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High resolution synchrotron powder diffraction data were collected using beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory using an average wavelength of _______ . Discrete detectors covering an angular range from -6 to 16 2( are scanned over a 34 2( range, with data points collected every 0.001 2( and scan speed of 0.01/s.
The 11-BM instrument uses x-ray optics with two platinum-striped mirrors and a double-crystal Si(111) monochromator, where the second crystal has an adjustable sagittal bend. ADDIN EN.CITE Wang200812212212217Jun WangBrian H. TobyPeter L. LeeLynn RibaudStyle AntaoCharles KurtzMohan RamanathanVon Dreele, Robert B. Mark A. BenoA dedicated powder diffraction beamline at the Advanced Photon Source: Commissioning and early operation resultsReview of Scientific InstrumentsReview of Scientific Instruments0851057920083(Wang et al., 2008) Ion chambers monitor incident flux. A vertical Huber 480 goniometer, equipped with a Heidenhain encoder, positions an analyzer system comprised of twelve perfect Si(111) analyzers and twelve Oxford-Danfysik LaCl3 scintillators, with a spacing of 2 2(. ADDIN EN.CITE Lee200812012012017Peter L. LeeDeming ShuMohan RamanathanCurt PreissnerJun WangMark A. BenoVon Dreele, Robert B. Lynn Ribaud, Charles KurtzSytle M. AntaoXuesong JiaoBrian H. TobyA twelve-analyzer detector system for high-resolution powder diffractionJournal of Synchrotron RadiationJournal of Synchrotron Radiation427-43215520086(Lee et al., 2008) Analyzer orientation can be adjusted individually on two axes. A three-axis translation stage holds the sample mounting and allows it to be spun, typically at ~5400 RPM (90 Hz). A Mitsubishi robotic arm is used to mount and dismount samples on the diffractometer. ADDIN EN.CITE Preissner200927272717Preissner, C.Shu, D.Toby, B. H.Lee, P.Wang, J.Kline, D.Goetze, KThe sample-changing robot for the 11-BM high-throughput powder diffraction beamlineNuclear Instruments and Methods in Physics Research ANuclear Instruments and Methods in Physics Research Ain press2009(Preissner et al., 2009) An Oxford Cryosystems Cryostream Plus device allows sample temperatures to be controlled over the range 80-500 K when the robot is used.
The diffractometer is controlled via EPICS ADDIN EN.CITE Dalesio199468686817Dalesio, L. R.Hill, J. O.Kraimer, M.Lewis, S.Murray, D.Hunt, S.Watson, W.Clausen, M.Dalesio, J.The Experimental Physics and Industrial Control-System Architecture - Past, Present, and FutureNuclear Instruments & Methods in Physics Research Section A-Accelerators Spectrometers Detectors and Associated EquipmentNuclear Instruments & Methods in Physics Research Section a-Accelerators Spectrometers Detectors and Associated Equipment179-1843521-219940168-9002WOS:A1994QA95300048(Dalesio et al., 1994). Data are collected while continually scanning the diffractometer 2( arm. A mixture of NIST standard reference materials, Si (SRM 640c) and Al2O3 (SRM 676) is used to calibrate the instrument, where the Si lattice constant determines the wavelength for each detector. Corrections are applied for detector sensitivity, 2( offset, small differences in wavelength between detectors, and the source intensity, as noted by the ion chamber before merging the data into a single set of intensities evenly spaced in 2(.
ADDIN EN.REFLIST Dalesio, L. R., Hill, J. O., Kraimer, M., Lewis, S., Murray, D., Hunt, S., Watson, W., Clausen, M., and Dalesio, J. (1994). The Experimental Physics and Industrial Control-System Architecture - Past, Present, and Future, Nuclear Instruments & Methods in Physics Research Section A-Accelerators Spectrometers Detectors and Associated Equipment 352, 179-184.
Lee, P. L., Shu, D., Ramanathan, M., Preissner, C., Wang, J., Beno, M. A., Von Dreele, R. B., Lynn Ribaud, Kurtz, C., Antao, S. M., Jiao, X., and Toby, B. H. (2008). A twelve-analyzer detector system for high-resolution powder diffraction, Journal of Synchrotron Radiation 15, 427-432.
Preissner, C., Shu, D., Toby, B. H., Lee, P., Wang, J., Kline, D., and Goetze, K. (2009). The sample-changing robot for the 11-BM high-throughput powder diffraction beamline, Nuclear Instruments and Methods in Physics Research A in press,
Wang, J., Toby, B. H., Lee, P. L., Ribaud, L., Antao, S., Kurtz, C., Ramanathan, M., Von Dreele, R. B., and Beno, M. A. (2008). A dedicated powder diffraction beamline at the Advanced Photon Source: Commissioning and early operation results, Review of Scientific Instruments 79, 085105.
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