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Micro-area X-ray diffraction measurement by SmartLab μHR diffractometer system with ultra-high brilliance microfocus X-ray optics and two-dimensional detector HyPix-3000

Winter 2016 Vol.32 No.1
Yuji Shiramata

X-ray diffraction is an analytical method for the characterization of the crystalline structure of a material, where the X-ray intensity (I) variation is recorded as a function of diffraction angle (2θ). The diffraction region where 2θ≦10° is called the Small Angle X-ray Scattering (SAXS) area, and the area where 2θ≧5° is called the Wide Angle X-ray Scattering (WAXS) or the Wide Angle X-ray Diffraction (WAXD) area. Since the X-ray diffraction method enables evaluation of various physical properties, it is widely applicable to qualitative analysis (crystal phase identification), quantitative analysis, crystal structure analysis, orientation analysis, particle size analysis and so on.

In general, with the powder X-ray diffraction method, measurement is performed by irradiating X-rays onto a large area of the sample surface, approx. 10 mm×2–3 mm. On the other hand, in order to perform an analysis of a tiny sample, or to analyze something like a micro area of a rock specimen, it is necessary to narrow the X-ray irradiation field to approx. 0.01 mm–1 mm. In the past, because these measurements used the slit collimation method to form a narrow beam by inserting a slit into the incident optical system, X-ray intensity was low and therefore measurements took a long time. However, with the latest X-ray diffractometers, which take advantage of the remarkable progress in technology for components such as the X-ray sources, optical components, detectors and so on, performing high-sensitivity measurements even for tiny samples has been made possible. In this article, various examples of characterizations realized by the state-of-the-art “SmartLab μHR” diffractometer system, equipped with cutting-edge technologies, such as the ultra-high brilliance microfocus X-ray source, a magnificent optic system,


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