Efeito do manganês sobre a estrutura cristalina da hidroxiapatita
Ano de defesa: | 2021 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | |
Tipo de documento: | Tese |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Não Informado pela instituição
|
Programa de Pós-Graduação: |
Pós-Graduação em Ciência e Engenharia de Materiais
|
Departamento: |
Não Informado pela instituição
|
País: |
Não Informado pela instituição
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://ri.ufs.br/jspui/handle/riufs/15077 |
Resumo: | Manganese (Mn) can develop magnetic properties in substituted hydroxyapatites (HA), as well as iron, copper, cobalt and samarium, but with the advantage of controlling several cellular activities. The occupation of the HA sites by Mn and its segregation from HA structure during heat treatments can affect magnetic properties. For this reason, the objective of this work was to study the accommodation of Mn into a carbonated HA, and its segregation mechanism at temperatures above 800°C yielding Mn3O4 nanoparticles. HAs with five different concentrations of Mn in relation to calcium were synthesized by the aqueous precipitation method: (Mn/(Mn+Ca) = 0, 5, 10, 15 and 20 at. %. Using wavelength dispersion X-ray fluorescence, X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy, it was possible to demonstrate that Mn was inserted into the HA structure in all concentrations, strongly compromising its crystalline structure. The regions around the hydroxyl channels were affected the most, with clear evidence of preferential Ca2 sites occupation, especially in the samples with a high content of CO3 2- replacing PO4 3- . When carbonate was released at high temperature and the crystallinity increased, the Ca1 sites seemed more susceptible to occupation by Mn. At temperatures above 1000°C, Mn segregated from the HA structure in the form of Mn3O4 nanoparticles, via hydroxyl channels, preferentially occupying Ca2 sites at the final segregation stage. The presence of Mn in several oxidation states also suggested that, in addition to the cationic substitutions, there were also anionic substitutions such as MnO4 3- at the PO4 3- sites. No cytotoxicity was detected for the lower concentration of Mn regarding osteoblastic cells. These results contributed to clarify the Mn behavior into HA and its segregation, being fundamental to the development of new strategies to synthesize magnetic-active hydroxyapatite-based scaffolds in the future. |
id |
UFS-2_0e3c8911c9505ddc64884137aa917db6 |
---|---|
oai_identifier_str |
oai:ufs.br:riufs/15077 |
network_acronym_str |
UFS-2 |
network_name_str |
Repositório Institucional da UFS |
repository_id_str |
|
spelling |
Oliveira Júnior, Paulo HenriqueSantos, Euler Araujo dosFerreira, Nilson dos Santos2022-02-24T21:50:53Z2022-02-24T21:50:53Z2021-04-28OLIVEIRA JUNIOR, Paulo Henrique. Efeito do manganês sobre a estrutura cristalina da hidroxiapatita. 2021. 105 f. Tese (Doutorado em Ciência e Engenharia de Materiais) – Universidade Federal de Sergipe, São Cristóvão, 2021.https://ri.ufs.br/jspui/handle/riufs/15077Manganese (Mn) can develop magnetic properties in substituted hydroxyapatites (HA), as well as iron, copper, cobalt and samarium, but with the advantage of controlling several cellular activities. The occupation of the HA sites by Mn and its segregation from HA structure during heat treatments can affect magnetic properties. For this reason, the objective of this work was to study the accommodation of Mn into a carbonated HA, and its segregation mechanism at temperatures above 800°C yielding Mn3O4 nanoparticles. HAs with five different concentrations of Mn in relation to calcium were synthesized by the aqueous precipitation method: (Mn/(Mn+Ca) = 0, 5, 10, 15 and 20 at. %. Using wavelength dispersion X-ray fluorescence, X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy, it was possible to demonstrate that Mn was inserted into the HA structure in all concentrations, strongly compromising its crystalline structure. The regions around the hydroxyl channels were affected the most, with clear evidence of preferential Ca2 sites occupation, especially in the samples with a high content of CO3 2- replacing PO4 3- . When carbonate was released at high temperature and the crystallinity increased, the Ca1 sites seemed more susceptible to occupation by Mn. At temperatures above 1000°C, Mn segregated from the HA structure in the form of Mn3O4 nanoparticles, via hydroxyl channels, preferentially occupying Ca2 sites at the final segregation stage. The presence of Mn in several oxidation states also suggested that, in addition to the cationic substitutions, there were also anionic substitutions such as MnO4 3- at the PO4 3- sites. No cytotoxicity was detected for the lower concentration of Mn regarding osteoblastic cells. These results contributed to clarify the Mn behavior into HA and its segregation, being fundamental to the development of new strategies to synthesize magnetic-active hydroxyapatite-based scaffolds in the future.O manganês (Mn) pode desenvolver propriedades