Modern Techniques in X-Ray Diffraction-Applied to Metallurgy (bbfe3d1b-22a8-4c28-9904-0ec5cfab25ed)

"Through the application of the Rietveld method, X-ray diffraction analysis has developed into a fully quantitative method for phase analysis. The Rietveld method itself has progressed from an unstable method that required constant operator intervention to a stable and robust method suited even for routine analysis. The method however, requires a good initial calibration and periodic checks on its precision and accuracy.Several examples from minerals processing, pyrometallurgy, and materials science show the strengths and applicability of the method. The limitations and sources of error are also discussed.1. IntroductionDiffraction of X-rays by matter has been used for more than 80 years, initially to elucidate the structure of crystalline matter, and to investigate the bonding between atoms. The first development of powder diffraction cameras and the later development of X-ray diffractometers saw the development of methods to identify phases and to try to quantify them in mixtures. A comprehensive database and search-match techniques have been developed over the ensuing years. Effective and accurate quantification had to wait for the so-called Rietveld' analysis where the total diffraction pattern is used and where the crystal structure data for the constituent phases are needed as input. Overlapping of diffraction peaks of different phases is handled without difficulty and reliable results can be obtained in spite of this occurrence.The development of methods for structure analysis from powder data has also progressed rapidly and more and more complex structures are being solved from first principles, i.e. without knowledge of unit cell or space group data. Because of the ease of use of the Rietveld method, it is finding increased application in metallurgy, especially in the quantification of phases of importance in minerals processing, in pyrometallurgical processes, and in materials characterization. This study will examine the principles of the Rietveld method, its application in metallurgy, and finally also the common pitfalls that need to be avoided.2. Rietve1d AnalysisAs the Rietveld method compares the experimental diffraction pattern with one calculated from known crystal structure data, the following data are needed:•,An XRD Pattern with as Iowa background as possible. This should have good resolution and high diffraction peak intensities. With modem X-ray detectors, this can be achieved in minutes rather than hours.•,Instrumental parameters such as goniometer radii and slit sizes are needed. These are the so-called ""Fundamental parameters"". They are used to calculate the shapes of the resultant diffraction peak profiles that are caused by the instrument. The parameters are used to correctly separate the instrumental effects on the diffraction pattern from the sample effects."