A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors

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dc.contributor.authorHoeher, Alexandriaen
dc.contributor.authorMergelsberg, Sebastian T.en
dc.contributor.authorBorkiewicz, Olaf J.en
dc.contributor.authorDove, Patricia M.en
dc.contributor.authorMichel, F. Marcen
dc.date.accessioned2021-10-13T13:13:06Zen
dc.date.available2021-10-13T13:13:06Zen
dc.date.issued2019-09-01en
dc.date.updated2021-10-13T13:13:03Zen
dc.description.abstractStructural investigations of amorphous and nanocrystalline phases forming in solution are historically challenging. Few methods are capable of in situ atomic structural analysis and rigorous control of the system. A mixed-flow reactor (MFR) is used for total X-ray scattering experiments to examine the short- and long-range structure of phases in situ with pair distribution function (PDF) analysis. The adaptable experimental setup enables data collection for a range of different system chemistries, initial supersaturations and residence times. The age of the sample during analysis is controlled by adjusting the flow rate. Faster rates allow for younger samples to be examined, but if flow is too fast not enough data are acquired to average out excess signal noise. Slower flow rates form older samples, but at very slow speeds particles settle and block flow, clogging the system. Proper background collection and subtraction is critical for data optimization. Overall, this MFR method is an ideal scheme for analyzing the in situ structures of phases that form during crystal growth in solution. As a proof of concept, high-resolution total X-ray scattering data of amorphous and crystalline calcium phosphates and amorphous calcium carbonate were collected for PDF analysis.en
dc.description.versionPublished versionen
dc.format.extentPages 758-765en
dc.format.extent8 page(s)en
dc.format.mimetypeapplication/pdfen
dc.identifier.doihttps://doi.org/10.1107/S2053273319008623en
dc.identifier.eissn2053-2733en
dc.identifier.issn2053-2733en
dc.identifier.issuePt 5en
dc.identifier.orcidMichel, Frederick [0000-0003-2817-980X]en
dc.identifier.otherS2053273319008623 (PII)en
dc.identifier.pmid31475919en
dc.identifier.urihttp://hdl.handle.net/10919/105283en
dc.identifier.volume75en
dc.language.isoenen
dc.publisherInternational Union of Crystallographyen
dc.relation.urihttp://gateway.webofknowledge.com/gateway/Gateway.cgi?GWVersion=2&SrcApp=PARTNER_APP&SrcAuth=LinksAMR&KeyUT=WOS:000484157300008&DestLinkType=FullRecord&DestApp=ALL_WOS&UsrCustomerID=930d57c9ac61a043676db62af60056c1en
dc.rightsCreative Commons Attribution 4.0 Internationalen
dc.rights.urihttp://creativecommons.org/licenses/by/4.0/en
dc.subjectPhysical Sciencesen
dc.subjectChemistry, Multidisciplinaryen
dc.subjectCrystallographyen
dc.subjectChemistryen
dc.subjectin situ X-ray total scatteringen
dc.subjectcrystallizationen
dc.subjectamorphous calcium phosphateen
dc.subjectamorphous calcium carbonateen
dc.subjectpair distribution function analysisen
dc.subjectPAIR DISTRIBUTION FUNCTIONen
dc.subjectCALCIUM-PHOSPHATEen
dc.subjectAREA DETECTORen
dc.subjectFLOW REACTORen
dc.subjectCARBONATEen
dc.subjectCLUSTERSen
dc.titleA new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactorsen
dc.title.serialActa Crystallographica A - Foundations and Advancesen
dc.typeArticle - Refereeden
dc.type.dcmitypeTexten
dc.type.otherArticleen
dc.type.otherJournalen
dcterms.dateAccepted2019-06-17en
pubs.organisational-group/Virginia Techen
pubs.organisational-group/Virginia Tech/Scienceen
pubs.organisational-group/Virginia Tech/Science/Geosciencesen
pubs.organisational-group/Virginia Tech/University Research Institutesen
pubs.organisational-group/Virginia Tech/University Research Institutes/Fralin Life Sciencesen
pubs.organisational-group/Virginia Tech/All T&R Facultyen
pubs.organisational-group/Virginia Tech/Science/COS T&R Facultyen
pubs.organisational-group/Virginia Tech/University Research Institutes/Fralin Life Sciences/Durelle Scotten

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