Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique

Detalhes bibliográficos
Autor(a) principal: Mosquim, Victor
Data de Publicação: 2019
Tipo de documento: Dissertação
Idioma: eng
Título da fonte: Biblioteca Digital de Teses e Dissertações da USP
Texto Completo: http://www.teses.usp.br/teses/disponiveis/25/25148/tde-26112019-161457/
Resumo: New glass ceramics enriched by polycrystalline materials has been produced by different processing methods. However, for these materials to be used as restorative dental materials in esthetical areas they must count with good optical properties, which are directly influenced by their structure and chemical composition. For these reasons, the aim of this study was to produce a new glass ceramic containing SiO2+Y-TZP via uniaxial/isostatic powder compression and to structurally and chemically characterize this material relating to its optical properties. SiO2 and Zpex® were used as starting powders. These two powders were mixed (97w%-3% ratio) and pressed in uniaxial (80MPa) and isostatic (206MPa) press and sintered at 1150ºC for 2h. The starting powders, the mixed powder (before sintering) and the sintered specimens were submitted to Scanning Electron Microscope/Energy Dispersive X-ray Spectroscopy (SEM/EDX), Transmission Electron Microscope (TEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The materials density was measured. The contrast ratio and translucency parameter of the sintered specimen were compared to lithium disilicate (IPS e.max® CAD HT A1) and zirconia-reinforced lithium silicate (Celtra Duo® HT A1), using Kruskal-Wallis and post-hoc Dunn tests with a significance level set at 5%. Agglomerations of SiO2 and Zpex could be seen under SEM/EDX analysis due to their reduced particle size, yet, when sintered, some remaining porosities could be seen. The TEM analysis evidenced the spherical character of SiO2 grains and the crystallographic pattern of the Zpex particles. When mixed, Zpex can be seen inside the grain of SiO2. XDR analysis pointed out that SiO2 was amorphous, and Zpex presented monoclinic (m) and tetragonal (t) peaks. After sintering, crystallization of SiO2 can be seen without new m peaks. The FTIR spectra bands suggested an interaction between Si, O and Zr. The theoretical density value of the experimental ceramics was 1.663 g/cm3. The contrast ratio and the translucency parameter of the experimental ceramic were higher (p=0,000001) and lower (p=0,000001), respectively, than those of lithium disilicate and zirconia-reinforced lithium silicate. It can be concluded that the uniaxial/isostatic powder compression is an efficient method to obtain experimental ceramics for dental purposes and 1150ºC for 2h is sufficient to crystallize SiO2 without inducing t-m transformation of zirconia. Yet, this sintering protocol seems to be insufficient to densify the experimental ceramic, which may the reason for its lack of translucency.
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spelling Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing techniqueCaracterizações estrutural, química e óptica de uma cerâmica experimental de SiO2-Y-TZP produzida pela técnica de prensagem uniaxial/isostáticaCerâmicaCeramicsDióxido de silícioSilicon dioxideZircônioZirconiumNew glass ceramics enriched by polycrystalline materials has been produced by different processing methods. However, for these materials to be used as restorative dental materials in esthetical areas they must count with good optical properties, which are directly influenced by their structure and chemical composition. For these reasons, the aim of this study was to produce a new glass ceramic containing SiO2+Y-TZP via uniaxial/isostatic powder compression and to structurally and chemically characterize this material relating to its optical properties. SiO2 and Zpex® were used as starting powders. These two powders were mixed (97w%-3% ratio) and pressed in uniaxial (80MPa) and isostatic (206MPa) press and sintered at 1150ºC for 2h. The starting powders, the mixed powder (before sintering) and the sintered specimens were submitted to Scanning Electron Microscope/Energy Dispersive X-ray Spectroscopy (SEM/EDX), Transmission Electron Microscope (TEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The materials density was measured. The contrast ratio and translucency parameter of the sintered specimen were compared to lithium disilicate (IPS e.max® CAD HT A1) and zirconia-reinforced lithium silicate (Celtra Duo® HT A1), using Kruskal-Wallis and post-hoc Dunn tests with a significance level set at 5%. Agglomerations of SiO2 and Zpex could be