Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas

Detalhes bibliográficos
Ano de defesa: 2018
Autor(a) principal: Storion, Ana Gabriela lattes
Orientador(a): Maestrelli, Sylma Carvalho lattes
Banca de defesa: Marques, Rodrigo Fernando Costa, Morales, Sergio Andres Villalba
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Alfenas
Programa de Pós-Graduação: Programa de Pós-Graduação em Ciência e Engenharia de Materiais
Departamento: Instituto de Ciência e Tecnologia
País: Brasil
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: https://repositorio.unifal-mg.edu.br/handle/123456789/1207
Resumo: Advanced Oxidation Processes (AOP) are widely studied as alternative water treatments. Heterogeneous photocatalysis (a method of POA) consists in the activation of a semiconductor by radiation, generating oxidizing and reducing sites, which will mineralize the pollutants. The surface area of ​​a photocatalyst is a very important property, since the processes will activate and occur on its surface, which makes it necessary to obtain powders on a nanometric scale. The present work aimed to study the application of High Energy Ball Milling performed in a SPEX 8000 Mixer/Mill, with ball to powder weight ratio of 5:1, to obtain nanostructured powders of TiO2:WO3 and ZnO, under different compositions and milling times. The photocatalytic activity was evaluated through decomposition of Rhodamine B (RhB). The powders were characterized by B.E.T., Helium pycnometry, X ray diffraction, DSC/TG and FTIR and submitted to the milling process. For the TiO2:WO3 system, different bulk compositions were considered (0:100, 30:70, 50:50, 70:30 and 100: 0), each one milled for 2, 4, 6 and 8 hours. For ZnO, milling times of 1, 2, 3, 4 and 5 hours were carried out. After grinding, acid leaching was performed to remove the iron from the grinding medium, using 6.5 M ​​hydrochloric acid and 0.5 M oxalic acid. The powders were deagglomerated and characterized by X-ray diffraction, scanning electron microscopy and X-ray fluorescence. Finally, the photocatalytic tests were carried out in a photochemical reactor with incidence of ultraviolet radiation. The results showed that High Energy Milling using SPEX 8000 mill presents potential of obtaining powders in nanometric scale. For zinc oxide, 1 hour of milling was enough to achieve nanometric scales, as well as 2 hours of milling for the TiO2:WO3 system. Through chemical analysis, it was observed that the leaching performed was not efficient in the iron removal. For the TiO2:WO3 system, both leaching decreased the iron percentage, but the hydrochloric acid led to the formation of larger agglomerates and particles of differentiated morphology. For ZnO, the use of oxalic acid led to the formation of zinc oxalate which, in turn, provided particle growth to micrometric scale. The processed materials via MAE presented lower photocatalytic activity for the degradation of RhB using UV radiation. This behavior may be related to the structural transformations occurred during processing, iron incorporation in the materials structure, appearance of crystalline imperfections and an elevation in the recombination rate of the photogenerated pairs.
