Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos
| Ano de defesa: | 2018 |
|---|---|
| Autor(a) principal: | |
| Orientador(a): | |
| Banca de defesa: | |
| Tipo de documento: | Tese |
| Tipo de acesso: | Acesso aberto |
| Idioma: | por |
| Instituição de defesa: |
Universidade Federal de São Carlos
Câmpus São Carlos |
| Programa de Pós-Graduação: |
Programa de Pós-Graduação em Ciência e Engenharia de Materiais - PPGCEM
|
| Departamento: |
Não Informado pela instituição
|
| País: |
Não Informado pela instituição
|
| Palavras-chave em Português: | |
| Palavras-chave em Inglês: | |
| Área do conhecimento CNPq: | |
| Link de acesso: | https://repositorio.ufscar.br/handle/20.500.14289/10929 |
Resumo: | In this thesis, we investigated the microstructural development of BaCe0,9Y0,1O3-ẟ starting from aggregate-free submicrometric and nanometric powders. The differential of these powders is that synthesis occurred via solid-state reaction, compared to powders commonly used in the literature in the same size range. Nanometric particles were obtained by alternating steps of calcination with steps of grinding using isopropyl alcohol as dispersion media in a vibratory mill, and varying grinding time and load (weight ratio of grinding media/powder), with care to particle deflocculation, as well as keeping the grinding jars filled at only 50% of total capacity. The sinterability of compacts was surprisingly high, compared to literature reports, so that sintered samples with density higher than 95% of theoretical density were obtained at only 1200°C with dwell time of 10 hours. Literature shows that this degree of sintering is only achieved with the use of sintering aids. Systematic monitoring of microstructural development of the green compacts made with the different powders obtained in this thesis allowed the detection of a liquid phase appearing around 1200°C, which has not yet been reported in the literature. In green compacts with aggregates, the liquid phase was consumed in the densification of these defects so that macroporosity would remain even after sintering at 1600°C. In aggregate-free green compacts, the liquid phase aided to achieve high and homogeneous densification, mostly around the initial temperature of its formation. However, even after achieving high densification at low temperatures, higher ones are required in order to develop the microstructure in ways to reach adequate protonic electrical conductivity. The microstructure developed by powders obtained by grinding with 20:1 ratio (grinding media/powder) for 24h and sintered at 1600°C showed a proton conductivity of 2x10-2S/cm at 600°C which is in agreement with the best results in the literature. |
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Ramos, KethlinnSouza, Dulcina Maria Pinatti Ferreira dehttp://lattes.cnpq.br/4100119317525940http://lattes.cnpq.br/5856791042277661fcc8310d-070d-4875-879b-86c56ab50f3c2019-02-08T16:24:28Z2019-02-08T16:24:28Z2018-11-28RAMOS, Kethlinn. Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos. 2018. Tese (Doutorado em Ciência e Engenharia de Materiais) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/20.500.14289/10929.https://repositorio.ufscar.br/handle/20.500.14289/10929In this thesis, we investigated the microstructural development of BaCe0,9Y0,1O3-ẟ starting from aggregate-free submicrometric and nanometric powders. The differential of these powders is that synthesis occurred via solid-state reaction, compared to powders commonly used in the literature in the same size range. Nanometric particles were obtained by alternating steps of calcination with steps of grinding using isopropyl alcohol as dispersion media in a vibratory mill, and varying grinding time and load (weight ratio of grinding media/powder), with care to particle deflocculation, as well as keeping the grinding jars filled at only 50% of total capacity. The sinterability of compacts was surprisingly high, compared to literature reports, so that sintered samples with density higher than 95% of theoretical density were obtained at only 1200°C with dwell time of 10 hours. Literature shows that this degree of sintering is only achieved with the use of sintering aids. Systematic monitoring of microstructural development of the green compacts made with the different powders obtained in this thesis allowed the detection of a liquid phase appearing around 1200°C, which has not yet been reported in the literature. In green compacts with aggregates, the liquid phase was consumed in the densification of these defects so that macroporosity