magnéticas em hidroxiapatitas (HA) substituídas, assim como o ferro, cobre, cobalto e samário, mas com a vantagem de também controlar diversas atividades celulares. O tipo e grau de ocupação dos sítios da HA e a possibilidade de segregação de óxidos desses elementos durante tratamentos térmicos definem as propriedades magnéticas resultantes. Por essa razão, o objetivo desse trabalho foi estudar de forma preliminar como ocorre a acomodação do Mn nos sítios de uma HA carbonatada, bem como seu mecanismo de segregação em temperaturas acima de 800°C com a formação de nanopartículas de Mn3O4. Para isso, HAs com cinco diferentes concentrações de Mn em relação ao cálcio foram sintetizadas pelo método de precipitação em meio aquoso: (Mn/(Mn+Ca) = 0, 5, 10, 15 e 20 % at. Usando-se fluorescência de raios X por dispersão de comprimento de onda, difração de raios X, espectroscopia no infravermelho com transformada de Fourier, microscopia eletrônica de transmissão e espectroscopia de fotoelétrons de raios X, ficou demonstrando que o Mn foi inserido na estrutura da HA para todas as concentrações, perturbando consideravelmente a sua estrutura cristalina. As regiões dos canais hexagonais de hidroxila sofreram as maiores perturbações, com evidências de ocupação preferencial dos sítios de Ca2, principalmente para as amostras verdes com alto teor de CO3 2- em substituição ao PO4 3- . Quando o CO3 2- é liberado em alta temperatura e a cristalinidade aumenta, os sítios de Ca1 parecem mais suscetíveis à ocupação por Mn. Em temperaturas acima de 1000°C, o Mn tendeu a ser segregado da estrutura da HA na forma de nanopartículas de Mn3O4, via canais de hidroxila, ocupando preferencialmente sítios de Ca2 no estágio final da segregação. A presença de Mn em diversos estados de oxidação também sugeriu que, além das substituições catiônicas, ocorreram também substituições aniônicas de MnO4 3- nos sítios de PO4 3- . Na sua concentração mais baixa, o Mn não apresentou citotoxicidade frente a osteoblastos humanos. Esses resultados são essenciais na compreensão do comportamento do Mn na HA e sua segregação, sendo fundamental para o desenvolvimento de novas estratégias para a produção de arcabouços magnéticos ativos baseados em hidroxiapatita no futuro.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESSão CristóvãoporCiência dos materiaisHidroxiapatitaÓxidos de manganêsNanopartículas magnéticasHidroxiapatitaÓxido de manganêsNanopartículas magnéticasEstrutura cristalinaHydroxyapatiteManganese oxideMagnetic nanoparticlesCrystalline structureENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICAEfeito do manganês sobre a estrutura cristalina da hidroxiapatitaEffect of manganese on the crystalline structure of hydroxiapatiteinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisPós-Graduação em Ciência e Engenharia de MateriaisUniversidade Federal de Sergipereponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessLICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/15077/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALPAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdfPAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdfapplication/pdf7392620https://ri.ufs.br/jspui/bitstream/riufs/15077/2/PAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf1826e981efaaddf0a47a46ebccb55aa7MD52TEXTPAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.txtPAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.txtExtracted texttext/plain152186https://ri.ufs.br/jspui/bitstream/riufs/15077/3/PAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.txtb6629884542110d4a94c221b296fa514MD53THUMBNAILPAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.jpgPAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.jpgGenerated Thumbnailimage/jpeg1221https://ri.ufs.br/jspui/bitstream/riufs/15077/4/PAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.jpge886d0c65ca5ae937941a596e7d1b760MD54riufs/150772022-02-24 18:50:53.377oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2022-02-24T21:50:53Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false |
dc.title.pt_BR.fl_str_mv |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
dc.title.alternative.eng.fl_str_mv |
Effect of manganese on the crystalline structure of hydroxiapatite |
title |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
spellingShingle |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita Oliveira Júnior, Paulo Henrique Ciência dos materiais Hidroxiapatita Óxidos de manganês Nanopartículas magnéticas Hidroxiapatita Óxido de manganês Nanopartículas magnéticas Estrutura cristalina Hydroxyapatite Manganese oxide Magnetic nanoparticles Crystalline structure ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
title_short |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
title_full |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
title_fullStr |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
title_full_unstemmed |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
title_sort |
Efeito do manganês sobre a estrutura cristalina da hidroxiapatita |
author |
