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An in situ XAS study of the activation of precursor-dependent Pd nanoparticles

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An in situ XAS study of the activation of precursor-dependent Pd nanoparticles

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dc.contributor.author Wittee Lopes, Christian es_ES
dc.contributor.author Cerrillo, José Luis es_ES
dc.contributor.author Palomares Gimeno, Antonio Eduardo es_ES
dc.contributor.author Rey Garcia, Fernando es_ES
dc.contributor.author Agostini, G. es_ES
dc.date.accessioned 2020-05-20T03:01:30Z
dc.date.available 2020-05-20T03:01:30Z
dc.date.issued 2018-05-14 es_ES
dc.identifier.issn 1463-9076 es_ES
dc.identifier.uri http://hdl.handle.net/10251/143781
dc.description.abstract [EN] The activation of precursor-dependent Pd nanoparticles was comprehensively followed by in situ X-ray absorption spectroscopy on two inorganic supports for rationalizing the final catalytic activity. Two series of Pd-based catalysts (7 wt% Pd) were prepared by impregnation of gamma-Al2O3 and activated carbon supports varying the metal precursor (Pd(NO3)(2), PdCl2 and Pd(OAc)(2)). The most relevant physicochemical properties of the studied catalysts were determined by several techniques including ICP-OES, XRD, N-2 adsorption and XAS. The results indicate that the thermal stability of the metal precursor plays an important role in the size and speciation of the formed Pd nanoparticles after the activation process. The Cl-based precursor, which presents high thermal stability, passes through a PdOxCly mixed phase when submitted to calcination on Pd/Al2O3 and leaves Cl-species after metal reduction on Pd/C (which can be detrimental to catalytic reactions). Differently, Pd(OAc)(2) and Pd(NO3)(2) promote the formation of larger species due to different precursor decomposition pathways. Ordered PdO is observed even before calcination when Pd(NO3)(2) was used as a metallic source, which translates into large nanoparticles after reduction in H-2. By using the average coordination numbers of Pd species obtained from EXAFS data of the as-reduced catalysts, a correlation was observed comparing the three precursors: PdCl2 generates smaller nanoparticles than Pd(OAc)(2), which in turn generates smaller nanoparticles than Pd(NO3)(2), regardless of the support used for catalyst preparation. es_ES
dc.description.sponsorship The authors thank the Spanish Ministry of Economy and Competitiveness through MAT2015-71842-P (MINECO/FEDER) and SEV-2016-0683 projects for the financial support. We gratefully acknowledge ALBA synchrotron for allocating beamtime (proposal 2015091414), Carlo Marini and CLAESS beamline staff for their help and technical support during our experiment. C. W. Lopes (Science without Frontiers - Process no. 13191/13-6) thanks CAPES for a predoctoral fellowship. J.L. Cerrillo wishes to thank MINECO for the Severo Ochoa contract for PhD formation (SVP-2014-068600). es_ES
dc.language Inglés es_ES
dc.publisher The Royal Society of Chemistry es_ES
dc.relation.ispartof Physical Chemistry Chemical Physics es_ES
dc.rights Reserva de todos los derechos es_ES
dc.subject.classification INGENIERIA QUIMICA es_ES
dc.title An in situ XAS study of the activation of precursor-dependent Pd nanoparticles es_ES
dc.type Artículo es_ES
dc.identifier.doi 10.1039/C8CP00517F es_ES
dc.relation.projectID info:eu-repo/grantAgreement/CAPES//13191%2F13-6/ es_ES
dc.relation.projectID info:eu-repo/grantAgreement/MINECO//SVP-2014-068600/ES/SVP-2014-068600/ es_ES
dc.relation.projectID info:eu-repo/grantAgreement/MINECO//MAT2015-71842-P/ES/SINTESIS Y CARACTERIZACION AVANZADA DE NUEVOS MATERIALES ZEOLITICOS Y APLICACIONES EN ADSORCION, MEDIOAMBIENTE Y EN LA CONSERVACION DE ALIMENTOS/ es_ES
dc.relation.projectID info:eu-repo/grantAgreement/MINECO//SEV-2016-0683/ es_ES
dc.rights.accessRights Abierto es_ES
dc.contributor.affiliation Universitat Politècnica de València. Instituto Universitario Mixto de Tecnología Química - Institut Universitari Mixt de Tecnologia Química es_ES
dc.contributor.affiliation Universitat Politècnica de València. Departamento de Ingeniería Química y Nuclear - Departament d'Enginyeria Química i Nuclear es_ES
dc.description.bibliographicCitation Wittee Lopes, C.; Cerrillo, JL.; Palomares Gimeno, AE.; Rey Garcia, F.; Agostini, G. (2018). An in situ XAS study of the activation of precursor-dependent Pd nanoparticles. Physical Chemistry Chemical Physics. 20(18):12700-12709. https://doi.org/10.1039/C8CP00517F es_ES
dc.description.accrualMethod S es_ES
dc.relation.publisherversion https://doi.org/10.1039/C8CP00517F es_ES
dc.description.upvformatpinicio 12700 es_ES
dc.description.upvformatpfin 12709 es_ES
dc.type.version info:eu-repo/semantics/publishedVersion es_ES
dc.description.volume 20 es_ES
dc.description.issue 18 es_ES
dc.identifier.pmid 29697116 es_ES
dc.relation.pasarela S\356558 es_ES
dc.contributor.funder Ministerio de Economía y Competitividad es_ES
dc.contributor.funder Coordenaçao de Aperfeiçoamento de Pessoal de Nível Superior, Brasil es_ES
dc.contributor.funder European Regional Development Fund es_ES
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