Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)

Detalhes bibliográficos
Ano de defesa: 2008
Autor(a) principal: Souza, Nicolau Silva de
Orientador(a): Moreira, Fernando Manuel Araújo lattes
Banca de defesa: Não Informado pela instituição
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de São Carlos
Programa de Pós-Graduação: Programa de Pós-Graduação em Física - PPGF
Departamento: Não Informado pela instituição
País: BR
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: https://repositorio.ufscar.br/handle/20.500.14289/5011
Resumo: In this work were studied the physical properties of magnetic nanoparticles, based on iron oxide, and magnetic graphite fluid particles. The work was developed in three steps: 1) synthesis of the magnetic nanoparticles of iron oxides by the sol-gel and co-precipitation methods, 2) synthesis of the magnetic graphite fluid particles, 3) structural, microstructural and magnetic characterization of the samples. The morphological properties of the iron oxide nanoparticles, by the MEV-FEG images, showed that the samples obtained by sol-gel technique have a large tendency to create powder agglomerates. By the way, the samples obtained by coprecipitation showed a mean powder diameter 11nm, calculated from the micrographs images. Although, the same value , obtained from the XRD pattern, and diffraction peaks intensity are ~1.5 nm. From the magnetization curves, zero field cooling (ZFC), field cooling (FC), it was possible to see a phase transition for the locked-state at T ( )K B ≈ 39 ±1 for the sample obtained by sol-gel, and at T ( )K B ≈ 179 ±1 for the sample obtained by co-precipitations. The magnetization values as a function of the applied field showed a superparamagnetic behavior, ensured by the electronic paramagnetic resonance (EPR). The morphological characterization of the magnetic fluid graphite, by the TEM images, also showed an agglomerate state, but it was possible to estimate a mean diameter ~10nm. This unpublished value is much smaller than the observed on the literature. The structural characterization of the magnetic fluid graphite, obtained by infrared spectroscopy, showed that the surfactant particles (CTAB) still present on the magnetic fluid graphite surface. The surfactant particles are the responsible for the solution stability; From the magnetization measurements, as a function of the field, the graphite particles showed a typical ferromagnetic behavior. The (ZFC) magnetization measurements showed that the graphite particles have a non-null magnetization at room temperature, and the aqueous suspension doesn`t have influence on the magnetization behavior. The obtained results according to the synthesis way agree with the results showed in the literature. For the iron oxide nanoparticles it has been observed the superparamagnetic behavior in all the samples. The structural properties are ruled according to the synthesis process. On the other hand, for the magnetic graphite fluid particles, the magnetization process was made by the oxi-reduction method controlled on the vapor phase, with controlled atmosphere. After the magnetization process, was obtained by the first time the synthesis of the magnetic graphite fluid, initially on water suspension, with the magnetization properties unchanged.
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spelling Souza, Nicolau Silva deMoreira, Fernando Manuel Araújohttp://lattes.cnpq.br/1809254923092721http://lattes.cnpq.br/63010846638792707ed37bc6-7d06-43f0-b0f9-29aa3625d3562016-06-02T20:16:44Z2009-09-172016-06-02T20:16:44Z2008-09-05SOUZA, Nicolau Silva de. Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF). 2008. 100 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.https://repositorio.ufscar.br/handle/20.500.14289/5011In this work were studied the physical properties of magnetic nanoparticles, based on iron oxide, and magnetic graphite fluid particles. The work was developed in three steps: 1) synthesis of the magnetic nanoparticles of iron oxides by the sol-gel and co-precipitation methods, 2) synthesis of the magnetic graphite fluid particles, 3) structural, microstructural and magnetic characterization of the samples. The morphological properties of the iron oxide nanoparticles, by the MEV-FEG images, showed that the samples obtained by sol-gel technique have a large tendency to create powder agglomerates. By the way, the samples obtained by coprecipitation showed a mean powder diameter 11nm, calculated from the micrographs images. Although, the same value , obtained from the XRD pattern, and diffraction peaks intensity are ~1.5 nm. From the magnetization curves, zero field cooling (ZFC), field cooling (FC), it was possible to see a phase transition for the locked-state at T ( )K B ≈ 39 ±1 for the sample obtained by sol-gel, and at T ( )K B ≈ 179 ±1 for the sample obtained by co-precipitations. The magnetization values as a function of the applied field showed a superparamagnetic behavior, ensured by the electronic paramagnetic resonance (EPR). The morphological characterization of the magnetic fluid graphite, by the TEM images, also showed an agglomerate state, but it was possible to estimate a mean diameter ~10nm. This unpublished value is much smaller than the observed on the literature. The