Analyzes of the structure, crystallite size and internal strain of a small crystal by a x-ray powder diffraction method

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This study aimed to determine the precise lattice parameters, crystallite size and internal strain of a very small crystal less than 100mum by applying a profile fitting technique to the x-ray powder diffraction data obtained with a Gandolfi camera. The brief summary of the results obtained in this study is as follows.1. By an application of a profile-fitting technique to the x-ray diffraction data obtained with a Gandolfi camera, the 2 rheta position of each diffraction line can be determined within an error of less than 0.01ﾟ(2rheta).2. In the case of the crystal which gives clear diffraction lines in the high angle range of a diffraction diagram, the lattice parameters of a very small crystal can be determined precisely by an extrapolation method.3. For the crystal which does not show a clear diffraction pattern in the high angle range of a diffraction diagram, an internal standard method was applied to estimate the systematic errors included in the diffraction line positions.A very small sized crystal less than 100 mum was coated with a standard material by using a syanoacrylate as the dispersing agent. After the correction of systematic errors, the lattice parameters of a very small crystal can be determined precisely by using a least-square technique.4. After the correction of the mechanical line broadening by referring the integral breadth of a standard material, the crystallite size and internal strain of a very small crystal can be estimated by the Williamson-Hall method.