Implementation of in situ SAXS/WAXS characterization into silicon/glass microreactors

Lab on a Chip
Thomas BeuvierAlain Gibaud

Abstract

A successful implementation of in situ X-ray scattering analysis of synthetized particle materials in silicon/glass microreactors is reported. Calcium carbonate (CaCO3) as a model material was precipitated inside the microchannels through the counter-injection of two aqueous solutions, containing carbonate ions and calcium ions, respectively. The synthesized calcite particles were analyzed in situ in aqueous media by combining Small Angle X-ray Scattering (SAXS) and Wide Angle X-ray Scattering (WAXS) techniques at the ESRF ID02 beam line. At high wavevector transfer, WAXS patterns clearly exhibit different scattering features: broad scattering signals originating from the solvent and the glass lid of the chip, and narrow diffraction peaks coming from CaCO3 particles precipitated rapidly inside the microchannel. At low wavevector transfer, SAXS reveals the rhombohedral morphology of the calcite particles together with their micrometer size without any strong background, neither from the chip nor from the water. This study demonstrates that silicon/glass chips are potentially powerful tools for in situ SAXS/WAXS analysis and are promising for studying the structure and morphology of materials in non-conventional conditions like g...Continue Reading

References

Jul 28, 2006·Nature·Jamil El-AliKlavs F Jensen
Jul 28, 2006·Nature·Paul YagerBernhard H Weigl
Oct 20, 2007·Journal of the American Chemical Society·Daniela C PopescuNico A J M Sommerdijk
Jan 2, 2009·Analytical Chemistry·Huabing YinMaggie Cusack
Aug 15, 2009·Lab on a Chip·Ryan L Hartman, Klavs F Jensen
Oct 30, 2009·Lab on a Chip·Fanny DestremautJean-Paul Chapel
Feb 25, 2010·Chemical Society Reviews·Samuel Marre, Klavs F Jensen
Dec 25, 2010·Lab on a Chip·A M NightingaleJ C deMello
Jan 8, 2011·Lab on a Chip·Martha Elisabeth BrennichSarah Köster
Jun 29, 2011·Angewandte Chemie·Ryan L HartmanKlavs F Jensen
Feb 23, 2013·Lab on a Chip·Ralf StehleSebastian Seiffert
May 29, 2014·Lab on a Chip·Klavs F JensenStephen G Newman

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Citations

Nov 26, 2015·Analytical Chemistry·Damith E W PatabadigeChristopher T Culbertson
Feb 12, 2020·Materials·Theyencheri Narayanan, Oleg Konovalov
Jun 14, 2018·Journal of Applied Crystallography·Carlos G LopezJoão T Cabral
Jul 1, 2021·Nanoscale·Nicolas RolleyBrice Calvignac

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