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spelling Storion, Ana Gabrielahttp://lattes.cnpq.br/0216431851054031Giraldi, Tania Reginahttp://lattes.cnpq.br/0847092755379350Marques, Rodrigo Fernando CostaMorales, Sergio Andres VillalbaMaestrelli, Sylma Carvalhohttp://lattes.cnpq.br/35207465304578902018-08-10T20:34:21Z2018-01-16STORION, Ana Gabriela. Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas. 2018. 133 f. Dissertação (Mestrado em Ciência e Engenharia de Materiais) - Universidade Federal de Alfenas, Poços de Caldas, 2018.https://repositorio.unifal-mg.edu.br/handle/123456789/1207Advanced Oxidation Processes (AOP) are widely studied as alternative water treatments. Heterogeneous photocatalysis (a method of POA) consists in the activation of a semiconductor by radiation, generating oxidizing and reducing sites, which will mineralize the pollutants. The surface area of ​​a photocatalyst is a very important property, since the processes will activate and occur on its surface, which makes it necessary to obtain powders on a nanometric scale. The present work aimed to study the application of High Energy Ball Milling performed in a SPEX 8000 Mixer/Mill, with ball to powder weight ratio of 5:1, to obtain nanostructured powders of TiO2:WO3 and ZnO, under different compositions and milling times. The photocatalytic activity was evaluated through decomposition of Rhodamine B (RhB). The powders were characterized by B.E.T., Helium pycnometry, X ray diffraction, DSC/TG and FTIR and submitted to the milling process. For the TiO2:WO3 system, different bulk compositions were considered (0:100, 30:70, 50:50, 70:30 and 100: 0), each one milled for 2, 4, 6 and 8 hours. For ZnO, milling times of 1, 2, 3, 4 and 5 hours were carried out. After grinding, acid leaching was performed to remove the iron from the grinding medium, using 6.5 M ​​hydrochloric acid and 0.5 M oxalic acid. The powders were deagglomerated and characterized by X-ray diffraction, scanning electron microscopy and X-ray fluorescence. Finally, the photocatalytic tests were carried out in a photochemical reactor with incidence of ultraviolet radiation. The results showed that High Energy Milling using SPEX 8000 mill presents potential of obtaining powders in nanometric scale. For zinc oxide, 1 hour of milling was enough to achieve nanometric scales, as well as 2 hours of milling for the TiO2:WO3 system. Through chemical analysis, it was observed that the leaching performed was not efficient in the iron removal. For the TiO2:WO3 system, both leaching decreased the iron percentage, but the hydrochloric acid led to the formation of larger agglomerates and particles of differentiated morphology. For ZnO, the use of oxalic acid led to the formation of zinc oxalate which, in turn, provided particle growth to micrometric scale. The processed materials via MAE presented lower photocatalytic activity for the degradation of RhB using UV radiation. This behavior may be related to the structural transformations occurred during processing, iron incorporation in the materials structure, appearance of crystalline imperfections and an elevation in the recombination rate of the photogenerated pairs.Processos Oxidativos Avançados (POA) são amplamente estudados como alternativas para tratamento de águas. A fotocatálise heterogênea (um tipo de POA) consiste na ativação por radiação de um semicondutor, gerando sítios oxidantes e redutores que irão atuar na mineralização dos poluentes. A área superficial de um fotocatalisador é de extrema importância, pois os processos irão se ativar e ocorrer na superfície do mesmo, tornando necessária a obtenção de pós em escala nanométrica. O presente trabalho estudou a aplicação da Moagem de Alta Energia (MAE), utilizando o moinho SPEX 8000 Mixer/Mill na obtenção de óxidos (na forma de pós nanométricos) para aplicação fotocatalítica. Foi utilizada a proporção bola:material de 5:1 e diferentes parâmetros de processamento para a obtenção de pós nanoestruturados de TiO2:WO3 e ZnO. A atividade fotocatalítica foi avaliada por meio da decomposição da Rodamina B (RhB). Os pós foram caracterizados via B.E.T. picnometria a Hélio, difração de raios X, DSC/TG e FTIR e submetidos ao processo de moagem. Para o sistema TiO2:WO3, foram avaliadas as composições em massa de 0:100, 30:70, 50:50, 70:30 e 100:0 e os