MTU XRD LAB.jpg


Using the Michigan Tech ACMAL SCINTAG XDS-2000 POWDER diffractometer[edit | edit source]

This method page will cover all steps need to conduct a percent crystallinity measurement on a 3-D printed sample. Before you begin: Contact Ed (below) about getting a badge for the XRD lab, YOU MUST HAVE A BADGE ON FILE PRIOR TO USING THE XRD!

ACMAL Link and point of contact[edit | edit source]

Lab supervisor: Ed Laitila (ealaitil@mtu.edu), Office: 628 M&M

XRD Lab - Room: 629 [Scintag XDS-Powder]


Sample Prep[edit | edit source]

1. Print out the XRD sample with your desired settings at 100% fill. Ensure the bottom is as smooth as possible and clear of any contamination (eg. no glue/hairspray and printed on smooth glass/PET tape/Kapton tape not blue painters tape) XRD Sample Piece

2. After printing make sure to keep the surface as clean as possible until you get to the XRD lab

3. Once in the lab use one of the wipes to clear off any residue that may have accumulated and use the compressed air to get any dust particles that may have settled off. Do this as close to mounting the sample as possible


Loading specimen[edit | edit source]

1. Check to make sure the X-Ray ON light is off (left side of the chamber for the diffractometer)

2. If off look for a sample in the holder, should there be a sample in the holder check the log book next to the diffractometer for the last user and the computer to make sure a scan is done.

  • Also re-check to make sure you did reserve time in the calendar and this is your scheduled time

3. Put sample in the holder by pulling down on the spring loaded metal tab and sliding the sample in with the smooth side up. Arrange the sample so the middle is as close to the etched line on the rim of the holder as possible. This will ensure that the beam is centered on the sample and will not interact with anything else at low angles.


Setting up diffractometer[edit | edit source]

1. Goto computer Warren.

2. Sign into the log book. Review the "How to" guide next to the log book. Make sure to record what hours the Diffractometer is at. (To find this number, look next to the red safety button)

3. If diffractometer is on. (See sheet on diffractometer for directions when it is OFF)

4.(SEE SHEET ON DIFFRACTOMETER FOR FULL DIRECTIONS) Push lever on kV knob to the left in order to turn kV knob. Turn kVs to -45.

5. (SEE SHEET ON DIFFRACTOMETER FOR FULL DIRECTIONS) Push lever on mA knob to the left in order to turn mA knob. Turn mAs to 30.

  • DO NOT EXCEED THESE SETTINGS!

6. Check slits to see if they are standard.

7. Carefully carry your prepared sample to the XRD.

8. Make sure X-rays are off.

9. Open XRD door (lift up)

11. Sample stage consists of a spring-loaded platform that holds the sample in place. Pull spring-loaded platform down far enough to slide your sample in.

12. Very carefully slide sample in and center the sample with the stage. (See pict)

13. Close the XRD door (pull down)

14. Hit the Red Safety button.


Scan parameters and starting scan[edit | edit source]

At computer Warren (only computer associated with running scans for this diffractometer)

Open DMSNT software

  • File -> New Event List
    • Scan -> Normal
      • Browse X: Drive -> Diffraction Data -> Find your username/file or consult Ed
        • Type in name for this scan (file name)
        • Type in ID area a description of sample (specific to sample : heat treatment, composition, mech testing, etc)
    • Select Slit
      • For normal slit widths, enter as in picture.
    • Select Scan
      • Choose settings that will give information needed for your scan (discuss with Ed).
    • Save Event
    • Save As -> Event name too.
    • Go From Top (STARTS SCAN)
      • Do you want to initialize hardware? -> Yes
        • Confirm goniometer position (discuss with Ed)
          • Select Real-Time Display in Scan Status Window to watch progress.

Analysis after Scan is done[edit | edit source]

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Authors Ben Wittbrodt
License CC-BY-SA-3.0
Language English (en)
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Created March 2, 2015 by Ben Wittbrodt
Modified March 2, 2022 by Page script
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