seen under SEM/EDX analysis due to their reduced particle size, yet, when sintered, some remaining porosities could be seen. The TEM analysis evidenced the spherical character of SiO2 grains and the crystallographic pattern of the Zpex particles. When mixed, Zpex can be seen inside the grain of SiO2. XDR analysis pointed out that SiO2 was amorphous, and Zpex presented monoclinic (m) and tetragonal (t) peaks. After sintering, crystallization of SiO2 can be seen without new m peaks. The FTIR spectra bands suggested an interaction between Si, O and Zr. The theoretical density value of the experimental ceramics was 1.663 g/cm3. The contrast ratio and the translucency parameter of the experimental ceramic were higher (p=0,000001) and lower (p=0,000001), respectively, than those of lithium disilicate and zirconia-reinforced lithium silicate. It can be concluded that the uniaxial/isostatic powder compression is an efficient method to obtain experimental ceramics for dental purposes and 1150ºC for 2h is sufficient to crystallize SiO2 without inducing t-m transformation of zirconia. Yet, this sintering protocol seems to be insufficient to densify the experimental ceramic, which may the reason for its lack of translucency.Novas cerâmicas vítreas enriquecidas por materiais policristalinos tem sido produzidas por diferentes métodos de processamento. Entretanto, para que sejam utilizados como materiais restauradores odontológicos em áreas estéticas, eles devem apresentar boas propriedades ópticas, que estão diretamente influenciadas por sua estrutura e composição química. Por esses motivos, o objetivo deste estudo foi produzir uma nova cerâmica vítrea contendo SiO2+Y-TZP através da via uniaxial/isostática, e caracterizar este material estrutural e quimicamente, relacionando às suas propriedades ópticas. SiO2 e Zpex® foram usados como pós de partida, misturados (97m%-3m%), prensados em prensa uniaxial (80MPa) e isostática (206MPa) e sinterizados à 1150ºC por 2h. Os pós de partida, o pó após a mistura (prévio à sinterização) e a amostra sinterizada foram submetidos à Microscopia Eletrônica de Varredura/Espectroscopia por Energia Dispersiva de Raios-X (MEV-EDX), Microscopia Eletrônica de Transmissão (MET), Difração de Raios-X (DRX) e Espectroscopia de Infravermelho com Transformada de Fourier (FTIR). A densidade do material foi mensurada. A razão de contraste e o parâmetro de translucidez da amostra sinterizada foram comparados aos do dissilicato de lítio (IPS e.max® CAD HT A1) e do silicato de lítio reforçado por zircônia (Celtra Duo® HT A1), utilizando os testes de Kruskal-Wallis e post-hoc Dunn com nível de significância de 5%. Aglomerações SiO2 e Zpex foram vistas sob MEV/EDX devido ao tamanho reduzido das partículas, porém, quando sinterizado, algumas porosidades puderam ser vistas. A análise em MET evidenciou o caráter esférico dos grãos de SiO2 e o padrão cristalográfico das partículas de Zpex. Quando misturados, Zpex pode ser visto dentro de uma partícula de SiO2. A análise em DRX destacou que a SiO2 era amorfo e Zpex apresentava picos monoclínicos (m) e tetragonais (t). Após a sinterização, a cristalização da SiO2 pode ser vista sem a formação de novos picos m. As bandas do espectro do FTIR sugeriram uma interação entre Si, O e Zr. A densidade do material foi 1,663g/cm3. A razão de contraste e o parâmetro de translucidez da cerâmica foi maior (p=0,000001) e menor (p=0,000001), respectivamente, que os do silicato de lítio e do silicato de lítio reforçado por zircônia. Podese concluir que a compressão dos pós em prensa uniaxial/isostática é um método eficiente em produzir cerâmicas experimentais para uso odontológico, e que 1150ºC por 2h é suficiente para cristalizar o SiO2 sem induzir transformação t-m na zirconia. Contudo, esse protocolo de sinterização parece ser insuficiente para densificar a cerâmica experimental, o que pode prejudicar sua translucidez.Biblioteca Digitais de Teses e Dissertações da USPBorges, Ana Flávia SanchesMosquim, Victor2019-04-29info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttp://www.teses.usp.br/teses/disponiveis/25/25148/tde-26112019-161457/reponame:Biblioteca Digital de Teses e Dissertações da USPinstname:Universidade de São Paulo (USP)instacron:USPLiberar o conteúdo para acesso público.info:eu-repo/semantics/openAccesseng2021-11-26T12:56:14Zoai:teses.usp.br:tde-26112019-161457Biblioteca Digital de Teses e Dissertaçõeshttp://www.teses.usp.br/PUBhttp://www.teses.usp.br/cgi-bin/mtd2br.plvirginia@if.usp.br|| atendimento@aguia.usp.br||virginia@if.usp.bropendoar:27212021-11-26T12:56:14Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)false