tempos de moagem de 2, 4, 6 e 8 horas; para o ZnO foi realizada a moagem durante 1, 2, 3, 4 e 5 horas do óxido puro. Após a moagem foi realizada lixívia ácida para a descontaminação do ferro provindo da MAE, utilizando-se Ácido Clorídrico 6,5 M ou Ácido Oxálico 0,5 M. Os pós processados foram então desaglomerados e caracterizados via difração de raios X, microscopia eletrônica de varredura e fluorescência de raios X (FRX). Ensaios fotocatalíticos foram realizados em um reator fotoquímico com incidência de radiação ultravioleta. Os resultados mostraram que a MAE utilizando moinho SPEX 8000 apresenta potencial na obtenção de pós em escala nanométrica, de modo que com 1 hora de moagem para o ZnO tais dimensões já foram alcançadas, bem como em 2 horas para o sistema TiO2:WO3. As análises químicas demonstraram que para o sistema TiO2:WO3 ambas as lixívias diminuíram o percentual de ferro, mas a lixívia realizada em ácido clorídrico levou à formação de maiores aglomerados e de partículas de morfologia diferenciada. Para o ZnO, a utilização do ácido oxálico levou a formação do oxalato de zinco que, por sua vez, proporcionou o crescimento das partículas para escala micrométrica. Os óxidos processados mediante a MAE apresentaram menor atividade fotocatalítica para a degradação da RhB utilizando radiação UV. Este comportamento pode estar ligado às transformações estruturais ocorridas durante o processamento, incorporação do Fe na estrutura dos materiais, surgimento de imperfeições cristalinas e elevação na taxa de recombinação dos pares fotogerados.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESapplication/pdfporUniversidade Federal de AlfenasPrograma de Pós-Graduação em Ciência e Engenharia de MateriaisUNIFAL-MGBrasilInstituto de Ciência e Tecnologiainfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/Fotocatálise.Moagem de alta energia.Óxido de Titânio.Óxido de Tungstênio.Óxido de Zinco.ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICANanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticasTiO2:WO3 and ZnO nanoparticles obtained by the use of a shaker mil: characterization and photocatalytic propertiesinfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/publishedVersion-4297417259498638931600600600-65375185333761334302075167498588264571reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifalinstname:Universidade Federal de Alfenas (UNIFAL)instacron:UNIFALStorion, Ana GabrielaLICENSElicense.txtlicense.txttext/plain; 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dc.title.pt-BR.fl_str_mv Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
dc.title.alternative.eng.fl_str_mv TiO2:WO3 and ZnO nanoparticles obtained by the use of a shaker mil: characterization and photocatalytic properties
title Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
spellingShingle Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
Storion, Ana Gabriela
Fotocatálise.
Moagem de alta energia.
Óxido de Titânio.
Óxido de Tungstênio.
Óxido de Zinco.
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
title_short Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
title_full Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
title_fullStr Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
title_full_unstemmed Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
title_sort Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas
author Storion, Ana Gabriela
author_facet Storion, Ana Gabriela
author_role author
dc.contributor.author.fl_str_mv Storion, Ana Gabriela
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/0216431851054031
dc.contributor.advisor-co1.fl_str_mv Giraldi, Tania Regina
dc.contributor.advisor-co1Lattes.fl_str_mv http://lattes.cnpq.br/0847092755379350
dc.contributor.referee1.fl_str_mv Marques, Rodrigo Fernando Costa
dc.contributor.referee2.fl_str_mv Morales, Sergio Andres Villalba
dc.contributor.advisor1.fl_str_mv Maestrelli, Sylma Carvalho
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/3520746530457890
contributor_str_mv Giraldi, Tania Regina
Marques, Rodrigo Fernando Costa
Morales, Sergio Andres Villalba
Maestrelli, Sylma Carvalho
dc.subject.por.fl_str_mv Fotocatálise.
Moagem de alta energia.
Óxido de Titânio.
Óxido de Tungstênio.
Óxido de Zinco.
topic Fotocatálise.
Moagem de alta energia.
Óxido de Titânio.
Óxido de Tungstênio.
Óxido de Zinco.