would remain even after sintering at 1600°C. In aggregate-free green compacts, the liquid phase aided to achieve high and homogeneous densification, mostly around the initial temperature of its formation. However, even after achieving high densification at low temperatures, higher ones are required in order to develop the microstructure in ways to reach adequate protonic electrical conductivity. The microstructure developed by powders obtained by grinding with 20:1 ratio (grinding media/powder) for 24h and sintered at 1600°C showed a proton conductivity of 2x10-2S/cm at 600°C which is in agreement with the best results in the literature.Nesta tese foi investigado o desenvolvimento microestrutural do BaCe0,9Y0,1O3 partindo de pós submicrométrico e nanométrico praticamente livres de agregados de partículas. O diferencial destes pós em relação àqueles normalmente utilizados na literatura, nesta faixa de tamanho de partículas, é que foram preparados pelo processo convencional de mistura de óxidos. Partículas nanométricas foram conseguidas utilizando calcinações alternadas com moagens em álcool isopropílico, realizadas em moinho vibratório variando tempo de moagem e relação (meios de moagem/ material) com cuidado em relação à defloculação, além de manter apenas 50% do volume do jarro preenchido. A sinterabilidade dos compactados foi surpreendentemente elevada em relação aos relatos da literatura, tendo sido obtidos corpos com densidade maior que 95% da densidade teórica a 1200ºC com patamar de 10 horas. Na literatura, este grau de sinterabilidade só é obtido com o uso de aditivo de sinterização. O acompanhamento sistemático do desenvolvimento microestrutural de compactos verdes dos diferentes pós obtidos nesta tese permitiram observar que no sistema investigado surge fase líquida em torno de 1200ºC, ainda não relatada na literatura. Se o compacto verde contém agregados, a fase líquida é consumida na densificação do próprio agregado e macroporos permanecem mesmo após sinterização a 1600ºC. Se o compacto verde é livre de agregados a fase líquida auxilia a densificação de forma homogênea e elevada densificação é rapidamente atingida em torno da temperatura de formação de fase líquida. Contudo, após densificação em baixa temperatura é necessário temperaturas maiores para ocorrer evolução microestrutural de modo a estabelecer a propriedade de interesse adequada, no caso, condutividade elétrica protônica. A microestrutura desenvolvida com pós obtidos na relação 20:1 (meio de moagem/material) com moagens de 24h intercaladas com calcinação e sinterizada a 1600°C apresentou condutividade protônica de 2 x 10-2S/cm a 600°C o que está em acordo com os melhores resultados da literatura.Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)CNPq: 140452/2014-1CAPES: Código de Financiamento 001porUniversidade Federal de São CarlosCâmpus São CarlosPrograma de Pós-Graduação em Ciência e Engenharia de Materiais - PPGCEMUFSCarCerato de bário dopado com ítrioSinterização via fase líquidaDesenvolvimento microestruturalCondução elétricaYttrium doped-barium cerateLiquid phase sinteringMicrostructural developmentElectrical conductionENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICASinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidosSinterability, microstructural development and electrical characterization of BaCe0,9Y0,1O3-ẟ nanometric powders obtained via solid-state reactioninfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisOnline60070fa011e-1108-4239-97ab-fe5cd4b2d233info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINALTese Versão Definitiva - KETHLINN RAMOS.pdfTese Versão Definitiva - KETHLINN RAMOS.pdfapplication/pdf4065897https://repositorio.ufscar.br/bitstreams/fc4a3a1e-b6ff-4f97-bdbd-983b0381ac97/download2a02bcc48435d6c54d624b206e73dc73MD51trueAnonymousREADLICENSElicense.txtlicense.txttext/plain; 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| dc.title.por.fl_str_mv |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| dc.title.alternative.eng.fl_str_mv |
Sinterability, microstructural development and electrical characterization of BaCe0,9Y0,1O3-ẟ nanometric powders obtained via solid-state reaction |
| title |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| spellingShingle |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos Ramos, Kethlinn Cerato de bário dopado com ítrio Sinterização via fase líquida Desenvolvimento microestrutural Condução elétrica Yttrium doped-barium cerate Liquid phase sintering Microstructural development Electrical conduction ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
