Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid

Autores
Parra, Rodrigo; Goes, M. S.; Castro, Miriam Susana; Longo, Elson; Bueno, Paulo Roberto; Varela, José Arana
Año de publicación
2008
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Anatase nanoparticles were obtained through a modified sol-gel route from titanium isopropoxide modified with acetic acid in order to control hydrolysis and condensation reactions. The modification of Ti(OiPr)4 with acetic acid reduces the availability of groups that hydrolyze and condense easily through the formation of a stable complex whose structure was determined to be Ti(OCOCH3)(OlPr)2 by means of FTIR and 13C NMR. The presence of this complex was confirmed with FTIR in the early stages of the process. A doublet in 1542 and 1440 cm-1 stands for the asymmetric and symmetric stretching vibrations of the carboxylic group coordinated to Ti as a bidentate ligand. The gap of 102 cm-1 between these signals suggests that acetate acts preferentially as a bidentate rather than as a bridging ligand between two titanium atoms. The use of acetic acid as modifier allows the control of both the degree of condensation and oligomerization of the precursor and leads to the preferential crystallization of TiO2 in the anatase phase. A possible reaction pathway toward the formation of anatase is proposed on the basis of the intermediate species present in a 1:1 Ti(OiPr)4:CH3COOH molar system in which esterification reactions that introduce H2O into the reaction mixture were seen to be negligible. The Rietveld refinement and TEM analysis revealed that the powder is composed of isotropic anatase nanocrystallites.
Fil: Parra, Rodrigo. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Goes, M. S.. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Fil: Castro, Miriam Susana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Longo, Elson. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Fil: Bueno, Paulo Roberto. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Fil: Varela, José Arana. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Materia
Anatase Synthesis
Sol-Gel Route
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/69242
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/69242
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acidParra, RodrigoGoes, M. S.Castro, Miriam SusanaLongo, ElsonBueno, Paulo RobertoVarela, José AranaAnatase SynthesisSol-Gel Routehttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1Anatase nanoparticles were obtained through a modified sol-gel route from titanium isopropoxide modified with acetic acid in order to control hydrolysis and condensation reactions. The modification of Ti(OiPr)4 with acetic acid reduces the availability of groups that hydrolyze and condense easily through the formation of a stable complex whose structure was determined to be Ti(OCOCH3)(OlPr)2 by means of FTIR and 13C NMR. The presence of this complex was confirmed with FTIR in the early stages of the process. A doublet in 1542 and 1440 cm-1 stands for the asymmetric and symmetric stretching vibrations of the carboxylic group coordinated to Ti as a bidentate ligand. The gap of 102 cm-1 between these signals suggests that acetate acts preferentially as a bidentate rather than as a bridging ligand between two titanium atoms. The use of acetic acid as modifier allows the control of both the degree of condensation and oligomerization of the precursor and leads to the preferential crystallization of TiO2 in the anatase phase. A possible reaction pathway toward the formation of anatase is proposed on the basis of the intermediate species present in a 1:1 Ti(OiPr)4:CH3COOH molar system in which esterification reactions that introduce H2O into the reaction mixture were seen to be negligible. The Rietveld refinement and TEM analysis revealed that the powder is composed of isotropic anatase nanocrystallites.Fil: Parra, Rodrigo. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Goes, M. S.. Universidade Estadual Paulista Julio de Mesquita Filho; BrasilFil: Castro, Miriam Susana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Longo, Elson. Universidade Estadual Paulista Julio de Mesquita Filho; BrasilFil: Bueno, Paulo Roberto. Universidade Estadual Paulista Julio de Mesquita Filho; BrasilFil: Varela, José Arana. Universidade Estadual Paulista Julio de Mesquita Filho; BrasilAmerican Chemical Society2008-01info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/69242Parra, Rodrigo; Goes, M. S.; Castro, Miriam Susana; Longo, Elson; Bueno, Paulo Roberto; et al.; Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid; American Chemical Society; Chemistry Of Materials; 20; 1; 1-2008; 143-1500897-4756CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/doi/10.1021/cm702286einfo:eu-repo/semantics/altIdentifier/url/https://pubs.acs.org/doi/abs/10.1021/cm702286einfo:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-29T10:03:38Zoai:ri.conicet.gov.ar:11336/69242instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-09-29 10:03:38.925CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
title Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
spellingShingle Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
Parra, Rodrigo
Anatase Synthesis
Sol-Gel Route
title_short Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
title_full Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
title_fullStr Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
title_full_unstemmed Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
title_sort Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid
dc.creator.none.fl_str_mv Parra, Rodrigo
Goes, M. S.
