Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia

Detalhes bibliográficos
Autor(a) principal: Silva, Francisco Iran Sousa da
Data de Publicação: 2018
Tipo de documento: Tese
Idioma: por
Título da fonte: Repositório Institucional da Universidade Federal do Ceará (UFC)
Texto Completo: http://www.repositorio.ufc.br/handle/riufc/37974
Resumo: This thesis presents studies on Fe-30Mn-6Si shape memory alloys produced by high energy mechanical milling. Elemental powders of iron, manganese and silicon were processed in a planetary mill with a rotational speed of 500 rpm with milling times of 1 to 10 h. X-ray diffractograms showed the evolution of the various crystallographic phases present in the material. A single FeMnSi austenitic phase with nanometric crystalline size is found at 4 h of milling time. This phase is stable up to 10 h of milling. Mössbauer spectra showed the existence of a ferromagnetic sextet and a paramagnetic singlet at the beginning of the milling process. During the course of grinding the sextet is replaced by the singlet. Only the paramagnetic singlet associated to the FeMnSi austenitic phase is seen from 4 h to 10 h. Scanning electron microscopy and granulometry results showed that the samples are not homogeneous and have particle sizes in the micrometer range. The powder sample milling for 4 h was compacted and sintered to produce cylinders with a height of 11 mm and a diameter of 8 mm. The sintered cylinders were subjected to compression deformation and subsequent heat treatment for shape recovery. X-ray diffraction results showed the presence of γ austenite phase and of a small fraction of ε martensite with HCP structure in the sintered cylinder. The diffractogram of the deformed sample showed that a large fraction of austenite was transformed into martensite. After heat treatment it was observed that part of the martensite phase was transformed back into austenite. The Mössbauer spectra of these samples showed that the Fe atoms are found in more than one paramagnetic environment, which is consistent with the results of X-ray diffraction. Scanning electron microscopy revealed the presence of pores created by the cylinder manufacturing process. Values of hardness can be associated to the porosity of the samples. Corrosion tests showed that the deformed sample showed the best corrosion performance, which is attributed to the higher presence of martensite in this sample. Deformation and shape recovery tests led to an elastic recovery of 5.3% after removal of the compressive load and a plastic recovery of 0.9% after the heat treatment, resulting in a total recovery of 6.2%. These results provide evidence that the shape memory effect occurs both after mechanical relief as well as after heat treatment. The plastic recovery effect is associated with ε − γ transformation observed by X-ray diffraction. The plastic recovery around 0.9% after the heat treatment obtained in this study is consistent with results previously reported for FeMnSi alloys with similar chemical composition.
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spelling Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energiaSynthesis and characterization of Fe-Mn-Si alloys with shape memory effect obtained by high energy mechanical millingCiência dos materiaisLigas de açoMoagem de alta energiaLigas com memória de formaShape memoryMechanical millingThis thesis presents studies on Fe-30Mn-6Si shape memory alloys produced by high energy mechanical milling. Elemental powders of iron, manganese and silicon were processed in a planetary mill with a rotational speed of 500 rpm with milling times of 1 to 10 h. X-ray diffractograms showed the evolution of the various crystallographic phases present in the material. A single FeMnSi austenitic phase with nanometric crystalline size is found at 4 h of milling time. This phase is stable up to 10 h of milling. Mössbauer spectra showed the existence of a ferromagnetic sextet and a paramagnetic singlet at the beginning of the milling process. During the course of grinding the sextet is replaced by the singlet. Only the paramagnetic singlet associated to the FeMnSi austenitic phase is seen from 4 h to 10 h. Scanning electron microscopy and granulometry results showed that the samples are not homogeneous and have particle sizes in the micrometer range. The powder sample milling for 4 h was compacted and sintered to produce cylinders with a height of 11 mm and a diameter of 8 mm. The sintered cylinders were subjected to compression deformation and subsequent heat treatment for shape recovery. X-ray diffraction results showed the presence of γ austenite phase and of a small fraction of ε martensite with HCP structure in the sintered cylinder. The diffractogram of the deformed sample showed that a large fraction of austenite was transformed into