2.3.2.2.

Acquisition and Treatment of Diffraction Data

- A diffractometer records changes of diffraction intensity with 2θ.
- Figure 2.18 displays the X-ray diffraction spectrum of a Si and Al 2O3 powder mixture,
with peaks corresponding to different crystallographic planes.

- The figure also shows the penetration depth of Cu Kα radiation at varying incident
angles.

- Spectrum matching is determined by the positions of the diffraction peak maxima and
the relative peak intensities among diffraction peaks.
- Modern diffractometers use computers for data acquisition and treatment. Important
factors for identifying a material include:
+ choosing a 2θ range (around 5-65◦)
+ X-ray radiation (copper Kα is popular because of its short wavelength)
+ step width for scanning (10-20 data points above the FWHM is recommended)
- To obtain a satisfactory diffraction spectrum, the following treatments of diffraction
data treatment should be done:
+ smooth the spectrum curve and subtracting the spectrum background
+ locate peak positions
+ strip Kα2 from the spectrum, particularly for peaks in the mid-value range of 2θ.
2.3.3. Distortions of Diffraction Spectra
2.3.3.1. Preferential Orientation
- Diffraction spectrum serves as a unique identifier for a material
- A comparison of acquired and standard spectra can confirm the sample's identity
2.3.3.2. Crystallite Size
- In a diffractometer, the incident X-ray beam deviates slightly from the Bragg angle θB,
generating diffraction peaks at a range of angles from θ 1 to θ2.
- This results in incompletely destructive interference, which produces diffraction
intensities around θB, widening the diffraction peak.
- Peak width increases with decreasing crystal size, as shown in Figure 2.21.
2.3.3.3 Residual Stress
- Residual stress in solid specimens can alter their X-ray diffraction spectra by shifting
peak positions.
- This stress generates strain by changing the spacing of crystallographic planes,
causing the Bragg angles to either increase or decrease.
- This can be used to examine residual stress in solids.
Figure 2.22: Effects of residual stress and strain on diffraction peak position and shape:
(a) no strain; (b) uniform strain; and (c) non-uniform strain.