Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo

Detalhes bibliográficos
Ano de defesa: 2020
Autor(a) principal: Carvalho, Renata Gomes
Orientador(a): Tentardini, Eduardo Kirinus
Banca de defesa: Não Informado pela instituição
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/14756
Resumo: The objective of the present work was the Nb1-xAlxN thin films deposition in order to verify the Al concentration influence on microstructure, phase transitions evaluating, mechanical properties and corrosion resistance of these coatings in comparison to NbN. Thin films were obtained by reactive magnetron sputtering technique, and investigated with the following characterizations: Energy dispersive spectrometry (EDS) and Rutherford backscattering spectroscopy (RBS); Grazing Incidence X-ray Diffraction (GIXRD); X-ray photoelectron spectroscopy (XPS); Field Emission Gun Microscopy (SEM-FEG); nanohardness tests; high temperature oxidation tests; Electrochemical tests; Scanning Electron Microscope (SEM). Nb1-xAlxN thin films were obtained with 0 ≤ x ≤ 60. From GIXRD analyzes it was possible to observe that the cubic phase B1 of NbN is remains until 55 at.% Al concentration, suggesting a solid solution substitutional formation, from this concentration it is possible to observe a reduction in the material crystallinity, the critical content of AlN being verified for samples with Al contents greater than 60 at.%. The AlN phase nucleation on higher Al contents samples was also verified through calculations of crystallite size and parameter lattice. XPS analyzes suggest a solid solution formation up to a concentration of 40 at.% Al, from the micrographs obtained by SEM - FEG it was possible to verify the columnar grains formation on samples up to 40 at.% Al, a more microstructure dense was verified for Nb0.45Al0.55N and Nb0.40Al0.60N samples. The highest hardness values were found for Nb0.45Al0.55N and Nb0.40Al0.60N samples. Regarding the H3/E2 ratio, Nb0.45Al0.55N and Nb0.40Al0.60N samples were the ones with the highest values, 0.55 and 0.58 GPa, respectively. Electrochemical analyzes showed that NbN sample showed better behavior xi against corrosion when compared to samples of Nb1-xAlxN, with x ≤ 0.4. After SEM analysis of the surface, it was possible to verify that after the electrochemical tests all samples showed surface flaws, leading to pitting corrosion of the coatings. Oxidation tests on samples Nb0.45Al0.55N and Nb0.40Al0.60N were performed at temperatures of 700, 800 and 900° C, it was found that an increase in Al concentration did not improve the oxidation resistance of the studied samples.
id UFS-2_6222bc76b8edf2066557f0dc2f519998
oai_identifier_str oai:ufs.br:riufs/14756
network_acronym_str UFS-2
network_name_str Repositório Institucional da UFS
repository_id_str
spelling Carvalho, Renata GomesTentardini, Eduardo Kirinus2021-11-18T21:11:57Z2021-11-18T21:11:57Z2020-07-31CARVALHO, Renata Gomes. Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo. 2020. 113 f. Tese (Doutorado em Ciência e Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, SE, 2020.https://ri.ufs.br/jspui/handle/riufs/14756The objective of the present work was the Nb1-xAlxN thin films deposition in order to verify the Al concentration influence on microstructure, phase transitions evaluating, mechanical properties and corrosion resistance of these coatings in comparison to NbN. Thin films were obtained by reactive magnetron sputtering technique, and investigated with the following characterizations: Energy dispersive spectrometry (EDS) and Rutherford backscattering spectroscopy (RBS); Grazing Incidence X-ray Diffraction (GIXRD); X-ray photoelectron spectroscopy (XPS); Field Emission Gun Microscopy (SEM-FEG); nanohardness tests; high temperature oxidation tests; Electrochemical tests; Scanning Electron Microscope (SEM). Nb1-xAlxN thin films were obtained with 0 ≤ x ≤ 60. From GIXRD analyzes it was possible to observe that the cubic phase B1 of NbN is remains until 55 at.% Al concentration, suggesting a solid solution substitutional formation, from this concentration it is possible to observe a reduction in the material crystallinity, the critical content of AlN being verified for samples with Al contents greater than 60 at.%. The AlN phase nucleation on higher Al contents samples was also verified through calculations of crystallite size and parameter lattice. XPS analyzes suggest a solid solution formation up to a concentration of 40 at.% Al, from the micrographs obtained by SEM - FEG it was possible to verify the columnar grains formation on samples up to 40 at.