATT based on that

6. Change back settings at the end of your session

   1. Remove receiving 0.5 PB element

   2. Replace 2-bounce monochromator hardware on receiving side optics

   3. Update the RINT2200 Right system software configurations that accompany 2-bounce hardware

      1. CBO 2 bounce monochro --> CBO

   4. Idle X-ray source (40kV / 44 mA --> 20 kV / 2 mA)