Castro, Miriam Susana
Longo, Elson
Bueno, Paulo Roberto
Varela, José Arana
author Parra, Rodrigo
author_facet Parra, Rodrigo
Goes, M. S.
Castro, Miriam Susana
Longo, Elson
Bueno, Paulo Roberto
Varela, José Arana
author_role author
author2 Goes, M. S.
Castro, Miriam Susana
Longo, Elson
Bueno, Paulo Roberto
Varela, José Arana
author2_role author
author
author
author
author
dc.subject.none.fl_str_mv Anatase Synthesis
Sol-Gel Route
topic Anatase Synthesis
Sol-Gel Route
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv Anatase nanoparticles were obtained through a modified sol-gel route from titanium isopropoxide modified with acetic acid in order to control hydrolysis and condensation reactions. The modification of Ti(OiPr)4 with acetic acid reduces the availability of groups that hydrolyze and condense easily through the formation of a stable complex whose structure was determined to be Ti(OCOCH3)(OlPr)2 by means of FTIR and 13C NMR. The presence of this complex was confirmed with FTIR in the early stages of the process. A doublet in 1542 and 1440 cm-1 stands for the asymmetric and symmetric stretching vibrations of the carboxylic group coordinated to Ti as a bidentate ligand. The gap of 102 cm-1 between these signals suggests that acetate acts preferentially as a bidentate rather than as a bridging ligand between two titanium atoms. The use of acetic acid as modifier allows the control of both the degree of condensation and oligomerization of the precursor and leads to the preferential crystallization of TiO2 in the anatase phase. A possible reaction pathway toward the formation of anatase is proposed on the basis of the intermediate species present in a 1:1 Ti(OiPr)4:CH3COOH molar system in which esterification reactions that introduce H2O into the reaction mixture were seen to be negligible. The Rietveld refinement and TEM analysis revealed that the powder is composed of isotropic anatase nanocrystallites.
Fil: Parra, Rodrigo. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Goes, M. S.. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Fil: Castro, Miriam Susana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Longo, Elson. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Fil: Bueno, Paulo Roberto. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
Fil: Varela, José Arana. Universidade Estadual Paulista Julio de Mesquita Filho; Brasil
description Anatase nanoparticles were obtained through a modified sol-gel route from titanium isopropoxide modified with acetic acid in order to control hydrolysis and condensation reactions. The modification of Ti(OiPr)4 with acetic acid reduces the availability of groups that hydrolyze and condense easily through the formation of a stable complex whose structure was determined to be Ti(OCOCH3)(OlPr)2 by means of FTIR and 13C NMR. The presence of this complex was confirmed with FTIR in the early stages of the process. A doublet in 1542 and 1440 cm-1 stands for the asymmetric and symmetric stretching vibrations of the carboxylic group coordinated to Ti as a bidentate ligand. The gap of 102 cm-1 between these signals suggests that acetate acts preferentially as a bidentate rather than as a bridging ligand between two titanium atoms. The use of acetic acid as modifier allows the control of both the degree of condensation and oligomerization of the precursor and leads to the preferential crystallization of TiO2 in the anatase phase. A possible reaction pathway toward the formation of anatase is proposed on the basis of the intermediate species present in a 1:1 Ti(OiPr)4:CH3COOH molar system in which esterification reactions that introduce H2O into the reaction mixture were seen to be negligible. The Rietveld refinement and TEM analysis revealed that the powder is composed of isotropic anatase nanocrystallites.
publishDate 2008
dc.date.none.fl_str_mv 2008-01
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/69242
Parra, Rodrigo; Goes, M. S.; Castro, Miriam Susana; Longo, Elson; Bueno, Paulo Roberto; et al.; Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid; American Chemical Society; Chemistry Of Materials; 20; 1; 1-2008; 143-150
0897-4756
CONICET Digital
CONICET
url http://hdl.handle.net/11336/69242
identifier_str_mv Parra, Rodrigo; Goes, M. S.; Castro, Miriam Susana; Longo, Elson; Bueno, Paulo Roberto; et al.; Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid; American Chemical Society; Chemistry Of Materials; 20; 1; 1-2008; 143-150
0897-4756
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/doi/10.1021/cm702286e
info:eu-repo/semantics/altIdentifier/url/https://pubs.acs.org/doi/abs/10.1021/cm702286e
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
application/pdf
dc.publisher.none.fl_str_mv American Chemical Society
publisher.none.fl_str_mv American Chemical Society
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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score 13.070432

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