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The absorption of X-rays in a heterogeneous material depends on the linear absorption coefficients and volume fractions of the components, and on die geometrical peculiarities of their distribution. The latter is called the microabsorption effect, it can be separated into a bulk and a surface contribution. Within the framework of a well-defined stochastic structure model, the bulk contribution to the microabsorption is calculated for arbitrary random multiphase systems in terms of dependence on volume fractions and mean chord lengths of particles. Expressions are derived which are suitable for eliminating the experimental errors of scattering intensities caused by the bulk contribution of microabsorption.
If only one wavelengtii of radiation is used, the mean chord lengths of the phases of the sample must be determined by other experimental techniques. A method is proposed to overcome this difficulty by using two or more wavelengths of radiation; this correction procedure works without the knowledge of the particle sizes of the phases.
The X-Ray powder diffraction patterns of three franckeite specimens from Bolivia all lack the 2.91 and 2.82 Å reflections of 100 intensity reported in PDF 15-25. A new indexed pattern is given for the franckeite of the San José mine, Oruro.
Citation analysis of the articles that appeared in the first five volumes of the journal Powder Diffraction showed that it is clearly a journal of crystallography with strong ties to materials science, mineralogy and analytical chemistry. This specific orientation makes Powder Diffraction invaluable in the existing network of scientific journals.
Accurate, digitized, spectral distribution data are given for CuKα radiation, comprising the profiles of CuKα1, CuKα2 and CuKα3,4. Three consistent analytical procedures are detailed for locating the peak of an X-ray emission line and are found to be superior to the conventional graphical centerline method.
The performances of Seeman-Bohlin (S-B) and Bragg-Brentano (B-B) diffractometers with flat thin film samples were compared on the basis of equal instrumental aberrations. It was found that the S-B arrangement has only a marginal advantage as regards diffracted intensity, and that both types of diffractometer may be successfully employed for characterization of thin films. Diffraction data obtained with very thin metallic films (down to 30 Å) are included for illustration. In order to eliminate reflections from the singlecrystal substrate in the B-B diffractometer, sample tilting was employed. Provided the tilting angle remains within 0.5°, sample tilting causes only moderate additional broadening of the thin film peaks.
Recent developments in the Rietveld method for the analysis of powder diffraction data have seen the method evolve from its original purpose of crystal structure refinement to include the determination of phase abundance in polycrystalline mixtures and the estimation of crystal size and strain parameters. However, the Rietveld method is not easy to use and may deter many powder diffractionists, who are not interested in structure refinement per se, from using the method in its non-structural applications.
In order to overcome the difficulties in using the Rietveld method, a program, QPDA (for Quantitative Powder Diffraction Analysis), has been written that sets the conditions necessary for a single or multi-phase refinement, runs the Rietveld program and extracts phase abundance and size/strain information from the refined parameters. The program comprises a user-friendly, default-driven system of subroutines, written initially in VAX Fortran, and operates from a database of inorganic materials frequently encountered in a wide range of minerals and materials science industries.
Powder diffraction data for 2-aminophenalenone at 295 K (P21/n, Z=4) are given, strong lines: 7.54/X, 7.26/9, 3.34/3. The cell parameters found are a=3.7213(3), b=16.550(2), c=15.095(2) Å, β=92.61(2)°. The crystal structure was determined using powder data and refined giving Rb=0.089. Disordered molecules form stacks along [100] with interplanar spacing of 3.48 Å.