Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico
Autor(a) principal: | |
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Data de Publicação: | 2013 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFRN |
Texto Completo: | https://repositorio.ufrn.br/jspui/handle/123456789/15848 |
Resumo: | In this work it was synthesized and characterized the cobalt ferrite (CoFe2O4) by two methods: complexation combining EDTA/Citrate and hydrothermal investigating the influence of the synthesis conditions on phase formation and on the crystallite size. The powders were mainly characterized by x-ray diffraction. In specific cases, it was also used scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray fluorescence (XRF) and isotherms of adsorption and desorption of nitrogen (BET method). The study of the crystallite size was based on the interpretation of x-ray diffractograms obtained and estimated by the method of Halder-Wagner-Scherrer and Langford. An experimental design was made in order to assist in quantifying the influence of synthesis conditions on the response variables. The synthesis parameters evaluated in this study were: pH of the reaction medium (8, 9 and 10), the calcination temperature (combined complexation method EDTA/Citrate 600°C, 800°C and 1000°C), synthesis temperature (hydrothermal method 120°C, 140°C and 160°C), calcination time (combined complexation method EDTA/Citrate - 2, 4 and 6 hours) and time of synthesis (hydrothermal method 6, 15 and 24 hours). By the hydrothermal method was possible to produce mesoporous powders with high purity, with an average crystallite size up to 7 nm, with a surface area of 113.44 m²/g in the form of pellets with irregular morphology. By using the method of combined complexation EDTA/Citrate, mesoporous powders were produced with greater purity, crystallite size up to 22nm and 27.95 m²/g of surface area in the form of pellets with a regular morphology of plaques. In the experimental design was found that the hydrothermal method to all the studied parameters (pH, temperature and time) have significant effect on the crystallite size, while to the combined complexation method EDTA/Citrate, only temperature and time were significant |
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Medeiros, Indira Aritana Fernandes dehttp://lattes.cnpq.br/0540859141209826http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781094H3Santos, Andarair Gomes doshttp://lattes.cnpq.br/3470634368296605Silva, Gilson Garcia dahttp://lattes.cnpq.br/8681275097040450Souza, Carlson Pereira de2014-12-17T15:01:34Z2014-06-202014-12-17T15:01:34Z2013-12-17MEDEIROS, Indira Aritana Fernandes de. Obtaining cobalt ferrite through two synthesis methods: Complexation Method Conbining EDTA/Citrate and Hydrothermal Method. 2013. 139 f. Dissertação (Mestrado em Pesquisa e Desenvolvimento de Tecnologias Regionais) - Universidade Federal do Rio Grande do Norte, Natal, 2013.https://repositorio.ufrn.br/jspui/handle/123456789/15848In this work it was synthesized and characterized the cobalt ferrite (CoFe2O4) by two methods: complexation combining EDTA/Citrate and hydrothermal investigating the influence of the synthesis conditions on phase formation and on the crystallite size. The powders were mainly characterized by x-ray diffraction. In specific cases, it was also used scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray fluorescence (XRF) and isotherms of adsorption and desorption of nitrogen (BET method). The study of the crystallite size was based on the interpretation of x-ray diffractograms obtained and estimated by the method of Halder-Wagner-Scherrer and Langford. An experimental design was made in order to assist in quantifying the influence of synthesis conditions on the response variables. The synthesis parameters evaluated in this study were: pH of the reaction medium (8, 9 and 10), the calcination temperature (combined complexation method EDTA/Citrate 600°C, 800°C and 1000°C), synthesis temperature (hydrothermal method 120°C, 140°C and 160°C), calcination time (combined complexation method EDTA/Citrate - 2, 4 and 6 hours) and time of synthesis (hydrothermal method 6, 15 and 24 hours). By the hydrothermal method was possible to produce mesoporous powders with high purity, with an average crystallite size up to 7 nm, with a surface area of 113.44 m²/g in the form of pellets with irregular morphology. By using the method of combined complexation EDTA/Citrate, mesoporous powders were produced with greater purity, crystallite size up to 22nm and 27.95 m²/g of surface area in the form of pellets with a regular morphology of plaques. In the experimental design was found that the hydrothermal method to all the studied parameters (pH, temperature and time) have significant effect on the crystallite size, while to the combined complexation method EDTA/Citrate, only temperature and time were significantNeste trabalho foi sintetizada e caracterizada a ferrita de cobalto (CoFe2O4) através dos métodos complexação combinada EDTA/Citrato e hidrotérmico, investigando a influência