Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.

Detalhes bibliográficos
Autor(a) principal: Mazuco, Felipe de Sousa
Data de Publicação: 2021
Tipo de documento: Dissertação
Idioma: eng
Título da fonte: Biblioteca Digital de Teses e Dissertações da USP
Texto Completo: https://www.teses.usp.br/teses/disponiveis/3/3151/tde-20122021-121522/
Resumo: The main restriction in the application of thick hydrogen-free amorphous carbon (a-C) coatings is the adhesion to the substrate, since high compressive stresses tend to delaminate the coating when a certain thickness is reached. In the present work, amorphous carbon films were deposited by unfiltered cathodic arc over a gas nitrided stainless steel substrate with metallic chromium as bond layer. An additional step was included, where carbon ions were accelerated by high bias potential before the deposition of functional a-C, to produce a carbon transition layer to act as a buffer layer. During a preliminary analysis, different thicknesses of this transition layer were produced, including a sample without this step, for reference purposes. The coating adhesion was evaluated by scratch test. In addition, the microstructure of the interface was analyzed by scanning transmission electron microscopy (STEM) and the sp-type bonds were quantified by electron energy loss spectroscopy (EELS). The analysis of the microstructure close to the interface with the chromium bond layer revealed a mixing layer of Cr and C. Furthermore, it was observed the formation of the transition layer characterized by a homogeneous carbon layer with high sp2 content, when compared to the functional amorphous carbon layer. Results indicate a significant enhancement of adhesion for the samples prepared with the carbon bombardment step, which can be correlated to the presence of the mixing layer and the carbon transition layer. Moreover, a decrease in adhesion was observed for an increase in the thickness of the transition layer, which can be attributed to the lower shear strength of this sp2 rich layer. In a second phase, three sets of experiments were designed to optimize the carbon bombardment step. The parameters studied were the duration combined with the bias voltage, the cathode current and the temperature. It was found that not only the thickness of the carbon transition layer is important for the adhesion but also the sp3 content. For instance, a lower bias voltage was able to increase the sp3 content of the carbon transition layer mitigating the negative impact of a thicker carbon transition layer. Also, an increase in the carbon cathode current could increase the adhesion possibly by extending the mixing layer. Finally, the best adhesion result was achieved when the substrate temperature of the bombardment was reduced. The most probable cause for that is a compositional modification in the mixing layer, like a change in the carbides formed in that region.
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spelling Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.Melhoria de adesão de recobrimentos espessos de DLC produzidos por evaporação por arco catódico sobre aço inoxidável utilizando etapa de bombardeamento de carbono.AdesãoAdhesionAmorphous carbonCathodic arcInterface analysisMateriaisMateriais nanoestruturadosRecobrimento espessosScratch testThick DLC coatingsThe main restriction in the application of thick hydrogen-free amorphous carbon (a-C) coatings is the adhesion to the substrate, since high compressive stresses tend to delaminate the coating when a certain thickness is reached. In the present work, amorphous carbon films were deposited by unfiltered cathodic arc over a gas nitrided stainless steel substrate with metallic chromium as bond layer. An additional step was included, where carbon ions were accelerated by high bias potential before the deposition of functional a-C, to produce a carbon transition layer to act as a buffer layer. During a preliminary analysis, different thicknesses of this transition layer were produced, including a sample without this step, for reference purposes. The coating adhesion was evaluated by scratch test. In addition, the microstructure of the interface was analyzed by scanning transmission electron microscopy (STEM) and the sp-type bonds were quantified by electron energy loss spectroscopy (EELS). The analysis of the microstructure close to the interface with the chromium bond layer revealed a mixing layer of Cr and C. Furthermore, it was observed the formation of the transition layer characterized by a homogeneous carbon layer with high sp2 content, when compared to the functional amorphous carbon layer. Results indicate a significant enhancement of adhesion for the samples prepared with the carbon