| title_short |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| title_full |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| title_fullStr |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| title_full_unstemmed |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| title_sort |
Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos |
| author |
Ramos, Kethlinn |
| author_facet |
Ramos, Kethlinn |
| author_role |
author |
| dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/5856791042277661 |
| dc.contributor.author.fl_str_mv |
Ramos, Kethlinn |
| dc.contributor.advisor1.fl_str_mv |
Souza, Dulcina Maria Pinatti Ferreira de |
| dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4100119317525940 |
| dc.contributor.authorID.fl_str_mv |
fcc8310d-070d-4875-879b-86c56ab50f3c |
| contributor_str_mv |
Souza, Dulcina Maria Pinatti Ferreira de |
| dc.subject.por.fl_str_mv |
Cerato de bário dopado com ítrio Sinterização via fase líquida Desenvolvimento microestrutural Condução elétrica |
| topic |
Cerato de bário dopado com ítrio Sinterização via fase líquida Desenvolvimento microestrutural Condução elétrica Yttrium doped-barium cerate Liquid phase sintering Microstructural development Electrical conduction ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
| dc.subject.eng.fl_str_mv |
Yttrium doped-barium cerate Liquid phase sintering Microstructural development Electrical conduction |
| dc.subject.cnpq.fl_str_mv |
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
| description |
In this thesis, we investigated the microstructural development of BaCe0,9Y0,1O3-ẟ starting from aggregate-free submicrometric and nanometric powders. The differential of these powders is that synthesis occurred via solid-state reaction, compared to powders commonly used in the literature in the same size range. Nanometric particles were obtained by alternating steps of calcination with steps of grinding using isopropyl alcohol as dispersion media in a vibratory mill, and varying grinding time and load (weight ratio of grinding media/powder), with care to particle deflocculation, as well as keeping the grinding jars filled at only 50% of total capacity. The sinterability of compacts was surprisingly high, compared to literature reports, so that sintered samples with density higher than 95% of theoretical density were obtained at only 1200°C with dwell time of 10 hours. Literature shows that this degree of sintering is only achieved with the use of sintering aids. Systematic monitoring of microstructural development of the green compacts made with the different powders obtained in this thesis allowed the detection of a liquid phase appearing around 1200°C, which has not yet been reported in the literature. In green compacts with aggregates, the liquid phase was consumed in the densification of these defects so that macroporosity would remain even after sintering at 1600°C. In aggregate-free green compacts, the liquid phase aided to achieve high and homogeneous densification, mostly around the initial temperature of its formation. However, even after achieving high densification at low temperatures, higher ones are required in order to develop the microstructure in ways to reach adequate protonic electrical conductivity. The microstructure developed by powders obtained by grinding with 20:1 ratio (grinding media/powder) for 24h and sintered at 1600°C showed a proton conductivity of 2x10-2S/cm at 600°C which is in agreement with the best results in the literature. |
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2018 |
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2018-11-28 |
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2019-02-08T16:24:28Z |
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2019-02-08T16:24:28Z |
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RAMOS, Kethlinn. Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos. 2018. Tese (Doutorado em Ciência e Engenharia de Materiais) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/20.500.14289/10929. |
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https://repositorio.ufscar.br/handle/20.500.14289/10929 |
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RAMOS, Kethlinn. Sinterabilidade, desenvolvimento microestrutural e caracterização elétrica do BaCe0,9Y0,1O3-ẟ nanométrico obtido por mistura de óxidos. 2018. Tese (Doutorado em Ciência e Engenharia de Materiais) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/20.500.14289/10929. |
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