Solid-state synthesis of embedded single-crystal metal oxide and phosphate nanoparticles and in situ crystallization

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dc.contributor.author Díaz, Carlos
dc.contributor.author Valenzuela, María Luisa
dc.contributor.author Bravo, Daniel
dc.contributor.author Dickinson, Calum
dc.contributor.author O'Dwyer, Colm
dc.date.accessioned 2016-06-29T15:06:08Z
dc.date.available 2016-06-29T15:06:08Z
dc.date.issued 2011-05-30
dc.identifier.citation Diaz, C., Valenzuela, M. L., Bravo, D., Dickinson, C. and O'Dwyer, C. (2011) 'Solid-state synthesis of embedded single-crystal metal oxide and phosphate nanoparticles and in situ crystallization', Journal of Colloid and Interface Science, 362(1), pp. 21-32. http://www.sciencedirect.com/science/article/pii/S0021979711006461 en
dc.identifier.volume 362 en
dc.identifier.issued 1 en
dc.identifier.startpage 21 en
dc.identifier.endpage 32 en
dc.identifier.issn 0021-9797
dc.identifier.uri http://hdl.handle.net/10468/2814
dc.identifier.doi 10.1016/j.jcis.2011.05.066
dc.description.abstract A new solid state organometallic route to embedded nanoparticle-containing inorganic materials is shown, through pyrolysis of metal-containing derivatives of cyclotriphosphazenes. Pyrolysis in air and at 800 °C of new molecular precursors gives individual single-crystal nanoparticles of SiP2O7, TiO2, P4O7, WP2O7 and SiO2, depending on the precursor used. High resolution transmission electron microscopy investigations reveal, in most cases, perfect single crystals of metal oxides and the first nanostructures of negative thermal expansion metal phosphates with diameters in the range 2–6 nm for all products. While all nanoparticles are new by this method, WP2O7 and SiP2O7 nanoparticles are reported for the first time. In situ recrystallization formation of nanocrystals of SiP2O7 was also observed due to electron beam induced reactions during measurements of the nanoparticulate pyrolytic products SiO2 and P4O7. The possible mechanism for the formation of the nanoparticles at much lower temperatures than their bulk counterparts in both cases is discussed. Degrees of stabilization from the formation of P4O7 affects the nanocrystalline products: nanoparticles are observed for WP2O7, with coalescing crystallization occurring for the amorphous host in which SiP2O7 crystals form as a solid within a solid. The approach allows the simple formation of multimetallic, monometallic, metal-oxide and metal phosphate nanocrystals embedded in an amorphous dielectric. The method and can be extended to nearly any metal capable of successful coordination as an organometallic to allow embedded nanoparticle layers and features to be deposited or written on surfaces for application as high mobility pyrophosphate lithium–ion cathode materials, catalysis and nanocrystal embedded dielectric layers. en
dc.description.sponsorship Fondo Nacional de Desarrollo Científico y Tecnológico, Chile (FONDECYT Grant No. 1085011); Irish Government (INSPIRE programme, Programme for Research in Third Level Institutions, Cycle 4, National Development Plan 2007–2013.) en
dc.format.mimetype application/pdf en
dc.language.iso en en
dc.publisher Elsevier en
dc.rights © 2011 Elsevier Inc. This manuscript version is made available under the CC-BY-NC-ND 4.0 license en
dc.rights.uri http://creativecommons.org/licenses/by-nc-nd/4.0/ en
dc.subject Embedded nanoparticles en
dc.subject Electron microscopy en
dc.subject Organometallics en
dc.subject Nanomaterials en
dc.subject Colloids en
dc.subject Synthesis en
dc.subject Metal oxide en
dc.subject Phosphates en
dc.subject Crystallization en
dc.title Solid-state synthesis of embedded single-crystal metal oxide and phosphate nanoparticles and in situ crystallization en
dc.type Article (peer-reviewed) en
dc.internal.authorcontactother Colm O'Dwyer, Chemistry, University College Cork, Cork, Ireland. +353-21-490-3000 Email: c.odwyer@ucc.ie en
dc.internal.availability Full text available en
dc.date.updated 2012-11-29T17:27:47Z
dc.description.version Accepted Version en
dc.internal.rssid 162343107
dc.contributor.funder Fondo Nacional de Desarrollo Científico y Tecnológico
dc.contributor.funder Higher Education Authority
dc.description.status Peer reviewed en
dc.identifier.journaltitle Journal of Colloid and Interface Science en
dc.internal.copyrightchecked No !!CORA!! en
dc.internal.licenseacceptance Yes en
dc.internal.IRISemailaddress c.odwyer@ucc.ie en


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© 2011 Elsevier Inc. This manuscript version is made available under the CC-BY-NC-ND 4.0 license Except where otherwise noted, this item's license is described as © 2011 Elsevier Inc. This manuscript version is made available under the CC-BY-NC-ND 4.0 license
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