% Al, a more microstructure dense was verified for Nb0.45Al0.55N and Nb0.40Al0.60N samples. The highest hardness values were found for Nb0.45Al0.55N and Nb0.40Al0.60N samples. Regarding the H3/E2 ratio, Nb0.45Al0.55N and Nb0.40Al0.60N samples were the ones with the highest values, 0.55 and 0.58 GPa, respectively. Electrochemical analyzes showed that NbN sample showed better behavior xi against corrosion when compared to samples of Nb1-xAlxN, with x ≤ 0.4. After SEM analysis of the surface, it was possible to verify that after the electrochemical tests all samples showed surface flaws, leading to pitting corrosion of the coatings. Oxidation tests on samples Nb0.45Al0.55N and Nb0.40Al0.60N were performed at temperatures of 700, 800 and 900° C, it was found that an increase in Al concentration did not improve the oxidation resistance of the studied samples.O presente trabalho teve como principal objetivo a deposição de filmes finos de Nb1- xAlxN para verificação da influência da concentração de Al em sua microestrutura, avaliando as transições de fase, as propriedades mecânicas e resistência à corrosão destes revestimentos em comparação ao NbN puro. Os filmes finos foram obtidos através da técnica de magnetron sputtering reativo, sendo investigados com as seguintes caracterizações: Espectroscopia de energia dispersiva (EDS) e Espectroscopia por Retroespalhamento Rutherford (RBS); Difração de raios X em ângulo rasante (GIXRD); Espectroscopia de Fotoelétrons Excitados por raios X (XPS); análises de Microscopia Eletrônica de Varredura em alta resolução (MEV-FEG); análises de nanodureza; testes de oxidação em altas temperaturas para amostras com concentração de Al acima de 40 at.%; análises de corrosão por polarização potenciodinâmica e Espectroscopia por Impedância Eletroquímica (EIE); análises de Microscopia Eletrônica de Varredura. Os filmes de Nb1-xAlxN foram obtidos com 0 ≤ x ≤ 60. A partir de análises de GIXRD foi possível observar que a fase cúbica B1 do NbN se mantém até a concentração de 55 at.% Al, sugerindo a presença de uma solução sólida substitucional, a partir desta concentração já é possível observar uma redução da cristalinidade do material, sendo o teor crítico de AlN verificado para amostras com teores de Al maiores que 60 at.%. A nucleação da fase AlN nas amostras com maiores teores de Al foi constatada também através dos cálculos de tamanho de cristalito e parâmetro de rede. Análises de XPS sugerem a formação de uma solução sólida até a concentração de 40 at.% Al, a partir das micrografias obtidas por MEV - FEG foi possível constatar a formação de grãos colunares para as amostras até 40 at.% Al, uma microestrutura mais ix densa foi verificada para as amostras Nb0.45Al0.55N e Nb0.40Al0.60N. Os maiores valores de dureza foram verificados para as amostras Nb0.45Al0.55N e Nb0.40Al0.60N. Com relação a razão H3 /E2 , as amostras Nb0.45Al0.55N e Nb0.40Al0.60N foram as que apresentaram os maiores valores, iguais a 0,55 e 0,58 GPa, respectivamente. Análises eletroquímicas mostraram que o revestimento de NbN puro apresentou melhor comportamento frente a corrosão quando comparado às amostras de Nb1-xAlxN, com x ≤ 0,4. Após análises de superfície por MEV foi possível constatar que após os testes eletroquímicos todas as amostras apresentaram falhas superficiais, levando à corrosão por pites dos revestimentos. Testes de oxidação nas amostras Nb0.45Al0.55N e Nb0.40Al0.60N foram realizados nas temperaturas de 700, 800 e 900° C, foi constatado que aumento da concentração de Al não melhorou a resistência à oxidação das amostras estudadas.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESSão Cristóvão, SEporEngenharia de materiaisCompostos de NióbioAlumínioFilmes finosCorrosãoNiobium nitrideAluminumSputteringCorrosion testsENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICADeposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativoinfo: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/14756/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALRENATA_GOMES_CARVALHO.pdfRENATA_GOMES_CARVALHO.pdfapplication/pdf4661457https://ri.ufs.br/jspui/bitstream/riufs/14756/2/RENATA_GOMES_CARVALHO.pdf3ed91b11de5d7fc863e86515c74d02d2MD52TEXTRENATA_GOMES_CARVALHO.pdf.txtRENATA_GOMES_CARVALHO.pdf.txtExtracted texttext/plain204863https://ri.ufs.br/jspui/bitstream/riufs/14756/3/RENATA_GOMES_CARVALHO.pdf.txtf90778e1a6507d7c0d31e604c37b3da4MD53THUMBNAILRENATA_GOMES_CARVALHO.pdf.jpgRENATA_GOMES_CARVALHO.pdf.jpgGenerated Thumbnailimage/jpeg1376https://ri.ufs.br/jspui/bitstream/riufs/14756/4/RENATA_GOMES_CARVALHO.pdf.jpg6e66a5920cdf3830592c40a1c5daf7adMD54riufs/147562021-11-18 18:11:57.164oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2021-11-18T21:11:57Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false
dc.title.pt_BR.fl_str_mv Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
title Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
spellingShingle Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
Carvalho, Renata Gomes