dc.title.none.fl_str_mv Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
Caracterizações estrutural, química e óptica de uma cerâmica experimental de SiO2-Y-TZP produzida pela técnica de prensagem uniaxial/isostática
title Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
spellingShingle Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
Mosquim, Victor
Cerâmica
Ceramics
Dióxido de silício
Silicon dioxide
Zircônio
Zirconium
title_short Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
title_full Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
title_fullStr Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
title_full_unstemmed Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
title_sort Structural, chemical and optical characterizations of an experimental SiO2-Y-TZP ceramic produced by the uniaxial/isostatic pressing technique
author Mosquim, Victor
author_facet Mosquim, Victor
author_role author
dc.contributor.none.fl_str_mv Borges, Ana Flávia Sanches
dc.contributor.author.fl_str_mv Mosquim, Victor
dc.subject.por.fl_str_mv Cerâmica
Ceramics
Dióxido de silício
Silicon dioxide
Zircônio
Zirconium
topic Cerâmica
Ceramics
Dióxido de silício
Silicon dioxide
Zircônio
Zirconium
description New glass ceramics enriched by polycrystalline materials has been produced by different processing methods. However, for these materials to be used as restorative dental materials in esthetical areas they must count with good optical properties, which are directly influenced by their structure and chemical composition. For these reasons, the aim of this study was to produce a new glass ceramic containing SiO2+Y-TZP via uniaxial/isostatic powder compression and to structurally and chemically characterize this material relating to its optical properties. SiO2 and Zpex® were used as starting powders. These two powders were mixed (97w%-3% ratio) and pressed in uniaxial (80MPa) and isostatic (206MPa) press and sintered at 1150ºC for 2h. The starting powders, the mixed powder (before sintering) and the sintered specimens were submitted to Scanning Electron Microscope/Energy Dispersive X-ray Spectroscopy (SEM/EDX), Transmission Electron Microscope (TEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The materials density was measured. The contrast ratio and translucency parameter of the sintered specimen were compared to lithium disilicate (IPS e.max® CAD HT A1) and zirconia-reinforced lithium silicate (Celtra Duo® HT A1), using Kruskal-Wallis and post-hoc Dunn tests with a significance level set at 5%. Agglomerations of SiO2 and Zpex could be seen under SEM/EDX analysis due to their reduced particle size, yet, when sintered, some remaining porosities could be seen. The TEM analysis evidenced the spherical character of SiO2 grains and the crystallographic pattern of the Zpex particles. When mixed, Zpex can be seen inside the grain of SiO2. XDR analysis pointed out that SiO2 was amorphous, and Zpex presented monoclinic (m) and tetragonal (t) peaks. After sintering, crystallization of SiO2 can be seen without new m peaks. The FTIR spectra bands suggested an interaction between Si, O and Zr. The theoretical density value of the experimental ceramics was 1.663 g/cm3. The contrast ratio and the translucency parameter of the experimental ceramic were higher (p=0,000001) and lower (p=0,000001), respectively, than those of lithium disilicate and zirconia-reinforced lithium silicate. It can be concluded that the uniaxial/isostatic powder compression is an efficient method to obtain experimental ceramics for dental purposes and 1150ºC for 2h is sufficient to crystallize SiO2 without inducing t-m transformation of zirconia. Yet, this sintering protocol seems to be insufficient to densify the experimental ceramic, which may the reason for its lack of translucency.
publishDate 2019
dc.date.none.fl_str_mv 2019-04-29
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
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dc.identifier.uri.fl_str_mv http://www.teses.usp.br/teses/disponiveis/25/25148/tde-26112019-161457/
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dc.language.iso.fl_str_mv eng
language eng
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dc.rights.driver.fl_str_mv Liberar o conteúdo para acesso público.
info:eu-repo/semantics/openAccess
rights_invalid_str_mv Liberar o conteúdo para acesso público.
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
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dc.publisher.none.fl_str_mv Biblioteca Digitais de Teses e Dissertações da USP
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