Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging

Detalhes bibliográficos
Autor(a) principal: Ernesto Byron Benalcazar Jalkh
Data de Publicação: 2021
Tipo de documento: Tese
Idioma: eng
Título da fonte: Biblioteca Digital de Teses e Dissertações da USP
Texto Completo: https://doi.org/10.11606/T.25.2021.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.
id USP_b80805e4462a906cdad5132f592339c0
oai_identifier_str oai:teses.usp.br:tde-07022022-122958
network_acronym_str USP
network_name_str Biblioteca Digital de Teses e Dissertações da USP
repository_id_str 2721
spelling info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesis 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 2021-11-03Estevam Augusto BonfantePaulo Francisco CesarEdmara Tatiely Pedroso BergamoPaulo Noronha Lisboa FilhoSergio Mazurek TebcheraniErnesto Byron Benalcazar JalkhUniversidade de São PauloCiências Odontológicas AplicadasUSPBR Composites Compósitos Mechanical properties Nanoindentação Nanoindentation Optical properties Propriedades Mecânicas Propriedades Ópticas Topografia Topography ZrO2Al2O3 ZrO2Al2O3 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. 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. https://doi.org/10.11606/T.25.2021.tde-07022022-122958info:eu-repo/semantics/openAccessengreponame:Biblioteca Digital de Teses e Dissertações da USPinstname:Universidade de São Paulo (USP)instacron:USP2023-12-21T18:22:24Zoai: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:27212023-12-22T12:15:58.017302Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)false
dc.title.en.fl_str_mv Experimental 70% Al2O3 - 30% ZrO2 composites: structural, topographical and mechanical characterization before and after aging
dc.title.alternative.pt.fl_str_mv 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
Ernesto Byron Benalcazar Jalkh
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 Ernesto Byron Benalcazar Jalkh
author_facet Ernesto Byron Benalcazar Jalkh
author_role author
dc.contributor.advisor1.fl_str_mv Estevam Augusto Bonfante
dc.contributor.advisor-co1.fl_str_mv Paulo Francisco Cesar
dc.contributor.referee1.fl_str_mv Edmara Tatiely Pedroso Bergamo
dc.contributor.referee2.fl_str_mv Paulo Noronha Lisboa Filho
dc.contributor.referee3.fl_str_mv Sergio Mazurek Tebcherani
dc.contributor.author.fl_str_mv Ernesto Byron Benalcazar Jalkh
contributor_str_mv Estevam Augusto Bonfante
Paulo Francisco Cesar
Edmara Tatiely Pedroso Bergamo
Paulo Noronha Lisboa Filho
Sergio Mazurek Tebcherani
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.issued.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://doi.org/10.11606/T.25.2021.tde-07022022-122958
url https://doi.org/10.11606/T.25.2021.tde-07022022-122958
dc.language.iso.fl_str_mv eng
language eng
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Universidade de São Paulo
dc.publisher.program.fl_str_mv Ciências Odontológicas Aplicadas
dc.publisher.initials.fl_str_mv USP
dc.publisher.country.fl_str_mv BR
publisher.none.fl_str_mv Universidade de São Paulo
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
_version_ 1794502535979991040