High-resolution and high-intensity powder diffractometer at BL15XU in SPring-8

Abstract

A new ultra-high-resolution powder diffractometer for synchrotron radiation has been constructed at beamline BL15XU, SPring-8. The two-axis diffractometer is optimized for high-flux and high-coherent X-ray beams, which are provided by combining a planar undulator and a large offset rotated-inclined Si(111) double-crystal mono-chromator. The optics design of the diffractometer is based on transmission geometry, which employs a capillary specimen and reflection geometries using a flat-plate specimen. The intensity data are collected using a 2θ step-scan technique in both geometries. The diffractometer can be arranged in a variety of optical configurations, e.g. simple receiving slits, flat crystal analyzer of Ge(111) or Si(111), and in-vacuum-type long horizontal parallel slits. A minimum full width at half-maximum against 2θ was 0.00572° at λ = 0.63582 Å for the (200) reflections from Si powder in the transmission geometry employing the Ge(111) crystal analyzer. A wide temperature range (32-900 K), which is controlled by a He/N2 gas stream system, is available. 288 structure parameters of a zeolite ZSM-5 sample have been demonstrated to successfully refine with a Rwp value of 6.96% by a Rietveld analysis of the high-resolution powder diffraction data from a 1 mm-diameter capillary specimen.