Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic

Detalhes bibliográficos
Autor(a) principal: Ferrairo, Brunna Mota
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-03122021-094954/
Resumo: Objectives: The aim of the study was to evaluate two methods of nanoparticulation methods of bovine hydroxyapatite (HA), synthesize an experimental SiO2/nano-hydroxyapatite composite ceramic and made a structurally and chemically characterization of them. Materials and Methods: Cortical of bovine femurs were selected and, after a pre-treatment, calcined and particulate. Sonication was performed with 40% of the maximum amplitude of 750W and 20Hz in aqueous solution added with HA and ammonia polyacrylate (4h of activation). Milling technique used a polyethylene jug (300 cm3) loaded with 40vol% (500g) milling elements (3Y zirconia balls, HA, isopropyl alcohol and para-aminobenzoic acid), placed in a rotatory mill (104rpm, 48h) followed by a vibratory mill (72h). Ball mill technique was used to mixture fumed silica and nano-HA from bovine bone source. Groups were divided into 3, 5 and 10% of HA addition, 1.2 and 2.4 wt.% of PVB, and 1100, 1200 and 1300 °C for maximum temperatures to firing plateau (4h). Characterization was performed by Transmission Electron Microscopy (TEM) / Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XDR) and Fourier Transform Infrared (FTIR). Results: The initial particle size is 75m and sonication (60 nm) and ball mill (40 nm) techniques, associated with prior calcination, were capable of producing nanosized bovine HA particles, maintaining an appropriate stoichiometry, morphology and purity. According to SH composite ceramic, the uniaxial/isostatic powder compression is an efficient method. The temperature of 1200 °C presented potentialized chemical bonds without the degradation of HA at XDR profile. SEM images suggests that 2.4 wt.% of PVB result in optimized compaction and a lower incidence of cracks and pores, and the SH composite ceramic with 5% of HA presents potential superior properties to biomaterial. Conclusion: The ball mill technique provided smaller particles of bovine hydroxyapatite and the experimental material SH composite ceramic with 5% of HA, 2.4 wt.% of PVB and sintered at 1200 °C presents potential superior properties to biomaterial.
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spelling Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramicMétodos de nanoparticulação da hidroxiapatita bovina, síntese e caracterização estrutural/química de um compósito cerâmico de SiO2/nano-hidroxiapatita experimentalCerâmicaCerâmica compostaCeramicsComposite ceramicHidroxiapatitaHydroxyapatiteSilicaSílicaObjectives: The aim of the study was to evaluate two methods of nanoparticulation methods of bovine hydroxyapatite (HA), synthesize an experimental SiO2/nano-hydroxyapatite composite ceramic and made a structurally and chemically characterization of them. Materials and Methods: Cortical of bovine femurs were selected and, after a pre-treatment, calcined and particulate. Sonication was performed with 40% of the maximum amplitude of 750W and 20Hz in aqueous solution added with HA and ammonia polyacrylate (4h of activation). Milling technique used a polyethylene jug (300 cm3) loaded with 40vol% (500g) milling elements (3Y zirconia balls, HA, isopropyl alcohol and para-aminobenzoic acid), placed in a rotatory mill (104rpm, 48h) followed by a vibratory mill (72h). Ball mill technique was used to mixture fumed silica and nano-HA from bovine bone source. Groups were divided into 3, 5 and 10% of HA addition, 1.2 and 2.4 wt.% of PVB, and 1100, 1200 and 1300 °C for maximum temperatures to firing plateau (4h). Characterization was performed by Transmission Electron Microscopy (TEM) / Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XDR) and Fourier Transform Infrared (FTIR). Results: The initial particle size is 75m and sonication (60 nm) and ball mill (40 nm) techniques, associated with prior calcination, were capable of producing nanosized bovine HA particles, maintaining an appropriate stoichiometry, morphology and purity. According to SH composite ceramic, the uniaxial/isostatic powder compression is an efficient method. The temperature of 1200 °C presented potentialized chemical bonds without the degradation of HA at XDR profile. SEM images suggests that 2.4 wt.% of PVB result in optimized compaction and a lower incidence of cracks and pores, and the SH composite ceramic with 5% of HA presents potential superior properties to biomaterial. Conclusion: The ball mill technique provided smaller particles of bovine hydroxyapatite and the experimental material SH composite ceramic with 5% of HA, 2.4 wt.% of PVB and sintered at 1200 °C presents potential superior properties to biomaterial.Objetivos: O objetivo deste trabalho foi testar dois métodos de nanoparticulação de hidroxiapatita bovina (HA), sintetizar um compósito cerâmico experimental SiO2/nanohidroxiapatita e caracterizá-los estrutural e quimicamente. Materiais e Métodos: Corticais de fêmures bovinos foram selecionadas e, após a remoção da matéria orgânica, calcinadas e particuladas. Para realização da nanoparticulação dois métodos foram selecionados: sonicação e moagem por moinho de bolas. A sonicação foi realizada com 40 % da amplitude máxima de 750 W e 20 Hz em solução aquosa acrescida de HA e poliacrilato de amônia (4 h de ativação). A técnica de moagem utilizou um jarro de polietileno (300 cm3) carregado com 40 vol% (500 g) de elementos de moagem (esferas de zircônia 3Y, HA, álcool isopropílico e ácido para-aminobenzóico), acoplados ao moinho rotatório (104 rpm, 48 h) seguido de moinho vibratório (72 h). Os produtos das técnicas de nanoparticulação foram caracterizados e a técnica de moagem foi utilizada para a síntese do compósito cerâmico experimental contendo sílica pirogênica e nano-HA de origem óssea bovina (SH). Os grupos