Crystallinity through X-ray Diffraction

Safety

• Do not use the diffractometer without permission.
  • One needs to have a plastic ring assigned to them in order to use the instrument
• Contact Dr. Ed Laitila about using this instrument

Sample Preparation

• In order for the analysis from x-ray diffraction to be effective, the sample must be flat.
  • For polymers used, the samples were not flat and had to be adjusted in order to meet this requirement.

1. Have a 30 mm x 80 mm sample.
2. Coat the flat part of the sample holder with a two-part resin.
   • This is done by mixing the two parts together until a uniform cloudy color appears.
   • Use a flat wooden stick to evenly coat the resin onto the sample holder.
3. Place the sample on top of the resin.
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     Template:Clear
4. Place a flat glass piece over the sample
   • Clean the glass with ethanol before to avoid contamination.
5. Place a heavy object on top of the glass.
   • This is to distribute the weight evenly across the sample.
6. Let the sample sit for 1 hour for the resin to dry.

Crystallinity Analysis

• The instrument used was XDS 2000 by Scintag Inc.
• X-ray diffraction on the specimen was done by Dr. Ed Laitila.
  • Settings used to obtain data were adjusted by Dr. Laitila.
• File of raw data was supplied.

1. Open DMSNT software on a computer.
2. Under tools, click on crystallinity
   • A new window should open.
3. Under file, go to new.
   • Select the raw data file that was uploaded from the scan.
   • The file type should be ".raw"
4. An intensity vs angle spectrum will appear.
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     Template:Clear
5. Make sure "Crystalline" is selected in the upper left corner.
6. Draw a line connecting the two ends of the base of the sharp peaks.
   • The region above the base should become blue.
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     Template:Clear
   • Repeat this until all the sharp peaks are filled in.
     • There are small peaks present on the broad peak, and would be need to be included as crystalline.
7. Select "total area" from the upper left corner.
8. Draw a line from the leftmost base of the spectrum to the rightmost base of the spectrum.
   • Make sure the the base line is below the spectrum at all times.
     • If not, reduce the length of the base line so that is underneath the spectrum.
   • The region of the base should become green.
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     Template:Clear
9. In the upper right corner of the spectrum, the percent crystalline will be shown.
   • This corresponds to how much crystalline is present in the sample.