das condições de síntese na formação da fase e no tamanho médio de cristalito. Os pós foram caracterizados principalmente por difração de raios-x. Em casos específicos, também foi utilizado microscopia eletrônica de varredura (MEV), espectroscopia de energia dispersiva (EDS), fluorescência de raios-x (FRX) e isotermas de adsorção e dessorção de nitrogênio (Método BET). O estudo do tamanho de cristalito foi baseado na interpretação dos difratogramas de raios-x obtidos e estimado através do método de Halder-Wagner-Langford (HWL) e de Scherrer. Um planejamento experimental foi realizado com a finalidade de auxiliar na quantificação da influência das condições de síntese nas variáveis-resposta. Os parâmetros de síntese avaliados neste trabalho foram: pH do meio reacional (8, 9 e 10), temperatura de calcinação (método de complexação combinando EDTA/Citrato 600°C, 800°C e 1000°C), temperatura de síntese (método hidrotérmico 120°C, 140°C e 160°C), tempo de calcinação (método de complexação combinando EDTA/Citrato 2, 4 e 6 hrs) e tempo de síntese (método hidrotérmico 6, 15 e 24 hrs). Pelo método hidrotérmico foi possível produzir pós mesoporosos com elevado grau de pureza, com tamanho médio de cristalito de até 7nm, com área superficial de 113,44m²/g e na forma de aglomerados com morfologia irregular. Ao se utilizar o método de complexação combinando EDTA/Citrato foram produzidos pós mesoporosos com maior pureza, cristalitos com até 22nm de tamanho, 27,95m²/g de área superficial e na forma de aglomerados com morfologia regular de placas. No planejamento experimental foi constatado que no caso do método hidrotérmico todos os parâmetros estudados (pH, Temperatura e tempo) apresentam efeito significativo no tamanho de cristalito, enquanto que, para o método de complexação combinando EDTA/Citrato, apenas a temperatura e o tempo foram significativosCoordenação de Aperfeiçoamento de Pessoal de Nível Superior2019-01-16application/pdfporUniversidade Federal do Rio Grande do NortePrograma de Pós-Graduação em Engenharia QuímicaUFRNBRPesquisa e Desenvolvimento de Tecnologias RegionaisFerrita de cobalto. Síntese via complexação combinando EDTA/Citrato. Síntese hidrotérmica. Caracterização de pós de óxidos. Planejamento experimentalCobalt Ferrite. Synthesis via combined complexation EDTA/Citrate. Hydrothermal synthesis. Characterization of oxide powders. Experimental designCNPQ::ENGENHARIAS::ENGENHARIA QUIMICAObtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmicoObtaining cobalt ferrite through two synthesis methods: Complexation Method Conbining EDTA/Citrate and Hydrothermal Methodinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFRNinstname:Universidade Federal do Rio Grande do Norte (UFRN)instacron:UFRNORIGINALIndiraAFM_DISSERT.pdfIndiraAFM_DISSERT.pdfapplication/pdf2764520https://repositorio.ufrn.br/bitstream/123456789/15848/1/IndiraAFM_DISSERT.pdf47a2552466803458b0edbc020e77922dMD51TEXTIndiraAFM_DISSERT.pdf.txtIndiraAFM_DISSERT.pdf.txtExtracted texttext/plain168748https://repositorio.ufrn.br/bitstream/123456789/15848/11/IndiraAFM_DISSERT.pdf.txt80b384ae2c04a5b94dc0f2fca2e89e1aMD511THUMBNAILIndiraAFM_DISSERT.pdf.jpgIndiraAFM_DISSERT.pdf.jpgIM Thumbnailimage/jpeg4189https://repositorio.ufrn.br/bitstream/123456789/15848/12/IndiraAFM_DISSERT.pdf.jpgae3a87cfa11b514d65a1296b62b939c6MD512123456789/158482024-03-19 01:03:24.102oai:https://repositorio.ufrn.br:123456789/15848Repositório de PublicaçõesPUBhttp://repositorio.ufrn.br/oai/opendoar:2024-03-19T04:03:24Repositório Institucional da UFRN - Universidade Federal do Rio Grande do Norte (UFRN)false |
dc.title.por.fl_str_mv |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
dc.title.alternative.eng.fl_str_mv |
Obtaining cobalt ferrite through two synthesis methods: Complexation Method Conbining EDTA/Citrate and Hydrothermal Method |
title |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
spellingShingle |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico Medeiros, Indira Aritana Fernandes de Ferrita de cobalto. Síntese via complexação combinando EDTA/Citrato. Síntese hidrotérmica. Caracterização de pós de óxidos. Planejamento experimental Cobalt Ferrite. Synthesis via combined complexation EDTA/Citrate. Hydrothermal synthesis. Characterization of oxide powders. Experimental design CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA |
title_short |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
title_full |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
title_fullStr |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
title_full_unstemmed |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
title_sort |
Obtenção de ferrita de cobalto através de dois métodos de síntese: método de complexação combinando EDTA/Citrato e método hidrotérmico |
author |
Medeiros, Indira Aritana Fernandes de |
author_facet |
Medeiros, Indira Aritana Fernandes de |
author_role |
author |
dc.contributor.authorID.por.fl_str_mv |
|
dc.contributor.authorLattes.por.fl_str_mv |
http://lattes.cnpq.br/0540859141209826 |
dc.contributor.advisorID.por.fl_str_mv |