foram conformados por compressão uniaxial/isostática, divididos em 3, 5 e 10 % de adição de HA, 1,2 e 2,4 % em peso de PVB e sinterizados à 1100, 1200 e 1300 °C para temperaturas máximas do platô (4 h). As caracterizações tanto dos métodos de nanoparticulaçõa, quanto do compósito cerâmico experimental foram realizadas por Microscopia Eletrônica de Transmissão (MET), Microscopia Eletrônica de Varredura (MEV), Espectroscopia de Energia Dispersiva de Raios-X (EDX), Difração de Raios-X (DRX) e Infravermelho por Transformada de Fourier (FTIR). Resultados: O tamanho inicial das partículas de HA foram em média 75 m e após as técnicas de sonicação e moinho de bolas foram de 60 nm e 40 nm, respectivamente. Ambas metodologias associadas à calcinação prévia, foram capazes de produzir partículas nanométricas de HA bovina, mantendo a estequiometria, morfologia e pureza adequadas. Com relação ao compósito cerâmico experimental SH, a compressão do pó foi um método eficiente. A temperatura de 1200 °C apresentou ligações químicas potencializadas sem a degradação do HA no perfil DRX. As imagens de MEV sugerem que 2,4 % em peso de PVB resultaram em uma melhor compactação e menor incidência de trincas e poros, e a proporção de 5 % de HA apresentou propriedades potencialmente superiores para o biomaterial. Conclusões: A técnica do moinho de bolas giratório e vibratório proporcionou uma maior redução das partículas de HA bovina e o compósito cerâmico experimental SH com 5 % de HA, 2,4 % em peso de PVB e sinterizado a 1200 °C apresentou propriedades potencialmente superiores para o biomaterial.Biblioteca Digitais de Teses e Dissertações da USPBorges, Ana Flávia SanchesRubo, Jose HenriqueFerrairo, Brunna Mota2021-01-28info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfhttps://www.teses.usp.br/teses/disponiveis/25/25146/tde-03122021-094954/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/openAccesseng2023-12-03T13:00:22Zoai:teses.usp.br:tde-03122021-094954Biblioteca 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:27212023-12-03T13:00:22Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)false
dc.title.none.fl_str_mv Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
Métodos de nanoparticulação da hidroxiapatita bovina, síntese e caracterização estrutural/química de um compósito cerâmico de SiO2/nano-hidroxiapatita experimental
title Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
spellingShingle Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
Ferrairo, Brunna Mota
Cerâmica
Cerâmica composta
Ceramics
Composite ceramic
Hidroxiapatita
Hydroxyapatite
Silica
Sílica
title_short Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
title_full Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
title_fullStr Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
title_full_unstemmed Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
title_sort Nanoparticulation methods of bovine hydroxyapatite, synthesis and structural/chemical characterization of an experimental SiO2/nanohydroxyapatite composite ceramic
author Ferrairo, Brunna Mota
author_facet Ferrairo, Brunna Mota
author_role author
dc.contributor.none.fl_str_mv Borges, Ana Flávia Sanches
Rubo, Jose Henrique
dc.contributor.author.fl_str_mv Ferrairo, Brunna Mota
dc.subject.por.fl_str_mv Cerâmica
Cerâmica composta
Ceramics
Composite ceramic
Hidroxiapatita
Hydroxyapatite
Silica
Sílica
topic Cerâmica
Cerâmica composta
Ceramics
Composite ceramic
Hidroxiapatita
Hydroxyapatite
Silica
Sílica
description Objectives: The aim of the study was to evaluate two methods of nanoparticulation methods of bovine hydroxyapatite (HA), synthesize an experimental SiO2/nano-hydroxyapatite composite ceramic and made a structurally and chemically characterization of them. Materials and Methods: Cortical of bovine femurs were selected and, after a pre-treatment, calcined and particulate. Sonication was performed with 40% of the maximum amplitude of 750W and 20Hz in aqueous solution added with HA and ammonia polyacrylate (4h of activation). Milling technique used a polyethylene jug (300 cm3) loaded with 40vol% (500g) milling elements (3Y zirconia balls, HA, isopropyl alcohol and para-aminobenzoic acid), placed in a rotatory mill (104rpm, 48h) followed by a vibratory mill (72h). Ball mill technique was used to mixture fumed silica and nano-HA from bovine bone source. Groups were divided into 3, 5 and 10% of HA addition, 1.2 and 2.4 wt.% of PVB, and 1100, 1200 and 1300 °C for maximum temperatures to firing plateau (4h). Characterization was performed by Transmission Electron Microscopy (TEM) / Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XDR) and Fourier Transform Infrared (FTIR). Results: The initial particle size is 75m and sonication (60 nm) and ball mill (40 nm) techniques, associated with prior calcination, were capable of producing nanosized bovine HA particles, maintaining an appropriate stoichiometry, morphology and purity. According to SH composite ceramic, the uniaxial/isostatic powder compression is an efficient method. The temperature of 1200 °C presented potentialized chemical bonds without the degradation of HA at XDR profile. SEM images suggests that 2.4 wt.% of PVB result in optimized compaction and a lower incidence of cracks and pores, and the SH composite ceramic with 5% of HA presents potential superior properties to biomaterial. Conclusion: The ball mill technique provided smaller particles of bovine hydroxyapatite and the experimental material SH composite ceramic with 5% of HA, 2.4 wt.% of PVB and sintered at 1200 °C presents potential superior properties to biomaterial.
publishDate 2021
dc.date.none.fl_str_mv 2021-01-28
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-03122021-094954/
url https://www.teses.usp.br/teses/disponiveis/25/25146/tde-03122021-094954/
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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