Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging
Autor(a) principal: | |
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Data de Publicação: | 2021 |
Tipo de documento: | Tese |
Idioma: | eng |
Título da fonte: | Biblioteca Digital de Teses e Dissertações da USP |
Texto Completo: | https://www.teses.usp.br/teses/disponiveis/25/25146/tde-07022022-122958/ |
Resumo: | Objectives: To evaluate the effect of aging on the crystalline structure, surface topography and mechanical properties of an experimental zirconia-toughened-alumina (ZTA) composite comprised by 70% Al2O3 and 30% of a 2nd-generation 3mol% yttria tetragonal zirconia polycrystal (3Y-TZP), compared to its individual counterpart materials. Materials and Methods: Disc-shaped ceramic specimens were divided in four groups (n=10/material): 1) 3YSB-E (1st-generation 3Y-TZP), 2) Zpex (2nd-generation 3Y-TZP), 3) Alumina, and 4) ZTA-Zpex 70/30. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the crystalline content and microstructure. Reflectance tests were performed to determine the contrast-ratio (CR) and translucency-parameter (TP). Mechanical properties were assessed by biaxial-flexural-strength (BFS) test to determine Weibull parameters. ZTA and its isolated materials were tested under nanoindentation to record elastic modulus (E) and hardness (H); and Interferometry to assess 3D surface roughness parameters (Sa, Sq). All analyses were conducted before and after autoclave aging (20h, 134oC, 2.2bar). Optical parameters were evaluated through repeated-measures analysis of variance and Tukey tests (p<0.05), BFS data were analyzed using Weibull statistics (95% CI); and nanoindentation and topographic results were analyzed using linear mixed-model and least square difference pos-hoc tests (a=5%). Results: High density values were found for all materials and SEM images exhibited a dense microstructure. While XRD patterns revealed the preservation of crystalline content in the ZTA composite, an increase in the monoclinic phase was observed for pure zirconias after aging. Higher CR and lower TP values were observed for ZTA, followed by Alumina, 3YSB-E, and Zpex. The highest characteristic stress was recorded for 3YSB-E, followed by intermediate values between ZTA and Zpex, and the lowest for Alumina. Conversely, Al2O3 yielded the highest H and E values, followed by ZTA-70/30 and Zpex. Aging affected the optical and mechanical properties of both zirconias, while remained stable for ZTA and alumina. Aging did not affect the surface roughness parameters of ZTA and Alumina, although a significant increase in Sa was recorded for Zpex following aging. Conclusion: The synthesis of the experimental 70-30% ZTA composite was successful and its relevance for dental applications relies on its higher masking ability, aging resistance, and strength similar to zirconia. |
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Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after agingCompósitos experimentais 70%Al2O3-30%ZrO2: caracterização estrutural, topográfica e mecânica antes e após envelhecimentoCompositesCompósitosMechanical propertiesNanoindentaçãoNanoindentationOptical propertiesPropriedades MecânicasPropriedades ÓpticasTopografiaTopographyZrO2Al2O3ZrO2Al2O3Objectives: To evaluate the effect of aging on the crystalline structure, surface topography and mechanical properties of an experimental zirconia-toughened-alumina (ZTA) composite comprised by 70% Al2O3 and 30% of a 2nd-generation 3mol% yttria tetragonal zirconia polycrystal (3Y-TZP), compared to its individual counterpart materials. Materials and Methods: Disc-shaped ceramic specimens were divided in four groups (n=10/material): 1) 3YSB-E (1st-generation 3Y-TZP), 2) Zpex (2nd-generation 3Y-TZP), 3) Alumina, and 4) ZTA-Zpex 70/30. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the crystalline content and microstructure. Reflectance tests were performed to determine the contrast-ratio (CR) and translucency-parameter (TP). Mechanical properties were assessed by biaxial-flexural-strength (BFS) test to determine Weibull parameters. ZTA and its isolated materials were tested under nanoindentation to record elastic modulus (E) and hardness (H); and Interferometry to assess 3D surface roughness parameters (Sa, Sq). All analyses were conducted before and after autoclave aging (20h, 134oC, 2.2bar). Optical parameters were evaluated through repeated-measures analysis of variance and Tukey tests (p<0.05), BFS data were analyzed using Weibull statistics (95% CI); and nanoindentation and topographic results were analyzed using linear mixed-model and least square difference pos-hoc tests (a=5%). Results: High density values were found for all materials and SEM images exhibited a dense microstructure. While XRD patterns revealed the preservation of crystalline content in the