X-RAY DIFFRACTION STUDY OF MICRO AMOUNTS OF POLYCRYSTALLINE SAMPLES
A. V. Alexeev, S. A. Gromilov
Keywords: Debye-Scherrer method, CCD-detector, reference, accuracy, unit cell parameters, preferred orientation
Pages: 772-784
Abstract
With the use of reference polycrystalline α-Al2O3 (NIST SRM-1976) and MoO3 samples we consider the most significant geometric and physical factors affecting the accuracy of X-ray diffraction data obtained on a diffractometer equipped with a flat two-dimensional detector (Debye-Scherrer scheme). A general strategy to measure polycrystalline samples in the amount of 20-30 μg is proposed. By the example of SRM-1976 it is shown that with the proper processing of two-dimensional diffraction patterns and the introduction of certain corrections the angles 2θ can be measured with the accuracy not less than ±0.01°. Even with a strong tendency of particles towards preferred orientation the relative intensities of diffraction reflections are shown to be obtained with the accuracy not less than ±10%.
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