|
dc.contributor.advisorLattes.por.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781094H3 |
dc.contributor.referees1.pt_BR.fl_str_mv |
Santos, Andarair Gomes dos |
dc.contributor.referees1ID.por.fl_str_mv |
|
dc.contributor.referees1Lattes.por.fl_str_mv |
http://lattes.cnpq.br/3470634368296605 |
dc.contributor.referees2.pt_BR.fl_str_mv |
Silva, Gilson Garcia da |
dc.contributor.referees2ID.por.fl_str_mv |
|
dc.contributor.referees2Lattes.por.fl_str_mv |
http://lattes.cnpq.br/8681275097040450 |
dc.contributor.author.fl_str_mv |
Medeiros, Indira Aritana Fernandes de |
dc.contributor.advisor1.fl_str_mv |
Souza, Carlson Pereira de |
contributor_str_mv |
Souza, Carlson Pereira de |
dc.subject.por.fl_str_mv |
Ferrita de cobalto. Síntese via complexação combinando EDTA/Citrato. Síntese hidrotérmica. Caracterização de pós de óxidos. Planejamento experimental |
topic |
Ferrita de cobalto. Síntese via complexação combinando EDTA/Citrato. Síntese hidrotérmica. Caracterização de pós de óxidos. Planejamento experimental Cobalt Ferrite. Synthesis via combined complexation EDTA/Citrate. Hydrothermal synthesis. Characterization of oxide powders. Experimental design CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA |
dc.subject.eng.fl_str_mv |
Cobalt Ferrite. Synthesis via combined complexation EDTA/Citrate. Hydrothermal synthesis. Characterization of oxide powders. Experimental design |
dc.subject.cnpq.fl_str_mv |
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA |
description |
In this work it was synthesized and characterized the cobalt ferrite (CoFe2O4) by two methods: complexation combining EDTA/Citrate and hydrothermal investigating the influence of the synthesis conditions on phase formation and on the crystallite size. The powders were mainly characterized by x-ray diffraction. In specific cases, it was also used scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray fluorescence (XRF) and isotherms of adsorption and desorption of nitrogen (BET method). The study of the crystallite size was based on the interpretation of x-ray diffractograms obtained and estimated by the method of Halder-Wagner-Scherrer and Langford. An experimental design was made in order to assist in quantifying the influence of synthesis conditions on the response variables. The synthesis parameters evaluated in this study were: pH of the reaction medium (8, 9 and 10), the calcination temperature (combined complexation method EDTA/Citrate 600°C, 800°C and 1000°C), synthesis temperature (hydrothermal method 120°C, 140°C and 160°C), calcination time (combined complexation method EDTA/Citrate - 2, 4 and 6 hours) and time of synthesis (hydrothermal method 6, 15 and 24 hours). By the hydrothermal method was possible to produce mesoporous powders with high purity, with an average crystallite size up to 7 nm, with a surface area of 113.44 m²/g in the form of pellets with irregular morphology. By using the method of combined complexation EDTA/Citrate, mesoporous powders were produced with greater purity, crystallite size up to 22nm and 27.95 m²/g of surface area in the form of pellets with a regular morphology of plaques. In the experimental design was found that the hydrothermal method to all the studied parameters (pH, temperature and time) have significant effect on the crystallite size, while to the combined complexation method EDTA/Citrate, only temperature and time were significant |
publishDate |
2013 |
dc.date.issued.fl_str_mv |
2013-12-17 |
dc.date.accessioned.fl_str_mv |
2014-12-17T15:01:34Z |
dc.date.available.fl_str_mv |
2014-06-20 2014-12-17T15:01:34Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
MEDEIROS, Indira Aritana Fernandes de. Obtaining cobalt ferrite through two synthesis methods: Complexation Method Conbining EDTA/Citrate and Hydrothermal Method. 2013. 139 f. Dissertação (Mestrado em Pesquisa e Desenvolvimento de Tecnologias Regionais) - Universidade Federal do Rio Grande do Norte, Natal, 2013. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufrn.br/jspui/handle/123456789/15848 |
identifier_str_mv |
MEDEIROS, Indira Aritana Fernandes de. Obtaining cobalt ferrite through two synthesis methods: Complexation Method Conbining EDTA/Citrate and Hydrothermal Method. 2013. 139 f. Dissertação (Mestrado em Pesquisa e Desenvolvimento de Tecnologias Regionais) - Universidade Federal do Rio Grande do Norte, Natal, 2013. |
url |
https://repositorio.ufrn.br/jspui/handle/123456789/15848 |
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por |
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Universidade Federal do Rio Grande do Norte |
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Programa de Pós-Graduação em Engenharia Química |
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UFRN |
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BR |
dc.publisher.department.fl_str_mv |
Pesquisa e Desenvolvimento de Tecnologias Regionais |
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Universidade Federal do Rio Grande do Norte |
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