Long Horizontal Parallel Slits with 0.03° Angular Resolution for Powder Diffraction Using Synchrotron Radiation

Toraya, Hideo; Takata, Masaki; Hibino, H.; Yoshino, J.; Ohsumi, Kazumasa

doi:10.1107/s0909049595002408

Cited by 5 publications

(3 citation statements)

References 9 publications

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“…Components of the diffractometer BL15XU are based on the multiple-detector system (MDS), which Toraya et al (1996) have constructed, although our diffractometer is equipped with a single detector arm. Either a crystal analyzer or in-vacuum-type long horizontal parallel slits (Parrish et al, 1986;Toraya et al, 1995) can be selected. The former gives a high angular resolution and a good signal-to-noise ratio, but its Bragg re¯ection angles must be realigned at each wavelength (Cox et al, 1986).…”

Section: Conceptmentioning

confidence: 99%

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

Ikeda¹,

Nisawa²,

Okui³

et al. 2003

J Synchrotron Radiat

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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.

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Section: Conceptmentioning

confidence: 99%

“…Various types of high-resolution powder diffractometers are commonly used, e.g. BM16 (Fitch, 1996) and SNBL at the ESRF, X3B1 and X7A at NSLS, BL-4B2 at KEK-PF (Toraya et al, 1996), BL02B2 at SPring-8 (Nishibori et al, 2001) and Station 2.3 at CLRC (Collins et al, 1992).…”

Section: Introductionmentioning

confidence: 99%

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

Ikeda¹,

Nisawa²,

Okui³

et al. 2003

J Synchrotron Radiat

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“…developed in a previous study (Toraya, Takata, Hibino, Yoshino & Ohsumi, 1995), and a set of receiving slits are available for use together with the Soller slits (angular aperture of 2°). Different types of fiat and channel-cut crystals and a clasp for attaching a Peltier-type solid-state detector will be available for use by the end of 1995.…”

Section: Multi-purpose Detector Armmentioning

confidence: 99%

A New Powder Diffractometer for Synchrotron Radiation with a Multiple-Detector System

Toraya¹,

Hibino²,

Ohsumi³

1996

J Synchrotron Radiat

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117

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A new powder diffractometer for synchrotron radiation with six detector arms has been constructed. Five detector arms are attached radially at intervals of 25 ° to the 20 axis and form a multiple-detector system. Five scintillation counters coupled with flat Ge(111) crystal analyzers on the respective arms can simultaneously record the whole powder pattern divided into five segments, each with an equal 20 span. The optics design is based on flat-specimen reflection geometry using a parallel beam. The intensity data are collected using a 20 step-scan technique in asymmetric diffraction at a fixed incident angle. A sixth multi-purpose detector arm can be used in the conventional single-arm scan mode. It can be equipped with various kinds of analyzers such as long horizontal parallel slits, a fiat or channel-cut crystal analyzer, a receiving slit and a solid-state detector. Test operations of the multiple-detector system, conducted at the Photon Factory in Tsukuba, recorded a full width at half maximum of 0.022 ° and a peak maximum intensity of more than 40000 counts s -I for the (111) reflection from Si powder. The whole powder pattern of Mg2SiO4 over a 20 range of 130 ° could be step-scanned at a step interval of 0.004 ° (20) in just 4 h. Results of whole-powder-pattern decomposition and Rietveld refinement of the Mg2SiO4 pattern are given.

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Quadrupole lamp furnace for high temperature (up to 2050K) synchrotron powder x-ray diffraction studies in air in reflection geometry

Sarin

Yoon

Jurkschat

et al. 2006

Review of Scientific Instruments

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A four-lamp thermal image furnace has been developed to conduct high temperature x-ray diffraction in reflection geometry on oxide ceramic powder samples in air at temperatures ⩽2050K using synchrotron radiation. A refractory crucible made of Pt20%Rh alloy was used as a specimen holder. A material with well characterized lattice expansion properties was used as an internal crystallographic thermometer to determine the specimen temperature and displacement. The performance of the apparatus was verified by measurement of the thermal expansion properties of CeO2, MgO, and Pt which were found to be within ±3% of the acceptable values. The advantages, limitations, and important considerations of the instrument developed are discussed.

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Long Horizontal Parallel Slits with 0.03° Angular Resolution for Powder Diffraction Using Synchrotron Radiation

Cited by 5 publications

References 9 publications

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

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

A New Powder Diffractometer for Synchrotron Radiation with a Multiple-Detector System

Quadrupole lamp furnace for high temperature (up to 2050K) synchrotron powder x-ray diffraction studies in air in reflection geometry

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