Oliveira Júnior, Paulo Henrique |
author_facet |
Oliveira Júnior, Paulo Henrique |
author_role |
author |
dc.contributor.author.fl_str_mv |
Oliveira Júnior, Paulo Henrique |
dc.contributor.advisor1.fl_str_mv |
Santos, Euler Araujo dos |
dc.contributor.advisor-co1.fl_str_mv |
Ferreira, Nilson dos Santos |
contributor_str_mv |
Santos, Euler Araujo dos Ferreira, Nilson dos Santos |
dc.subject.por.fl_str_mv |
Ciência dos materiais Hidroxiapatita Óxidos de manganês Nanopartículas magnéticas Hidroxiapatita Óxido de manganês Nanopartículas magnéticas Estrutura cristalina |
topic |
Ciência dos materiais Hidroxiapatita Óxidos de manganês Nanopartículas magnéticas Hidroxiapatita Óxido de manganês Nanopartículas magnéticas Estrutura cristalina Hydroxyapatite Manganese oxide Magnetic nanoparticles Crystalline structure ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
dc.subject.eng.fl_str_mv |
Hydroxyapatite Manganese oxide Magnetic nanoparticles Crystalline structure |
dc.subject.cnpq.fl_str_mv |
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
description |
Manganese (Mn) can develop magnetic properties in substituted hydroxyapatites (HA), as well as iron, copper, cobalt and samarium, but with the advantage of controlling several cellular activities. The occupation of the HA sites by Mn and its segregation from HA structure during heat treatments can affect magnetic properties. For this reason, the objective of this work was to study the accommodation of Mn into a carbonated HA, and its segregation mechanism at temperatures above 800°C yielding Mn3O4 nanoparticles. HAs with five different concentrations of Mn in relation to calcium were synthesized by the aqueous precipitation method: (Mn/(Mn+Ca) = 0, 5, 10, 15 and 20 at. %. Using wavelength dispersion X-ray fluorescence, X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy, it was possible to demonstrate that Mn was inserted into the HA structure in all concentrations, strongly compromising its crystalline structure. The regions around the hydroxyl channels were affected the most, with clear evidence of preferential Ca2 sites occupation, especially in the samples with a high content of CO3 2- replacing PO4 3- . When carbonate was released at high temperature and the crystallinity increased, the Ca1 sites seemed more susceptible to occupation by Mn. At temperatures above 1000°C, Mn segregated from the HA structure in the form of Mn3O4 nanoparticles, via hydroxyl channels, preferentially occupying Ca2 sites at the final segregation stage. The presence of Mn in several oxidation states also suggested that, in addition to the cationic substitutions, there were also anionic substitutions such as MnO4 3- at the PO4 3- sites. No cytotoxicity was detected for the lower concentration of Mn regarding osteoblastic cells. These results contributed to clarify the Mn behavior into HA and its segregation, being fundamental to the development of new strategies to synthesize magnetic-active hydroxyapatite-based scaffolds in the future. |
publishDate |
2021 |
dc.date.issued.fl_str_mv |
2021-04-28 |
dc.date.accessioned.fl_str_mv |
2022-02-24T21:50:53Z |
dc.date.available.fl_str_mv |
2022-02-24T21:50:53Z |
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.citation.fl_str_mv |
OLIVEIRA JUNIOR, Paulo Henrique. Efeito do manganês sobre a estrutura cristalina da hidroxiapatita. 2021. 105 f. Tese (Doutorado em Ciência e Engenharia de Materiais) – Universidade Federal de Sergipe, São Cristóvão, 2021. |
dc.identifier.uri.fl_str_mv |
https://ri.ufs.br/jspui/handle/riufs/15077 |
identifier_str_mv |
OLIVEIRA JUNIOR, Paulo Henrique. Efeito do manganês sobre a estrutura cristalina da hidroxiapatita. 2021. 105 f. Tese (Doutorado em Ciência e Engenharia de Materiais) – Universidade Federal de Sergipe, São Cristóvão, 2021. |
url |
https://ri.ufs.br/jspui/handle/riufs/15077 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.publisher.program.fl_str_mv |
Pós-Graduação em Ciência e Engenharia de Materiais |
dc.publisher.initials.fl_str_mv |
Universidade Federal de Sergipe |
dc.source.none.fl_str_mv |
reponame:Repositório Institucional da UFS instname:Universidade Federal de Sergipe (UFS) instacron:UFS |
instname_str |
Universidade Federal de Sergipe (UFS) |
instacron_str |
UFS |
institution |
UFS |
reponame_str |
Repositório Institucional da UFS |
collection |
Repositório Institucional da UFS |
bitstream.url.fl_str_mv |
https://ri.ufs.br/jspui/bitstream/riufs/15077/1/license.txt https://ri.ufs.br/jspui/bitstream/riufs/15077/2/PAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf https://ri.ufs.br/jspui/bitstream/riufs/15077/3/PAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.txt https://ri.ufs.br/jspui/bitstream/riufs/15077/4/PAULO_HENRIQUE_OLIVEIRA_JUNIOR.pdf.jpg |
bitstream.checksum.fl_str_mv |
098cbbf65c2c15e1fb2e49c5d306a44c 1826e981efaaddf0a47a46ebccb55aa7 b6629884542110d4a94c221b296fa514 e886d0c65ca5ae937941a596e7d1b760 |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS) |
repository.mail.fl_str_mv |
repositorio@academico.ufs.br |
_version_ |
1793351065310068736 |