ZTA composite, an increase in the monoclinic phase was observed for pure zirconias after aging. Higher CR and lower TP values were observed for ZTA, followed by Alumina, 3YSB-E, and Zpex. The highest characteristic stress was recorded for 3YSB-E, followed by intermediate values between ZTA and Zpex, and the lowest for Alumina. Conversely, Al2O3 yielded the highest H and E values, followed by ZTA-70/30 and Zpex. Aging affected the optical and mechanical properties of both zirconias, while remained stable for ZTA and alumina. Aging did not affect the surface roughness parameters of ZTA and Alumina, although a significant increase in Sa was recorded for Zpex following aging. Conclusion: The synthesis of the experimental 70-30% ZTA composite was successful and its relevance for dental applications relies on its higher masking ability, aging resistance, and strength similar to zirconia.Objetivo: Avaliar o efeito do envelhecimento na estrutura cristalina, topografia de superfície e propriedades mecânicas de um compósito experimental de alumina reforçada com zircônia (ZTA) composto por 70% de Al2O3 e 30% de uma zirconia de segunda geração, em comparação com os seus materiais individuais. Materiais e métodos: Espécimes em formato de discos foram divididos em quatro grupos (n = 10 / material): 1) 3YSB-E (3Y-TZP de primeira geração), 2) Zpex (3Y-TZP de segunda geração), 3) Alumina e 4) ZTA-Zpex 70/30. Difração de raios X (DRX) e microscopia eletrônica de varredura (MEV) foram usados para caracterizar o conteúdo cristalino e a microestrutura dos materiais. Testes de refletância foram realizados para determinar a razão de contraste (RC) e o parâmetro de translucidez (PT). As propriedades mecânicas foram avaliadas pelo teste de resistência à flexão biaxial (RFB) para determinar os parâmetros de Weibull. ZTA, Zpex e Alumina foram adicionalmente testados sob nanoindentação para obter módulo de elasticidade (E) e dureza (H); e por Interferometria para avaliar parâmetros de rugosidade superficial 3D (Sa, Sq). Todas as análises foram realizadas antes e após o envelhecimento artificial (20h, 134oC, 2,2 bar). Os dados de propriedades ópticas foram avaliados por meio da análise de variância de medidas repetidas e testes de Tukey (p <0,05); os dados da RFB foram analisados pela estatística de Weibull (IC95%); e dados de nanoindentação e resultados topográficos foram analisados usando modelos lineares mistos e testes pos-hoc de diferença de mínimos quadrados (a = 5%). Resultados: Valores de alta densidade foram encontrados para todos os materiais e as imagens de MEV exibiram uma microestrutura densa. Os padrões de XRD revelaram a preservação do conteúdo cristalino no compósito ZTA, enquanto um aumento nos picos monoclínicos foi observado para zircônias puras após envelhecimento. Maior RC e menor PT foram observados para o compósito ZTA, seguido por alumina, 3YSB-E e Zpex. O maior estresse característico foi registrado para 3YSB-E, seguido por valores intermediários entre Zpex e ZTA, e o menor para Alumina. Al2O3 apresentou os maiores valores de H e E, seguido por ZTA-70/30 e Zpex, todos significativamente diferentes. O envelhecimento afetou as propriedades ópticas e mecânicas de ambas as zircônias, enquanto se manteve estável para o compósito ZTA e alumina. O envelhecimento não afetou os parâmetros de rugosidade da superfície de ZTA-70/30 e Al2O3, embora um aumento significativo de Sa tenha sido registrado para Zpex após o envelhecimento. Conclusão: A síntese experimental do compósito ZTA 70-30% foi bem-sucedida e sua relevância para aplicações odontológicas está em sua maior capacidade de mascaramento, resistência ao envelhecimento em todos os parâmetros testados e resistência semelhante à zircônia. O envelhecimento aumentou significativamente o conteúdo monoclínico das zircônias puras e afetou as suas propriedades ópticas e mecânicas, bem como sua rugosidade superficial.Biblioteca Digitais de Teses e Dissertações da USPBonfante, Estevam AugustoCesar, Paulo FranciscoJalkh, Ernesto Byron Benalcazar2021-11-03info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfhttps://www.teses.usp.br/teses/disponiveis/25/25146/tde-07022022-122958/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/openAccesseng2022-02-08T14:44:02Zoai:teses.usp.br:tde-07022022-122958Biblioteca 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:27212022-02-08T14:44:02Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)false |
dc.title.none.fl_str_mv |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging Compósitos experimentais 70%Al2O3-30%ZrO2: caracterização estrutural, topográfica e mecânica antes e após envelhecimento |
title |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging |