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
dc.subject.cnpq.fl_str_mv ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
description Advanced Oxidation Processes (AOP) are widely studied as alternative water treatments. Heterogeneous photocatalysis (a method of POA) consists in the activation of a semiconductor by radiation, generating oxidizing and reducing sites, which will mineralize the pollutants. The surface area of ​​a photocatalyst is a very important property, since the processes will activate and occur on its surface, which makes it necessary to obtain powders on a nanometric scale. The present work aimed to study the application of High Energy Ball Milling performed in a SPEX 8000 Mixer/Mill, with ball to powder weight ratio of 5:1, to obtain nanostructured powders of TiO2:WO3 and ZnO, under different compositions and milling times. The photocatalytic activity was evaluated through decomposition of Rhodamine B (RhB). The powders were characterized by B.E.T., Helium pycnometry, X ray diffraction, DSC/TG and FTIR and submitted to the milling process. For the TiO2:WO3 system, different bulk compositions were considered (0:100, 30:70, 50:50, 70:30 and 100: 0), each one milled for 2, 4, 6 and 8 hours. For ZnO, milling times of 1, 2, 3, 4 and 5 hours were carried out. After grinding, acid leaching was performed to remove the iron from the grinding medium, using 6.5 M ​​hydrochloric acid and 0.5 M oxalic acid. The powders were deagglomerated and characterized by X-ray diffraction, scanning electron microscopy and X-ray fluorescence. Finally, the photocatalytic tests were carried out in a photochemical reactor with incidence of ultraviolet radiation. The results showed that High Energy Milling using SPEX 8000 mill presents potential of obtaining powders in nanometric scale. For zinc oxide, 1 hour of milling was enough to achieve nanometric scales, as well as 2 hours of milling for the TiO2:WO3 system. Through chemical analysis, it was observed that the leaching performed was not efficient in the iron removal. For the TiO2:WO3 system, both leaching decreased the iron percentage, but the hydrochloric acid led to the formation of larger agglomerates and particles of differentiated morphology. For ZnO, the use of oxalic acid led to the formation of zinc oxalate which, in turn, provided particle growth to micrometric scale. The processed materials via MAE presented lower photocatalytic activity for the degradation of RhB using UV radiation. This behavior may be related to the structural transformations occurred during processing, iron incorporation in the materials structure, appearance of crystalline imperfections and an elevation in the recombination rate of the photogenerated pairs.
publishDate 2018
dc.date.accessioned.fl_str_mv 2018-08-10T20:34:21Z
dc.date.issued.fl_str_mv 2018-01-16
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
format masterThesis
status_str publishedVersion
dc.identifier.citation.fl_str_mv STORION, Ana Gabriela. Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas. 2018. 133 f. Dissertação (Mestrado em Ciência e Engenharia de Materiais) - Universidade Federal de Alfenas, Poços de Caldas, 2018.
dc.identifier.uri.fl_str_mv https://repositorio.unifal-mg.edu.br/handle/123456789/1207
identifier_str_mv STORION, Ana Gabriela. Nanopartículas de TiO2:WO3 e ZnO obtidas pela utilização de moinho vibratório: caracterização e propriedades fotocatalíticas. 2018. 133 f. Dissertação (Mestrado em Ciência e Engenharia de Materiais) - Universidade Federal de Alfenas, Poços de Caldas, 2018.
url https://repositorio.unifal-mg.edu.br/handle/123456789/1207
dc.language.iso.fl_str_mv por
language por
dc.relation.department.fl_str_mv -4297417259498638931
dc.relation.confidence.fl_str_mv 600
600
600
dc.relation.cnpq.fl_str_mv -6537518533376133430
dc.relation.sponsorship.fl_str_mv 2075167498588264571
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
rights_invalid_str_mv http://creativecommons.org/licenses/by-nc-nd/4.0/
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Alfenas
dc.publisher.program.fl_str_mv Programa de Pós-Graduação em Ciência e Engenharia de Materiais
dc.publisher.initials.fl_str_mv UNIFAL-MG
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Instituto de Ciência e Tecnologia
publisher.none.fl_str_mv Universidade Federal de Alfenas
dc.source.none.fl_str_mv reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifal
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