Síntese de nanocristais coloidais de TiO2 via método solvotermal

Detalhes bibliográficos
Autor(a) principal: Mambrini, Giovanni Pimenta
Data de Publicação: 2008
Tipo de documento: Tese
Idioma: por
Título da fonte: Repositório Institucional da UFSCAR
Texto Completo: https://repositorio.ufscar.br/handle/ufscar/6132
Resumo: This work presents a systematic study about preparing titanium oxide nanoparticles by solvothermal method. TiO2 is a much studied material because its applications in areas like catalysis, sensors, energy conversion devices, and others. It is speculated that all this technologies can be promoted by using nanostructured oxide. In order to confirm this, it is necessary to develop synthetic routes that allow preparing the desired material with controlled size and shapes. The methodology utilized in this research work consists in dissolve titanium isopropoxide in a phenyl ether and oleic acid mixture. After the complete dissolution, a hydrogen peroxide aqueous solution is fast injected in the medium. Then, the resulting suspension is heated at 120oC and maintained by time intervals between 12 and 192 hours. It was analyzed the influence of Lewis bases addition at the reaction medium, using chloride, nitrate and sulfate in these experiments. The influence of different surfactants on the oxide properties was analized too. The powders were characterized by X-ray diffraction, Raman spectroscopy, infrared spectroscopy and scanning-transmission electron microscopy. It was verified that the addition of a Lewis bases is a key rule to obtain crystalline TiO2 by the proposed route. This could be observed by the addition of simple bases as well as by addition of basic surfactants. The synthesis methodology developed in this work allows the synthesis of nanostructured materials with narrow size distribution, with diameters between 7 and 4 nm and standard deviation of about 1 nm. It was observed that the materials have a hydrophobic character; this was attributed to the presence of surfactants bounded to the particles surface. Infrared spectroscopy allowed that confirmation. In summary, it was developed a synthetic methodology of TiO2 colloidal nanocrystals that allows a good control of the final material characteristics.
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spelling Mambrini, Giovanni PimentaLeite, Edson Robertohttp://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4783657E4http://lattes.cnpq.br/7723027354150918673d3195-633e-41fe-afbc-cf72d79b78412016-06-02T20:34:14Z2009-10-272016-06-02T20:34:14Z2008-08-07MAMBRINI, Giovanni Pimenta. Synthesis of TIO2 colloidal nanocrystals by solvothermal method. 2008. 108 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.https://repositorio.ufscar.br/handle/ufscar/6132This work presents a systematic study about preparing titanium oxide nanoparticles by solvothermal method. TiO2 is a much studied material because its applications in areas like catalysis, sensors, energy conversion devices, and others. It is speculated that all this technologies can be promoted by using nanostructured oxide. In order to confirm this, it is necessary to develop synthetic routes that allow preparing the desired material with controlled size and shapes. The methodology utilized in this research work consists in dissolve titanium isopropoxide in a phenyl ether and oleic acid mixture. After the complete dissolution, a hydrogen peroxide aqueous solution is fast injected in the medium. Then, the resulting suspension is heated at 120oC and maintained by time intervals between 12 and 192 hours. It was analyzed the influence of Lewis bases addition at the reaction medium, using chloride, nitrate and sulfate in these experiments. The influence of different surfactants on the oxide properties was analized too. The powders were characterized by X-ray diffraction, Raman spectroscopy, infrared spectroscopy and scanning-transmission electron microscopy. It was verified that the addition of a Lewis bases is a key rule to obtain crystalline TiO2 by the proposed route. This could be observed by the addition of simple bases as well as by addition of basic surfactants. The synthesis methodology developed in this work allows the synthesis of nanostructured materials with narrow size distribution, with diameters between 7 and 4 nm and standard deviation of about 1 nm. It was observed that the materials have a hydrophobic character; this was attributed to the presence of surfactants bounded to the particles surface. Infrared spectroscopy allowed that confirmation. In summary, it was developed a synthetic methodology of TiO2 colloidal nanocrystals that allows a good control of the final material characteristics.Este trabalho apresenta um estudo sistemático acerca do preparo de nanopartículas de óxido de titânio via método solvotermal. O TiO2 é um material bastante estudado devido às suas aplicações em áreas como catálise, sensores, conversão de energia, dentre outras. Especula-se que todas estas tecnologias podem ser promovidas com a utilização do óxido nanoparticulado. Para confirmar isto, torna-se necessário o desenvolvimento de métodos de síntese que permitam preparar o material desejado com tamanho e forma de partículas controlados. O método utilizado neste trabalho consiste em dissolver isopropóxido de titânio em uma mistura de ácido oléico e difenil éter. Após a completa dissolução, é injetada rapidamente uma solução de peróxido de hidrogênio. Em seguida, a suspensão resultante passou por um tratamento solvotermal a 120oC por intervalos de tempo entre 12 e 192 horas. Foi analisada a influência da adição de bases de Lewis ao meio reacional, utilizando-se para isso cloreto, nitrato e sulfato. Analisou-se também a influência de diferentes surfactantes nas características do material obtido. Os pós foram caracterizados por difratometria de raios X, espectroscopia Raman, espectroscopia na região do infravermelho e microscopia eletrônica de transmissãovarredura. Verificou-se que a adição da