Engenharia de materiais
Compostos de Nióbio
Alumínio
Filmes finos
Corrosão
Niobium nitride
Aluminum
Sputtering
Corrosion tests
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
title_short Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
title_full Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
title_fullStr Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
title_full_unstemmed Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
title_sort Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
author Carvalho, Renata Gomes
author_facet Carvalho, Renata Gomes
author_role author
dc.contributor.author.fl_str_mv Carvalho, Renata Gomes
dc.contributor.advisor1.fl_str_mv Tentardini, Eduardo Kirinus
contributor_str_mv Tentardini, Eduardo Kirinus
dc.subject.por.fl_str_mv Engenharia de materiais
Compostos de Nióbio
Alumínio
Filmes finos
Corrosão
topic Engenharia de materiais
Compostos de Nióbio
Alumínio
Filmes finos
Corrosão
Niobium nitride
Aluminum
Sputtering
Corrosion tests
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
dc.subject.eng.fl_str_mv Niobium nitride
Aluminum
Sputtering
Corrosion tests
dc.subject.cnpq.fl_str_mv ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
description The objective of the present work was the Nb1-xAlxN thin films deposition in order to verify the Al concentration influence on microstructure, phase transitions evaluating, mechanical properties and corrosion resistance of these coatings in comparison to NbN. Thin films were obtained by reactive magnetron sputtering technique, and investigated with the following characterizations: Energy dispersive spectrometry (EDS) and Rutherford backscattering spectroscopy (RBS); Grazing Incidence X-ray Diffraction (GIXRD); X-ray photoelectron spectroscopy (XPS); Field Emission Gun Microscopy (SEM-FEG); nanohardness tests; high temperature oxidation tests; Electrochemical tests; Scanning Electron Microscope (SEM). Nb1-xAlxN thin films were obtained with 0 ≤ x ≤ 60. From GIXRD analyzes it was possible to observe that the cubic phase B1 of NbN is remains until 55 at.% Al concentration, suggesting a solid solution substitutional formation, from this concentration it is possible to observe a reduction in the material crystallinity, the critical content of AlN being verified for samples with Al contents greater than 60 at.%. The AlN phase nucleation on higher Al contents samples was also verified through calculations of crystallite size and parameter lattice. XPS analyzes suggest a solid solution formation up to a concentration of 40 at.% Al, from the micrographs obtained by SEM - FEG it was possible to verify the columnar grains formation on samples up to 40 at.% Al, a more microstructure dense was verified for Nb0.45Al0.55N and Nb0.40Al0.60N samples. The highest hardness values were found for Nb0.45Al0.55N and Nb0.40Al0.60N samples. Regarding the H3/E2 ratio, Nb0.45Al0.55N and Nb0.40Al0.60N samples were the ones with the highest values, 0.55 and 0.58 GPa, respectively. Electrochemical analyzes showed that NbN sample showed better behavior xi against corrosion when compared to samples of Nb1-xAlxN, with x ≤ 0.4. After SEM analysis of the surface, it was possible to verify that after the electrochemical tests all samples showed surface flaws, leading to pitting corrosion of the coatings. Oxidation tests on samples Nb0.45Al0.55N and Nb0.40Al0.60N were performed at temperatures of 700, 800 and 900° C, it was found that an increase in Al concentration did not improve the oxidation resistance of the studied samples.
publishDate 2020
dc.date.issued.fl_str_mv 2020-07-31
dc.date.accessioned.fl_str_mv 2021-11-18T21:11:57Z
dc.date.available.fl_str_mv 2021-11-18T21:11:57Z
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 CARVALHO, Renata Gomes. Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo. 2020. 113 f. Tese (Doutorado em Ciência e Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, SE, 2020.
dc.identifier.uri.fl_str_mv https://ri.ufs.br/jspui/handle/riufs/14756
identifier_str_mv CARVALHO, Renata Gomes. Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo. 2020. 113 f. Tese (Doutorado em Ciência e Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, SE, 2020.
url https://ri.ufs.br/jspui/handle/riufs/14756
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/14756/1/license.txt
https://ri.ufs.br/jspui/bitstream/riufs/14756/2/RENATA_GOMES_CARVALHO.pdf
https://ri.ufs.br/jspui/bitstream/riufs/14756/3/RENATA_GOMES_CARVALHO.pdf.txt
https://ri.ufs.br/jspui/bitstream/riufs/14756/4/RENATA_GOMES_CARVALHO.pdf.jpg
bitstream.checksum.fl_str_mv 098cbbf65c2c15e1fb2e49c5d306a44c
3ed91b11de5d7fc863e86515c74d02d2
f90778e1a6507d7c0d31e604c37b3da4
6e66a5920cdf3830592c40a1c5daf7ad
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_ 1793351125443805184