structural characterization of the magnetic fluid graphite, obtained by infrared spectroscopy, showed that the surfactant particles (CTAB) still present on the magnetic fluid graphite surface. The surfactant particles are the responsible for the solution stability; From the magnetization measurements, as a function of the field, the graphite particles showed a typical ferromagnetic behavior. The (ZFC) magnetization measurements showed that the graphite particles have a non-null magnetization at room temperature, and the aqueous suspension doesn`t have influence on the magnetization behavior. The obtained results according to the synthesis way agree with the results showed in the literature. For the iron oxide nanoparticles it has been observed the superparamagnetic behavior in all the samples. The structural properties are ruled according to the synthesis process. On the other hand, for the magnetic graphite fluid particles, the magnetization process was made by the oxi-reduction method controlled on the vapor phase, with controlled atmosphere. After the magnetization process, was obtained by the first time the synthesis of the magnetic graphite fluid, initially on water suspension, with the magnetization properties unchanged.Tendo como motivação a aplicabilidade das nanopartículas magnéticas o presente trabalho tem como objetivos principais estudar as características físicoquímicas das nanopartículas magnéticas, a base de óxido de ferro, e partículas de grafite magnético fluido. O desenvolvimento do trabalho se deu em três etapas: 1) síntese das nanopartículas magnéticas a base de óxido de ferro pelos métodos de sol-gel e co-precipitação; 2) síntese das partículas de grafite magnética fluida; 3) caracterização estrutural, microestrutural e magnética das amostras obtidas. A caracterização morfológica das nanoparticulas de óxido de ferro, usando a técnica de MEV-FEG, mostrou que amostras obtidas via sol-gel apresentam maior aglomeração dos pós, impossibilitando que uma analise qualitativa de seu tamanho fosse realizada. Já as amostras obtidas pelo método da co-precipitação encontrouse, por análise qualitativa, uma estimativa da distribuição média do diâmetro em torno de 11nm, cujo valor, calculado através da técnica de DRX, está na ordem de 7,5nm. Mediante as curvas de magnetização, esfriamento com campo zero (ZFC) e esfriamento com campo aplicado (FC) foi observada uma transição para o estado de bloqueio para as amostras sintetizadas por sol-gel ( T )K B ≈ 39 ±1 e para coprecipitção T ( )K B ≈ 179 ±1 . Medidas de magnetização em função do campo mostraram que os materiais têm comportamento superparamagnético, confirmado por meio de ressonsncia paramagnética eletrônica (RPE). A caracterização morfológica das partículas de grafite magnética fluida, usando a técnica de TEM, revelaram que as partículas estão aglomeradas, sendo possível estimar que as partículas apresentam diâmetro médio em torno de 10 nm. Este valor obtido surpreende, já que não existe na literatura atual nenhum trabalho que mostre um tamanho tão reduzido para partículas de grafite. A caracterização estrutural da grafite magnética fluido foi realizada através da técnica de espectroscopia na região do infravermelho, onde foi observado a presença de moléculas do surfactante (CTAB) na superfície da grafite magnético fluido. Acreditase que tal mudança proporciona a sua estabilidade em solução aquosa; Mediante medidas de magnetização em função do campo realizado, observou-se um comportamento ferromagnético típico. Já as medidas de magnetização à ZFC das amostras, permitem concluir que, após o tratamento químico, a grafite apresenta uma magnetização a temperatura ambiente, e que a suspensão, não prejudicou em nada a sua magnetização. As análises dos resultados e a escolha do método de síntese foram essenciais para validar os resultados obtidos junto à literatura existente. No caso das nanopartículas de óxido de ferro pode-se observar o comportamento superparamagnético em todas as amostras. No entando, as caracteristicas estruturais apresentaram uma dependência referente ao método de síntese empregado. Já no caso das partículas de grafite magnético, o processo de magnetização foi realizado através de reação de oxidação-redução controlada em fase de vapor, com rigoroso controle de atmosfera. Depois de magnetizado, foi realizado o processo inédito de síntese do grafite magnético fluido, inicialmente em uma suspensão aquosa, de modo que a magnetização obtida não se foi prejudicada.Financiadora de Estudos e Projetosapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Física - PPGFUFSCarBRNanopartículasGrafiteMagnetitaFluídos complexosSol-GelCIENCIAS EXATAS E DA TERRA::FISICASíntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesis041b8a99-2c17-4a25-9ccb-49458db891fcinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARTEXT2224.pdf.txt2224.pdf.txtExtracted texttext/plain103291https://repositorio.ufscar.br/bitstreams/59b2853b-bc50-4b69-8572-950df641ab5e/download2365fc74539a2ad4f637a9459fedae7fMD53falseAnonymousREADORIGINAL2224.pdfapplication/pdf2663151https://repositorio.ufscar.br/bitstreams/a8c7a389-d987-47f5-8924-ddcd6ee44280/downloadb8216bb3c62b2148a34c038a44ed490dMD51trueAnonymousREADTHUMBNAIL2224.pdf.jpg2224.pdf.jpgIM Thumbnailimage/jpeg6635https://repositorio.ufscar.br/bitstreams/ba47ff6f-ba24-4b04-b3ed-feb67dfb9030/download42183f47cbac00519d67415305bf33eeMD52falseAnonymousREAD20.500.14289/50112025-02-06 05:11:36.462open.accessoai:repositorio.ufscar.br:20.500.14289/5011https://repositorio.ufscar.brRepositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestrepositorio.sibi@ufscar.bropendoar:43222025-02-06T08:11:36Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false
