Rigaku SmartLab X-ray Diffraction System

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Rigaku SmartLab X-ray Diffraction System

Institute for Imaging & Analytical Technologies (I2AT) hosts a wide variety of equipment that can be utilized for the characterization of material. Among the equipment is Rigaku SmartLab X-ray Diffraction System allows for multiple types of analysis using the following available techniques.

  • texture/pole figures
  • powder diffraction (focusing beam)
  • powder diffraction (parallel beam)
  • small angle x-ray scattering (SAXS)
  • thin film diffraction (in-plane)
  • thin film diffraction (high-resolution)
  • thin film diffraction (glancing incidence)
  • x-ray reflectometery; in-plane diffraction
  • Rietveld analysis
  • reciprocal space maps for film epitaxy, thickness, lattice tilt, and crystal perfection
  • residual stress analysis

Machine Specifications

  • 2.2kW Long-Fine Focus X-ray Tube
  • Cross Beam Optics (CBO)
    • High-resolution Parallel Beam Optics
    • Bragg-Brentano Para-Focusing Optics
  • GE (220) 4-Bounce Incident Beam Monochromator
  • High-resolution Vertical Theta/Theta 4-Circle Goniometer with horizontal sample stage and Eulerian cradle
    • Measuring range: Thetas/Thetad -3° to 160° 2Theta
  • Small Area Camera System for sample alignment
  • Anton Paar Domed Hot Stage (to 900°C)
  • Scintillation Detector

Operating Manual for Bulk Texture Evaluation

1. Click on '1 Optics Alignment'. Prior to operating the XRD machine, request the machine technician to perform the Optics alignment. This step does not require a sample to be present and thus, can help save precious time.

Optics Alignment

2. Click on '2 Sample Alignment'. Note the height, length, and width of the sample. This step requires a sample to be inserted inside the chamber at approximately the center of 'Wafer Sample Plate' before proceeding towards the alignment. Click on 'RAXVIDEO' icon on the desktop to start a live camera feed whose center roughly coincides with X-ray beam. Place the sample such that it is roughly in the center of the RAXVIDEO camera view by primarily adjusting the height of the sample or by slightly moving the sample in the lateral direction. Clicking on the sample alignment tab will prompt a window where the sample dimensions noted earlier are going to be inserted. For the case of a rectangular cross-section in a cold mount, the height of the cold mount is going to be inserted in place of 'Sample thickness (mm)'. The dimensions of the rectangular specimens are going to be inserted in place of 'Sample width (mm)' and 'Sample height (mm)' in any order.

Sample Alignment
RAXVIDEO Desktop Icon
RAXVIDEO Camera View
Sample Alignment Tab

3. Close the machine door and click on 'Execute' to perform sample alignment. Follow the instructions as prompted by the machine in 'SmartMessage' tab to perform optical configurations. If the instructions provided by the machine are not followed properly, the option to click OK on the 'SmartMessage' tab will not be enabled. Once the instructions have been followed, the alignment process will commence. If the alignment is unsuccessful, the machine will prompt an error and will require you to readjust the position of the sample in the machine. If the alignment is successful, no error will be prompted. Click on OK in the Sample Alignment tab.

SmartMessage Prompt

4. Click on '3 Pole Figure Measurement'. This tab includes the planer information (2-Theta angle, etc.) required to capture the information from a certain plane. These conditions are configured already and should not be altered. Click on the '...' button to browse to a desired location to save the output files. Finally, click OK.

Pole Figure Measurement
Output file path is selected in the Pole Figure Measurement tab.

5. Perform the same task mentioned earlier but for each subsequent 'Pole Figure Measurement' tab until the 8th and final tab is configured. There are a total of 6 output files generated.

6. Click on the '3 Pole Figure Measurement' tab once again and then click OK. This step will enable the third tab to be highlighted in yellow. Finally, click on the 'Run' button and select Yes on the first prompt and then select No on the second prompt. The pole figure measurement procedure will now commence and last for approximately 6 hours.

Select Yes
Select No

7. Click on 'RAS data converter' on the desktop to open a user interface that will allow us to convert the output files (generated by SmartLab Guidance software) that are in 'R-ASCII' file type format to the 'RINT' file type. The six raw files are selected by clicking on 'Select Files' button and a destination folder is selected by clicking on 'Change Folder' button. The output file format is ensured to be 'RINT Binary' format from the drop down menu.

RAS Data Converter Icon
RAS Data Converter Interface

8. Click on '3D Explore' on the desktop to open the raw files generated from the 'RAS data converter'. A background correction is executed before the data is exported as a text file for generation of pole figures using the MTEX software.

Optics Alignment

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