spellingShingle |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging Jalkh, Ernesto Byron Benalcazar Composites Compósitos Mechanical properties Nanoindentação Nanoindentation Optical properties Propriedades Mecânicas Propriedades Ópticas Topografia Topography ZrO2Al2O3 ZrO2Al2O3 |
title_short |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging |
title_full |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging |
title_fullStr |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging |
title_full_unstemmed |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging |
title_sort |
Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging |
author |
Jalkh, Ernesto Byron Benalcazar |
author_facet |
Jalkh, Ernesto Byron Benalcazar |
author_role |
author |
dc.contributor.none.fl_str_mv |
Bonfante, Estevam Augusto Cesar, Paulo Francisco |
dc.contributor.author.fl_str_mv |
Jalkh, Ernesto Byron Benalcazar |
dc.subject.por.fl_str_mv |
Composites Compósitos Mechanical properties Nanoindentação Nanoindentation Optical properties Propriedades Mecânicas Propriedades Ópticas Topografia Topography ZrO2Al2O3 ZrO2Al2O3 |
topic |
Composites Compósitos Mechanical properties Nanoindentação Nanoindentation Optical properties Propriedades Mecânicas Propriedades Ópticas Topografia Topography ZrO2Al2O3 ZrO2Al2O3 |
description |
Objectives: To evaluate the effect of aging on the crystalline structure, surface topography and mechanical properties of an experimental zirconia-toughened-alumina (ZTA) composite comprised by 70% Al2O3 and 30% of a 2nd-generation 3mol% yttria tetragonal zirconia polycrystal (3Y-TZP), compared to its individual counterpart materials. Materials and Methods: Disc-shaped ceramic specimens were divided in four groups (n=10/material): 1) 3YSB-E (1st-generation 3Y-TZP), 2) Zpex (2nd-generation 3Y-TZP), 3) Alumina, and 4) ZTA-Zpex 70/30. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the crystalline content and microstructure. Reflectance tests were performed to determine the contrast-ratio (CR) and translucency-parameter (TP). Mechanical properties were assessed by biaxial-flexural-strength (BFS) test to determine Weibull parameters. ZTA and its isolated materials were tested under nanoindentation to record elastic modulus (E) and hardness (H); and Interferometry to assess 3D surface roughness parameters (Sa, Sq). All analyses were conducted before and after autoclave aging (20h, 134oC, 2.2bar). Optical parameters were evaluated through repeated-measures analysis of variance and Tukey tests (p<0.05), BFS data were analyzed using Weibull statistics (95% CI); and nanoindentation and topographic results were analyzed using linear mixed-model and least square difference pos-hoc tests (a=5%). Results: High density values were found for all materials and SEM images exhibited a dense microstructure. While XRD patterns revealed the preservation of crystalline content in the ZTA composite, an increase in the monoclinic phase was observed for pure zirconias after aging. Higher CR and lower TP values were observed for ZTA, followed by Alumina, 3YSB-E, and Zpex. The highest characteristic stress was recorded for 3YSB-E, followed by intermediate values between ZTA and Zpex, and the lowest for Alumina. Conversely, Al2O3 yielded the highest H and E values, followed by ZTA-70/30 and Zpex. Aging affected the optical and mechanical properties of both zirconias, while remained stable for ZTA and alumina. Aging did not affect the surface roughness parameters of ZTA and Alumina, although a significant increase in Sa was recorded for Zpex following aging. Conclusion: The synthesis of the experimental 70-30% ZTA composite was successful and its relevance for dental applications relies on its higher masking ability, aging resistance, and strength similar to zirconia. |
publishDate |
2021 |
dc.date.none.fl_str_mv |
2021-11-03 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
https://www.teses.usp.br/teses/disponiveis/25/25146/tde-07022022-122958/ |
url |
https://www.teses.usp.br/teses/disponiveis/25/25146/tde-07022022-122958/ |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
|
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 |
dc.coverage.none.fl_str_mv |
|
dc.publisher.none.fl_str_mv |
Biblioteca Digitais de Teses e Dissertações da USP |
publisher.none.fl_str_mv |
Biblioteca Digitais de Teses e Dissertações da USP |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações da USP instname:Universidade de São Paulo (USP) instacron:USP |
instname_str |
Universidade de São Paulo (USP) |
instacron_str |
USP |
institution |
USP |
reponame_str |
Biblioteca Digital de Teses e Dissertações da USP |
collection |
Biblioteca Digital de Teses e Dissertações da USP |
repository.name.fl_str_mv |
Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP) |
repository.mail.fl_str_mv |
virginia@if.usp.br|| atendimento@aguia.usp.br||virginia@if.usp.br |
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1815256775828439040 |