Basics of X-ray Diffraction (original) (raw)

X-Ray Diffraction in Mineralogical Research

Journal of ISAS

A brief account of role of X-ray diffraction (XRD) in mineralogical research with special reference to radioactive and atomic minerals is given. Aspects of research methodology such as sample preparation, analysis time, limitations, search match methods for identification, and complimentary techniques are also given. The most common applications of XRD in mineralogical researches related to radioactive/atomic minerals include identification of primary and secondary uranium and associated ore and gangue minerals, determination of the oxidation grade of uraninites, identification of Th, Nb, Ta, Sn, Be, Li, Zr, Hf, Ti, rare-earth elements (REE) minerals, investigations on degree of structural disordering in Nb-Ta minerals, X-ray crystallographic and substitutional solid solution studies, clay minerals, triclinicity of K-feldspar, metamict minerals and influence of the degree of metamictisation on uranium beneficiation, characterisation of leached residue, beneficiated, heat-treated pro...

X-Ray Diffraction Techniques for Mineral Characterization: A Review for Engineers of the Fundamentals, Applications, and Research Directions

X-ray diffraction (XRD) is an important and widely used material characterization technique. With the recent development in material science technology and understanding, various new materials are being developed, which requires upgrading the existing analytical techniques such that emerging intricate problems can be solved. Although XRD is a well-established non-destructive technique, it still requires further improvements in its characterization capabilities, especially when dealing with complex mineral structures. The present review conducts comprehensive discussions on atomic crystal structure, XRD principle, its applications, uncertainty during XRD analysis, and required safety precautions. The future research directions, especially the use of artificial intelligence and machine learning tools, for improving the effectiveness and accuracy of the XRD technique, are discussed for mineral characterization. The topics covered include how XRD patterns can be utilized for a thorough understanding of the crystalline structure, size, and orientation, dislocation density, phase identification, quantification, and transformation, information about lattice parameters, residual stress, and strain, and thermal expansion coefficient of materials. All these important discussions on XRD analysis for mineral characterization are compiled in this comprehensive review, so that it can benefit specialists and engineers in the chemical, mining, iron, metallurgy, and steel industries.

Mineral characterization using micro x-ray diffraction (micro XRD), a state-of-the-art non-destructive technique

Micro x-ray diffraction, a technique that enables imaging and mapping of the phase distribution in complex minerals, was used to explore the mineralogy of bauxite samples and to obtain x-ray diffraction patterns of trace level minerals. Micro x-ray diffraction can be used to obtain information on unusual and or trace level samples that cannot be studied by conventional powder x-ray diffraction methods and or solid samples that are not in powder form. High quality x-ray diffraction patterns of trace level samples of gibbsite, boehmite and hematite. Micro x-ray diffraction mapping and line scan of bauxite samples and leach residue (whole rock and polished) revealed details of the mineralogy and grain location of the minerals in bauxite.

Combining XRF and XRD analyses and sample preparation to solve mineralogical problems

South African Journal of Geology, 2008

X-ray Fluorescence Spectroscopy (XRF) has reached the stage where it is classified as a mature analytical technique. The theoretical principles are well understood. In addition modern instrumentation demonstrates enhanced generator and temperature stability. High sensitivity is possible even for light elements and effective matrix correction software is available to the modem day spectroscopist. Apart from its continued applications in researcli and development. XRF has become u routine prcjcess control tool. X-ray Powder diffraction (XRD), on the other hand, has with minor exceptions as in the cement industry, largely remained a research tool, despite being an older analytical technique than XRF XRD has progressed significantly in the past decade from a mainly qualitative technique for the identification of crystalline materials to a quantitative tool with the advance of more powerful software packages. This software has improved instrument control, but also quantification and structure determination using the Rietveld method. Consequently, XRD is rapidly entering the process control environment. In this paper the authors demonstrate, with practical examples from different industrial applications, how combined XRF and XRD use can provide truly quantitative phase analyses. XRF is used to verify XRD data and visa versa. The data obtained in this study clearly illustrate the value that can be added to either technique if XRF and XRD data are used together, and indicate some applications in routine process co.

Quantitative X-ray diffraction analysis of clay-bearing rocks from random preparations

… Clay Minerals, 2001

An internal standard X-ray diffraction (XRD) analysis technique permits reproducible and accurate calculation of the mineral contents of rocks, including the major clay mineral families: Fe-rich chlorites + berthierine, Mg-rich chlorites, Fe-rich dioctahedral 2:1 clays and micas, Al-rich dioctahedral 2:1 clays and micas, and kaolinites. A single XRD pattern from an air-dried random specimen is used. Clays are quantified from their 060 reflections which are well resolved and insensitive to structural defects. Zincite is used as the internal standard instead of corundum, because its reflections are more conveniently located and stronger, allowing for a smaller amount of spike (10%). The grinding technique used produces powders free of grains coarser than 20 ixm and suitable for obtaining random and rigid specimens.

Study of Crystallite Size and Microstrain Using X-Ray Diffractometer (XRD

IRJET, 2022

With latest expansion in the field of substantial science technology novel resources are being developed, the prevailing methods of analysis and trying cannot keep up. Hence the obligation of upgrading the current analytical methods or emerging new ones to solve the intricate problems vacant by the development of new ingredients. XRD (X-Ray Diffraction) is performance involving X-rays to be passed through a given material, be it powdered, and observe the rays ephemeral through it to understand/gover the assembly of the factual. XRD works be computing the angles and intensity of the passing through rays and engendering a 3D model with proper bulks of the given material sample. The need for XRD is due to the fact that crystals formed in earth’s crust are widely affected by peripheral factors such a temperature, pressure and the rate at which they cool down. These factors affect the prearrangement of atoms in minerals and owing it to these preparations, the physical belongings of minerals widely differ. With the help of XRD, the translucent structure, size orientation, density etc. and residual stress & strain are calculated. The XRD skill in turn gives out results/data in the form of diffractogram, the diffractogram thus gained is in the form of a line or peak with different intensities and spots that are specific to the material being used for examination. Each pulverized crystalline phase has a diffractogram which is distinguishing which is unique to each material

Portable X-ray powder diffractometer for the analysis of art and archaeological materials

2011

Phase identification based on nondestructive analytical techniques using portable equipment is ideal for the analysis of art and archaeological objects. Portable(p)-XRF and p-Raman are very widely used for this purpose, yet p-XRD is relatively rare despite its importance for the analysis of crystalline materials. This paper overviews 6 types of p-XRD systems developed for analysis of art and archaeological materials. The characteristics of each system are compared. One of the p-XRD systems developed by the authors was brought to many museums as well as many archeological sites in Egypt and Syria to characterize the cultural heritage artifacts, e.g., amulet made of Egyptian blue, blue painted pottery, and Islamic pottery from Egypt, jade from China, variscite from Syria, a Japanese classic painting drawn by Korin Ogata, and oil paintings drawn by Taro Okamoto. Practical application data are shown to demonstrate the potential ability of the method for analysis of various art and archaeological materials.