dc.title.por.fl_str_mv Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
title Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
spellingShingle Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
Souza, Nicolau Silva de
Nanopartículas
Grafite
Magnetita
Fluídos complexos
Sol-Gel
CIENCIAS EXATAS E DA TERRA::FISICA
title_short Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
title_full Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
title_fullStr Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
title_full_unstemmed Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
title_sort Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF)
author Souza, Nicolau Silva de
author_facet Souza, Nicolau Silva de
author_role author
dc.contributor.authorlattes.por.fl_str_mv http://lattes.cnpq.br/6301084663879270
dc.contributor.author.fl_str_mv Souza, Nicolau Silva de
dc.contributor.advisor1.fl_str_mv Moreira, Fernando Manuel Araújo
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/1809254923092721
dc.contributor.authorID.fl_str_mv 7ed37bc6-7d06-43f0-b0f9-29aa3625d356
contributor_str_mv Moreira, Fernando Manuel Araújo
dc.subject.por.fl_str_mv Nanopartículas
Grafite
Magnetita
Fluídos complexos
Sol-Gel
topic Nanopartículas
Grafite
Magnetita
Fluídos complexos
Sol-Gel
CIENCIAS EXATAS E DA TERRA::FISICA
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::FISICA
description In this work were studied the physical properties of magnetic nanoparticles, based on iron oxide, and magnetic graphite fluid particles. The work was developed in three steps: 1) synthesis of the magnetic nanoparticles of iron oxides by the sol-gel and co-precipitation methods, 2) synthesis of the magnetic graphite fluid particles, 3) structural, microstructural and magnetic characterization of the samples. The morphological properties of the iron oxide nanoparticles, by the MEV-FEG images, showed that the samples obtained by sol-gel technique have a large tendency to create powder agglomerates. By the way, the samples obtained by coprecipitation showed a mean powder diameter 11nm, calculated from the micrographs images. Although, the same value , obtained from the XRD pattern, and diffraction peaks intensity are ~1.5 nm. From the magnetization curves, zero field cooling (ZFC), field cooling (FC), it was possible to see a phase transition for the locked-state at T ( )K B ≈ 39 ±1 for the sample obtained by sol-gel, and at T ( )K B ≈ 179 ±1 for the sample obtained by co-precipitations. The magnetization values as a function of the applied field showed a superparamagnetic behavior, ensured by the electronic paramagnetic resonance (EPR). The morphological characterization of the magnetic fluid graphite, by the TEM images, also showed an agglomerate state, but it was possible to estimate a mean diameter ~10nm. This unpublished value is much smaller than the observed on the literature. The structural characterization of the magnetic fluid graphite, obtained by infrared spectroscopy, showed that the surfactant particles (CTAB) still present on the magnetic fluid graphite surface. The surfactant particles are the responsible for the solution stability; From the magnetization measurements, as a function of the field, the graphite particles showed a typical ferromagnetic behavior. The (ZFC) magnetization measurements showed that the graphite particles have a non-null magnetization at room temperature, and the aqueous suspension doesn`t have influence on the magnetization behavior. The obtained results according to the synthesis way agree with the results showed in the literature. For the iron oxide nanoparticles it has been observed the superparamagnetic behavior in all the samples. The structural properties are ruled according to the synthesis process. On the other hand, for the magnetic graphite fluid particles, the magnetization process was made by the oxi-reduction method controlled on the vapor phase, with controlled atmosphere. After the magnetization process, was obtained by the first time the synthesis of the magnetic graphite fluid, initially on water suspension, with the magnetization properties unchanged.
publishDate 2008
dc.date.issued.fl_str_mv 2008-09-05
dc.date.available.fl_str_mv 2009-09-17
2016-06-02T20:16:44Z
dc.date.accessioned.fl_str_mv 2016-06-02T20:16:44Z
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dc.identifier.citation.fl_str_mv SOUZA, Nicolau Silva de. Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF). 2008. 100 f. Dissertação (Mestrado 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/20.500.14289/5011
identifier_str_mv SOUZA, Nicolau Silva de. Síntese e caracterização de nanopartículas de óxido de ferro e de grafite magnética fluida (GMF). 2008. 100 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.
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