base de Lewis ao meio reacional é fundamental para que ocorra a cristalização do TiO2 pela rota proposta. Isso pôde ser observado tanto pela adição de bases simples bem como com a adição de surfactantes com caráter básico. A rota sintética desenvolvida permitiu o preparo de materiais com tamanho controlado de partículas, entre 7 e 4 nm, em geral com desvio padrão de distribuição de tamanhos da ordem de 1 nm. Observou-se que os materiais sintetizados têm caráter hidrofóbico, atribuído à presença de surfactante ligado à superfície dos mesmos, o que foi observado por ensaios de espectroscopia. Assim, foi desenvolvido um método de síntese de nanocristais coloidais de TiO2 que permite um bom controle das características do material sintetizado.Universidade Federal de Minas Geraisapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRSíntese de nanopartículasFísico-QuímicaSíntese inorgânicaNanopartículasÓxidosCIENCIAS EXATAS E DA TERRA::QUIMICASíntese de nanocristais coloidais de TiO2 via método solvotermalSynthesis of TIO2 colloidal nanocrystals by solvothermal methodinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesis-1-19c25e6a7-a2cd-4058-97ed-441bc2793123info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL2076.pdfapplication/pdf4680709https://repositorio.ufscar.br/bitstream/ufscar/6132/1/2076.pdf9a7b1415428ae059e0e9b3df261cfd90MD51THUMBNAIL2076.pdf.jpg2076.pdf.jpgIM Thumbnailimage/jpeg8739https://repositorio.ufscar.br/bitstream/ufscar/6132/2/2076.pdf.jpg32ab95e5c6e10cb564c6dc41c4bfdee5MD52ufscar/61322023-09-18 18:31:09.924oai:repositorio.ufscar.br:ufscar/6132Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:31:09Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false
dc.title.por.fl_str_mv Síntese de nanocristais coloidais de TiO2 via método solvotermal
dc.title.alternative.eng.fl_str_mv Synthesis of TIO2 colloidal nanocrystals by solvothermal method
title Síntese de nanocristais coloidais de TiO2 via método solvotermal
spellingShingle Síntese de nanocristais coloidais de TiO2 via método solvotermal
Mambrini, Giovanni Pimenta
Síntese de nanopartículas
Físico-Química
Síntese inorgânica
Nanopartículas
Óxidos
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Síntese de nanocristais coloidais de TiO2 via método solvotermal
title_full Síntese de nanocristais coloidais de TiO2 via método solvotermal
title_fullStr Síntese de nanocristais coloidais de TiO2 via método solvotermal
title_full_unstemmed Síntese de nanocristais coloidais de TiO2 via método solvotermal
title_sort Síntese de nanocristais coloidais de TiO2 via método solvotermal
author Mambrini, Giovanni Pimenta
author_facet Mambrini, Giovanni Pimenta
author_role author
dc.contributor.authorlattes.por.fl_str_mv http://lattes.cnpq.br/7723027354150918
dc.contributor.author.fl_str_mv Mambrini, Giovanni Pimenta
dc.contributor.advisor1.fl_str_mv Leite, Edson Roberto
dc.contributor.advisor1Lattes.fl_str_mv http://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4783657E4
dc.contributor.authorID.fl_str_mv 673d3195-633e-41fe-afbc-cf72d79b7841
contributor_str_mv Leite, Edson Roberto
dc.subject.por.fl_str_mv Síntese de nanopartículas
Físico-Química
Síntese inorgânica
Nanopartículas
Óxidos
topic Síntese de nanopartículas
Físico-Química
Síntese inorgânica
Nanopartículas
Óxidos
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description This work presents a systematic study about preparing titanium oxide nanoparticles by solvothermal method. TiO2 is a much studied material because its applications in areas like catalysis, sensors, energy conversion devices, and others. It is speculated that all this technologies can be promoted by using nanostructured oxide. In order to confirm this, it is necessary to develop synthetic routes that allow preparing the desired material with controlled size and shapes. The methodology utilized in this research work consists in dissolve titanium isopropoxide in a phenyl ether and oleic acid mixture. After the complete dissolution, a hydrogen peroxide aqueous solution is fast injected in the medium. Then, the resulting suspension is heated at 120oC and maintained by time intervals between 12 and 192 hours. It was analyzed the influence of Lewis bases addition at the reaction medium, using chloride, nitrate and sulfate in these experiments. The influence of different surfactants on the oxide properties was analized too. The powders were characterized by X-ray diffraction, Raman spectroscopy, infrared spectroscopy and scanning-transmission electron microscopy. It was verified that the addition of a Lewis bases is a key rule to obtain crystalline TiO2 by the proposed route. This could be observed by the addition of simple bases as well as by addition of basic surfactants. The synthesis methodology developed in this work allows the synthesis of nanostructured materials with narrow size distribution, with diameters between 7 and 4 nm and standard deviation of about 1 nm. It was observed that the materials have a hydrophobic character; this was attributed to the presence of surfactants bounded to the particles surface. Infrared spectroscopy allowed that confirmation. In summary, it was developed a synthetic methodology of TiO2 colloidal nanocrystals that allows a good control of the final material characteristics.
publishDate 2008
dc.date.issued.fl_str_mv 2008-08-07
dc.date.available.fl_str_mv 2009-10-27
2016-06-02T20:34:14Z
dc.date.accessioned.fl_str_mv 2016-06-02T20:34:14Z
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dc.identifier.citation.fl_str_mv MAMBRINI, Giovanni Pimenta. Synthesis of TIO2 colloidal nanocrystals by solvothermal method. 2008. 108 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.
dc.identifier.uri.fl_str_mv https://repositorio.ufscar.br/handle/ufscar/6132
identifier_str_mv MAMBRINI, Giovanni Pimenta. Synthesis of TIO2 colloidal nanocrystals by solvothermal method. 2008. 108 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.
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