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Master's Dissertation
DOI
https://doi.org/10.11606/D.25.2022.tde-11112022-120208
Document
Author
Full name
Pedro Rodrigues Minim
Institute/School/College
Knowledge Area
Date of Defense
Published
Bauru, 2022
Supervisor
Committee
Rubo, Jose Henrique (President)
Borges, Ana Flávia Sanches
Fortulan, Carlos Alberto
Lisboa Filho, Paulo Noronha
Title in Portuguese
Efeitos dos parâmetros de sinterização e da adição de aglutinantes nas características estruturais de biocerâmicas densas de hidroxiapatita bovina
Keywords in Portuguese
Cerâmica
Durapatita
Materiais biocompatíveis
Abstract in Portuguese
A hidroxiapatita (HA) proveniente de estrutura óssea bovina tem elevada importância dentre os biomateriais devido à sua biocompatibilidade e bioatividade. Entretanto, as cerâmicas densas de hidroxiapatita bovina apresentam propriedades mecânicas insuficientes para a confecção de infra-estuturas de prótese fixa. O presente estudo objetivou avaliar o efeito da adição de polivinilbutiral (PVB) e ácido esteárico (AE) e de duas metodologias de sinterização (2-step e convencional), nas propriedades mecânicas de biocerâmica densa policristalina de HA de origem bovina. Dessa forma, a partir de um esquema fatorial 2x2, 4 grupos foram avaliados. Para tanto, a HA foi extraída de ossos bovinos, calcinados a 900 °C, nanoparticuladas em moinho de bolas e submetida à prensagem uniaxial estática em discos, conforme a norma ISO 6872. Os grupos submetidos a sinterização convencional (HAAC e HASC) tiveram pico máximo de temperatura de 1300 °C e resfriamento lento até a temperatura ambiente. Já os grupos com sinterização 2-step (HAA2 e HAS2), tiveram pico máximo de 950 °C com resfriamento rápido para 880 °C e posterior resfriamento lento a temperatura ambiente. As amostras dos 4 grupos foram caracterizadas por difratometria de raios-x (DRX), análise térmica diferencial (DTA) e espectroscopia de infravermelho por transformada de Fourrier (FTIR), e avaliadas pelos testes de microscopia eletrônica de varredura (MEV) densidade relativa, através do princípio de Arquimedes, pelo teste de resistência à flexão biaxial e pela análise do módulo de elasticidade. Os valores obtidos de densidade relativa e resistência à flexão foram submetidos ao teste de normalidade de Shapiro-Wilk e a partir disso foi realizado teste de Kruskal-Wallis e pós teste de Dunn, para todos os testes. Foi possível concluir que as cerâmicas de HA submetidas a sinterização convencional e sem a adição de aglutinantes obteve melhores propriedades mecânicas que os demais grupos.
Title in English
Effects of the sintering parameters and the addition of agglutinants on the structural characteristics of bovine hydroxyapatite dense bioceramics
Keywords in English
Biocompatible materials
Ceramics
Durapatite
Abstract in English
Hydroxyapatite (HA) from bovine bone structure has high importance among biomaterials due to its biocompatibility and bioactivity. However, hydroxyapatite dense ceramics have inadequate mechanical properties for their intended purpose. The present study aimed to evaluate the effect of the addition of polyvinyl butyral (PVB) and stearic acid (SA) and two sintering methodologies (2-step and conventional) on the mechanical properties of bovine hydroxyapatite dense polycrystalline bioceramic. Thus, from a 2x2 factorial scheme, 4 groups were evaluated. Therefore, HA was extracted from bovine bones, turned into nanoparticles in a ball mill and subjected to uniaxial and isostatic pressing into discs, according to the ISO 6872 standard. The groups submitted to conventional sintering (HAAC and HASC) had a maximum temperature peak of 1300 °C and slow cooling to room temperature. The groups with 2-step sintering (HAA2 and HAS2) had a maximum peak of 950 °C with rapid cooling to 880 °C and subsequent slow cooling to room temperature. The samples of the 4 groups were characterized by x-ray diffractometry (XRD), differential thermal analysis (DTA) and Fourrier transform infrared spectroscopy (FTIR), and evaluated by scanning electron microscopy (SEM) relative density, through the Archimedes principle, by the biaxial flexural strength test and by the analysis of the modulus of elasticity. The values obtained for relative density and flexural strength were submitted to the Shapiro-Wilk normality test and from there, the Kruskal-Wallis test and Dunn's post-test were performed for all tests. It was possible to conclude that the HA ceramics submitted to conventional sintering and without the addition of binders obtained better mechanical properties than the other groups.
 
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Publishing Date
2022-12-14
 
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