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XRD data acquisition and analysis for tin dioxide powder samples
Software: DMSNT ThermoARL
Location: Central Campus EMAL facility
Equipment: Scintag Powder X-Ray Diffraction Instrument

Sample preparation
Lay the sample using a blade in a 1cm square pattern, thick enough to be opaque. Use Isopropyl alcohol for adhesion and uniformity.

Data Acquisition
User the following parameters for the full scan and the 2 peak (high resolution) scan:

Scan Type

Scan

Step

Range

Scan rate

Time

     

[deg]

[deg/min]

[min]

Full Scan

continuous

0.02

15-90

4.0

18

2 peak Scan

continuous

0.02

23-36

0.5

28

For superimposing tin dioxide index pattern use 41-1445 and for gold 4-784. To analyze gold particle size use the second gold peak at high resolution scan from 43-46 degree scan at 0.5 deg/min scan rate. Note: the first gold peak.

Data Analysis

  1. Subtract Background. Once the data is acquired, use the Background Subtraction option under Analysis in the menu bar. Use the default options with Box Car Curve Fit with default value of 1.5 degrees for background subtraction.
  2. Find Peaks . Once the background is subtracted, the Peak Finder option under Analysis will become available. Use the Peak Finder default options: Peak Finder using Digital Filtering of ESD 4 and Ripple Multiplier of 1.5. Make sure only the peaks you are interested in are captured. If not, play with the numbers to achieve this as best possible.
  3. Fitting a Profile. Use the Profile Fit option under Analysis and see all the peaks are listed - if more than you need, you can remove the one's that are not needed. On the right hand side of the panel there are options for the fit. Use the Pearson 7 fit since it best describes the peak and click Calculate to proceed. See the curve fitting results on your plot and note the error shown on the calculation window. Sometimes the first time fit may not match accurately, select Gaussian or any other and go then go back to Pearson 7.
  4. Acquire values. Note down the peak, the amplitude (CPS), Position (degrees) and the FWHM (degrees) for later calculation in the Scherrer formula. Export the raw file into text format with CPS as your y-axis.
  5. Calculation. Use Scherrer formula at http://www.d.umn.edu/~bhar0022/dpcalculator/



designed by: Smitesh Bakrania
maintained by: Scott Wagnon, swagnon@umich.edu
last updated: March 5, 2015