Deposição e caracterização microestrutural, dureza e corrosão de filmes finos de BbN/AIN depositados por magnetron sputtering reativo
Autor(a) principal: | |
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Data de Publicação: | 2020 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFS |
Texto Completo: | 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. |
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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 |
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Pós-Graduação em Ciência e Engenharia de Materiais |
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Universidade Federal de Sergipe |
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