Abstract
Crystal truncation rod (CTR) X-ray diffraction is an invaluable tool for measuring mineral surface and adsorbate structures, and has been applied to several environmentally and geochemically important systems. Traditionally, the method has been restricted to single crystals with lateral dimensions >3 mm. Minerals that meet this size criterion represent a minute fraction of those that are relevant to interfacial geochemistry questions, however. Crystal screening, data collection, and CTR measurement methods have been developed for crystals of <0.3 mm in lateral size using the manganese oxide mineral chalcophanite (ZnMn3O7·3H2O) as a case study. This work demonstrates the feasibility of applying the CTR technique to previously inaccessible surfaces, opening up a large suite of candidate substrates for future study.
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ACKNOWLEDGMENTS
The authors thank Dr. Jeffrey E. Post at the National Museum of Natural History for providing chalcophanite crystals as well as fruitful discussions. Instrumentation developments, measurements, and analysis were supported by U.S. Department of Energy (DOE), Basic Energy Sciences (BES), Chemical Sciences, Geosciences, and Biosciences (CSGB) Division, Geosciences program (DE-FG02-94ER14466 and DE-SC0019108). CTR measurements were made at GeoSoilEnviroCARS, The University of Chicago – a user facility supported by the National Science Foundation, Earth Sciences (EAR – 1634415). GeoSoilEnviroCARS is located at the Advanced Photon Source, a DOE Office of Science User Facility operated by Argonne National Laboratory under Contract No. DE-AC02-06CH11357.
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This article is a product of the 2020 CMS Workshop held in conjunction with the 57th Annual Meeting of The Clay Minerals Society, Richland, Washington, USA.
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Stubbs, J.E., Wanhala, A.K. & Eng, P.J. INTERFACIAL X-RAY SCATTERING FROM SMALL SURFACES: ADAPTING MINERAL-FLUID STRUCTURE METHODS FOR MICROCRYSTALLINE MATERIALS. Clays Clay Miner. 69, 688–701 (2021). https://doi.org/10.1007/s42860-021-00155-4
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DOI: https://doi.org/10.1007/s42860-021-00155-4