bombardment step, which can be correlated to the presence of the mixing layer and the carbon transition layer. Moreover, a decrease in adhesion was observed for an increase in the thickness of the transition layer, which can be attributed to the lower shear strength of this sp2 rich layer. In a second phase, three sets of experiments were designed to optimize the carbon bombardment step. The parameters studied were the duration combined with the bias voltage, the cathode current and the temperature. It was found that not only the thickness of the carbon transition layer is important for the adhesion but also the sp3 content. For instance, a lower bias voltage was able to increase the sp3 content of the carbon transition layer mitigating the negative impact of a thicker carbon transition layer. Also, an increase in the carbon cathode current could increase the adhesion possibly by extending the mixing layer. Finally, the best adhesion result was achieved when the substrate temperature of the bombardment was reduced. The most probable cause for that is a compositional modification in the mixing layer, like a change in the carbides formed in that region.A principal restrição na aplicação de revestimentos espessos de carbono amorfo como diamante livre de hidrogênio (em inglês a-C amorphous carbon) é a adesão ao substrato, uma vez que as altas tensões internas tendem a delaminar o revestimento quando uma certa espessura é alcançada. Neste trabalho, um filme de carbono amorfo (a-C) foi depositado por arco catódico não filtrado sobre um substrato de aço inoxidável nitretado a gás com Cr metálico como camada de ligação. Foi incluído um passo adicional em que os íons de carbono foram acelerados por alto potencial de polarização antes da deposição do recobrimento funcional de a-C, para produzir uma camada de transição de carbono. Durante a primeira fase do trabalho, diferentes espessuras desta camada de transição foram produzidas, incluindo uma amostra sem esta etapa, para fins de referência. A adesão do revestimento foi avaliada por teste de riscamento (esclerometria). Além disso, a microestrutura da interface foi analisada por microscopia eletrônica de transmissão no modo varredura (STEM) e as ligações do tipo sp3/sp2 foram quantificadas por espectroscopia de perda de energia de elétrons (EELS). A análise da microestrutura próxima à interface com a camada intermediária de Cr revelou uma camada mista composta por Cr e C. Além disso, observou-se a formação da camada de transição caracterizada por uma camada de carbono homogênea com alto teor de sp2, quando comparado ao a-C funcional. Os resultados indicam um aumento significativo da adesão nas amostras de a-C preparadas com o passo de bombardeamento de carbono, o que pode ser correlacionado com a presença da camada mista e da camada de transição de carbono. Além disso, observou-se diminuição da adesão para aumento da espessura da camada de transição, o que pode ser atribuído à menor resistência ao cisalhamento desta camada rica em sp2. Em uma segunda fase do trabalho, três conjuntos de experimentos foram projetados para otimizar a etapa de bombardeamento por carbono. Os parâmetros estudados foram a duração em combinação com voltagem de polarização, a corrente de cátodo e a temperatura. Foi encontrado que, além da espessura da camada de transição, a quantidade de ligações sp3 também é importante para a adesão. Por exemplo, uma menor tensão de polarização foi responsável pelo aumento da quantidade de ligações sp3 presentes na camada de transição de carbono, mitigando o impacto negativo de uma camada de transição mais espessa. Também, um aumento na corrente de cátodo de carbono pode aumentar a adesão, possivelmente pelo aumento da camada mista. Finalmente, o melhor resultado de adesão foi alcançado quando a temperatura do substrato durante o bombardeamento foi reduzida. A causa mais provável para esse efeito é a modificação química da camada mista, como uma mudança nos carbonetos formados nessa região.Biblioteca Digitais de Teses e Dissertações da USPSouza, Roberto Martins deMazuco, Felipe de Sousa2021-09-23info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttps://www.teses.usp.br/teses/disponiveis/3/3151/tde-20122021-121522/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/openAccesseng2024-10-09T13:16:04Zoai:teses.usp.br:tde-20122021-121522Biblioteca 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:27212024-10-09T13:16:04Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)false
dc.title.none.fl_str_mv Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
Melhoria de adesão de recobrimentos espessos de DLC produzidos por evaporação por arco catódico sobre aço inoxidável utilizando etapa de bombardeamento de carbono.
title Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
spellingShingle Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
Mazuco, Felipe de Sousa
Adesão
Adhesion
Amorphous carbon
Cathodic arc
Interface analysis
Materiais
Materiais nanoestruturados
Recobrimento espessos
Scratch test
Thick DLC coatings
title_short Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
title_full Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
title_fullStr Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
title_full_unstemmed Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
title_sort Adhesion improvement of thick DLC coatings produced by cathodic arc evaporation over stainless steel using carbon bombardment step.
author Mazuco, Felipe de Sousa
author_facet Mazuco, Felipe de Sousa
author_role author
dc.contributor.none.fl_str_mv Souza, Roberto Martins de
dc.contributor.author.fl_str_mv Mazuco, Felipe de Sousa
dc.subject.por.fl_str_mv Adesão
Adhesion
Amorphous carbon
Cathodic arc
Interface analysis
Materiais
Materiais nanoestruturados
Recobrimento espessos
Scratch test
Thick DLC coatings
topic Adesão
Adhesion
Amorphous carbon
Cathodic arc
Interface analysis
Materiais
Materiais nanoestruturados
Recobrimento espessos
Scratch test
Thick DLC coatings
description The main restriction in the application of thick hydrogen-free amorphous carbon (a-C) coatings is the adhesion to the substrate, since high compressive stresses tend to delaminate the coating when a certain thickness is reached. In the present work, amorphous carbon films were deposited by unfiltered cathodic arc over a gas nitrided stainless steel substrate with metallic chromium as bond layer. An additional step was included, where carbon ions were accelerated by high bias potential before the deposition of functional a-C, to produce a carbon transition layer to act as a buffer layer. During a preliminary analysis, different thicknesses of this transition layer were produced, including a sample without this step, for reference purposes. The coating adhesion was evaluated by scratch test. In addition, the microstructure of the interface was analyzed by scanning transmission electron microscopy (STEM) and the sp-type bonds were quantified by electron energy loss spectroscopy (EELS). The analysis of the microstructure close to the interface with the chromium bond layer revealed a mixing layer of Cr and C. Furthermore, it was observed the formation of the transition layer characterized by a homogeneous carbon layer with high sp2 content, when compared to the functional amorphous carbon layer. Results indicate a significant enhancement of adhesion for the samples prepared with the carbon bombardment step, which can be correlated to the presence of the mixing layer and the carbon transition layer. Moreover, a decrease in adhesion was observed for an increase in the thickness of the transition layer, which can be attributed to the lower shear strength of this sp2 rich layer. In a second phase, three sets of experiments were designed to optimize the carbon bombardment step. The parameters studied were the duration combined with the bias voltage, the cathode current and the temperature. It was found that not only the thickness of the carbon transition layer is important for the adhesion but also the sp3 content. For instance, a lower bias voltage was able to increase the sp3 content of the carbon transition layer mitigating the negative impact of a thicker carbon transition layer. Also, an increase in the carbon cathode current could increase the adhesion possibly by extending the mixing layer. Finally, the best adhesion result was achieved when the substrate temperature of the bombardment was reduced. The most probable cause for that is a compositional modification in the mixing layer, like a change in the carbides formed in that region.
publishDate 2021
dc.date.none.fl_str_mv 2021-09-23
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
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dc.language.iso.fl_str_mv eng
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dc.rights.driver.fl_str_mv Liberar o conteúdo para acesso público.
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eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
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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
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reponame:Biblioteca Digital de Teses e Dissertações da USP
instname:Universidade de São Paulo (USP)
instacron:USP
instname_str Universidade de São Paulo (USP)
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reponame_str Biblioteca Digital de Teses e Dissertações da USP
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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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