High-resolution and high-intensity powder diffractometer at BL15XU in SPring-8.
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 monochromator. 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 2theta 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 2theta was 0.00572 degrees at lambda = 0.63582 A 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/N(2) gas stream system, is available. 288 structure parameters of a zeolite ZSM-5 sample have been demonstrated to successfully refine with a R(wp) value of 6.96% by a Rietveld analysis of the high-resolution powder diffraction data from a 1 mm-diameter capillary specimen.
Ikeda
Takuji
T
Advanced Materials Laboratory, National Institute for Material Science, Namiki 1-1, Tsukuba, Ibaraki 305-0044, Japan. takuji-ikeda@aist.go.jp
Nisawa
Atsushi
A
Okui
Masato
M
Yagi
Nobuhiro
N
Yoshikawa
Hideki
H
Fukushima
Sei
S
D003460:Crystallization / Q000379:methods*; D003461:Crystallography / Q000295:instrumentation / Q000379:methods; D004867:Equipment Design; D019544:Equipment Failure Analysis; D033362:Powder Diffraction / Q000295:instrumentation* / Q000379:methods; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D017356:Synchrotrons / Q000295:instrumentation*; D014961:X-Ray Diffraction / Q000295:instrumentation* / Q000379:methods; D017641:Zeolites / Q000737:chemistry* / Q000145:classification*
D017641:Zeolites