This paper describes the development and testing of a novel capillary flow cell for use in in situ powder X-ray diffraction experiments. It is designed such that it achieves 200° of rotation of the capillary whilst still allowing the flow of gas through the sample and the monitoring of off gas via mass spectrometry, gas chromatography, or other such analytical techniques. This high degree of rotation provides more uniform heating of the sample than can be achieved in static cells or those with lower rotational ranges and consequently also improves particle statistics.
View Article and Find Full Text PDFSynchrotron X-ray tomography (SXRT) has been applied to the study of defects within three-dimensional printed titanium parts. These parts were made using the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V) as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron.
View Article and Find Full Text PDFSynchrotron X-ray tomography has been applied to the study of titanium parts fabricated by additive manufacturing (AM). The AM method employed here was the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V), as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron.
View Article and Find Full Text PDFThis paper reports the results of time-resolved synchrotron small-angle scattering and powder diffraction experiments where natrojarosites were synthesized in situ in order to observe the species produced at the earliest stages of nucleation. The sample temperatures were 333, 353 and 368 K. These compounds were synthesized by co-precipitation from solution on the Small and Wide Angle Scattering and Powder Diffraction beamlines at the Australian Synchrotron.
View Article and Find Full Text PDFJ Synchrotron Radiat
March 2013
This paper reports the results of time-resolved synchrotron powder diffraction experiments where jarosites with different K/H(3)O, K/Na and Na/H(3)O ratios were synthesized in situ at temperatures of 353, 368 and 393 K in order to observe the effect on kinetics and species produced. The Na/H(3)O sample formed monoclinic jarosite at all three temperatures, whereas the K/H(3)O and K/Na samples formed as rhombohedral jarosites at 353 K, and as mixtures of rhombohedral and monoclinic jarosites at the higher temperatures. The relative amount of the monoclinic phase increased with increase in temperature.
View Article and Find Full Text PDFThis paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate the in situ characterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during an in situ study of an operational Fray-Farthing-Chen Cambridge electrowinning cell, featuring molten CaCl(2) as the electrolyte.
View Article and Find Full Text PDFThe design, construction, and commissioning of a stainless steel flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions is described. The use of the cell is demonstrated by a study of Al(OH)(3) scale formation on a mild steel substrate from synthetic Bayer liquor at 70 degrees C. The cell design allows for interchangeable parts and substrates and would be suitable for the study of scale formation in other industrial processes.
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