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Notes: Design features of a proposed high-resolution, high-speed powder diffractometer for operation at a synchrotron source are described. A key feature of the design is the use of imaging plates to record an almost complete range of data including both the high-angle and the small-angle scattering regime. The x-ray optics involve the use of a condensing-collimating channel-cut monochromator (CCCC) to achieve narrow parallel beams with cross sections of the order of 50 μm in the plane of diffraction, so that geometrical aberrations are very low and the beam cross section is well matched to the spatial resolution of the imaging plate detector. Angular resolution in 2θ of the diffractometer is easily variable, and designed to range from 0.01° upwards. Optional translation of the detector perpendicular to the incident-beam direction makes it possible to obtain time-resolved data. Applications of the instrument include high-resolution powder data collection for Rietveld analysis, studies of dynamic phenomena such as chemical reactions and phase transformations, particle-size determination, texture analysis, residual-stress measurements, single-crystal studies of the truncation-rod effect and surface scattering, microdiffraction, combined high-angle and small-angle scattering measurements, and studies of multilayer structures. As an illustration of the sort of results attainable with the proposed system, we present an oscillation photograph of the crystal-truncation rod effect for a Si wafer which was recorded at a synchrotron source using an imaging plate as the detector.

Notes: A diffractometer has been constructed for structural studies of high-temperature melt with synchrotron radiation. It was designed to measure diffracted intensities from the free surface of a molten sample by scanning a scintillation counter with a fixed glancing angle of the incident beam. In order to heat samples up to 1500 °C, a small electric furnace is attached to the diffractometer. It carries a hemicircular (100 mm in diameter) cover, which has a window for the passage of x rays. The window is covered with a Kapton film. The sample container made of 30 Rh-Pt is mounted at the center of the furnace. A test measurement was performed on GeO2. Monochromatic beams with λ=1.32 A and its second harmonics were taken out of synchrotron radiation by a β-alumina crystal (d002=11.3 A) and used as incident beams. To partial scattering curves obtained with λ and λ/2 were combined to a single curve after correction for absorption. The radial distribution function obtained from these data is in good agreement with that previously reported which was derived from diffraction data collected on a conventional diffractometer.

Notes: In the field of material sciences, it has long been desired to develope the equipment to obtain crystallographic information of micrometer-size crystalline substances. Synchrotron radiation (SR) could be a candidate to deal with such a small specimen other than electron microscope. It seems more advantageous to utilize SR from the viewpoint that the processing of the diffraction data that has already been established for identification of the materials, structure analysis, and refinement. Even in the case of SR, special care should be taken for the measurement of very weak diffracted intensities. In the case not using SR, the size of 50 μm might be the limit for the specimen to be examined by the diffraction method. The diffracted intensity is proportional to the volume of the specimen, and that of micrometer-size crystal is estimated as 10−5 times of that of the limit mentioned above. The noise level of the experiment, therefore, should be as low as possible. If the noise level becomes negligibly small, the signal could be accumulated continually to the desired intensity level by adjusting measuring time. The experiment, for the purpose, should be carried out in vacuum with the stational crystal method and with very narrow collimated x-ray beams.The Laue method is employed by the above reason, as well as the fact that the intensity of each Bragg reflection on a reciprocal row passing through the origin of the reciprocal space is superposed with each other, which also intensifies a diffraction spot on the photographic plate. The Laue camera is set up at BL-4B of Photon Factory, sealed in vacuum and installed with a very narrow collimater. The development of the system has been performed to the level which several Bragg reflections of molybdenum single crystal with 0.8 μm in its diameter can be taken on the imaging plate for 50-min exposure with ring current from 128 to 125 mA. The origin of diamonds in meteorites has been a controversy as to whether they are formed from carbonaceous materials by impact shock or directly formed from vapor. Recent discovery of vapor-growth diamonds in carbonaceous chondrites has generated a renewed interest in the origin of ureilite diamonds. Two types of micrometer-size diamonds were prepared. One of them was grown under low pressure by chemical vapor deposition (CVD) from gaseous mixtures of H2 and CH4, and another was synthesized by shock effect (kindly offered by Nippon Oil & Fats Co., Ltd.) The micro-Laue method was applied to them in order to get information about their microstructures. Two characteristics are recognized in profiles of reflections themselves and in whole patterns of the Laue photographs. The reflections of CVD diamonds are elongated but symmetric in their profiles and are distributed regularly as they are indexed by the diamond lattice, while those of shock effect are also elongated and asymmetric, and are distributed at random as they cannot be indexed. The characteristics observed by the method may be useful to ascribe the origin to CVD or shock effect.