martensite. After heat treatment it was observed that part of the martensite phase was transformed back into austenite. The Mössbauer spectra of these samples showed that the Fe atoms are found in more than one paramagnetic environment, which is consistent with the results of X-ray diffraction. Scanning electron microscopy revealed the presence of pores created by the cylinder manufacturing process. Values of hardness can be associated to the porosity of the samples. Corrosion tests showed that the deformed sample showed the best corrosion performance, which is attributed to the higher presence of martensite in this sample. Deformation and shape recovery tests led to an elastic recovery of 5.3% after removal of the compressive load and a plastic recovery of 0.9% after the heat treatment, resulting in a total recovery of 6.2%. These results provide evidence that the shape memory effect occurs both after mechanical relief as well as after heat treatment. The plastic recovery effect is associated with ε − γ transformation observed by X-ray diffraction. The plastic recovery around 0.9% after the heat treatment obtained in this study is consistent with results previously reported for FeMnSi alloys with similar chemical composition.Esta tese apresenta estudos feitos em ligas Fe-30Mn-6Si com efeito memória de forma produzidas por moagem mecânica de altas energias. Pós elementares de ferro, manganês e silício foram processados em moinho planetário com velocidade de rotação de 500 rpm com tempo de 1 a 10 h de moagem. Os difratogramas de raios-X mostraram a evolução das várias fases cristalográficas presentes no material. A partir de 4 h de moagem só há a presença de uma única fase austenítica FeMnSi com tamanho de cristalino nanométrico. Esta fase se mantém estável até 10 h de moagem. Os espectros Mössbauer mostraram a existência de um sexteto ferromagnético e de um singleto paramagnético no início da moagem. Durante o curso da moagem o sexteto é substituı́do pelo singleto. A partir de 4 h de moagem o sexteto desaparece, permanecendo somente o singleto paramagnético associado à fase austenítica FeMnSi. Resultados de microscopia eletrônica de varredura e granulometria mostraram que as amostras não são homogêneas e que apresentam tamanhos de partícula na faixa dos micrômetros. A amostra em pó moída por 4 horas foi compactada e sinterizada para produzir cilindros com altura de 11 mm e diâmetro de 8 mm. Os cilindros sinterizados foram submetidos a deformação por compressão e posterior tratamento térmico para recuperação de forma. Resultados de difração de raios-X mostraram a presença da fase austenita γ além de uma pequena fração da fase martensita ε coestrutura HCP no cilindro sinterizado. O difratograma da amostra deformada mostrou que grande parte do volume da fase austenita γ foi transformado em martensita ε. Após o tratamento térmico foi observado que parte da fase martensita ε foi transformada de volta em austenita γ. Os espectros Mössbauer dessas amostras mostraram que os átomos de Fe se encontram em mais de um ambiente paramagnético, o que é consistente com os resultados de difração de raios-X. Microscopia eletrônica de varredura revelou presença de poros provenientes do processo de fabricação dos cilindros. Valores de dureza obtidos estão relacionados com a porosidade das amostras. Ensaios de corrosão mostraram que amostra deformada apresentou o melhor desempenho à corrosão, o que é atribuído à maior presença de martensita ε nesta amostra. Ensaios de deformação e recuperação de forma levaram a uma recuperação elástica de 5,3% após retirada da carga compressiva e uma recuperação plástica de 0,9% após o tratamento térmico, perfazendo uma recuperação total de 6,2%. Estes resultados fornecem evidências de que o efeito de memória de forma ocorre tanto após o alívio mecânico, bem como após o tratamento térmico. O efeito de recuperação plástica está associado a transformação ε − γ observada por difração de raios-X. A recuperação plástica em torno de 0,9% após o tratamento térmico obtido neste estudo é consistente com resultados reportados anteriormente para ligas FeMnSi com composição quıímica similar.Vasconcelos, Igor Frota deSilva, Francisco Iran Sousa da2018-12-11T11:36:54Z2018-12-11T11:36:54Z2018info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfSILVA, F. I. S. da. Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia. 2018. 93 f. Tese (Doutorado em Engenharia e Ciência de Materiais)-Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2018.http://www.repositorio.ufc.br/handle/riufc/37974porreponame:Repositório Institucional da Universidade Federal do Ceará (UFC)instname:Universidade Federal do Ceará (UFC)instacron:UFCinfo:eu-repo/semantics/openAccess2020-08-25T15:09:12Zoai:repositorio.ufc.br:riufc/37974Repositório InstitucionalPUBhttp://www.repositorio.ufc.br/ri-oai/requestbu@ufc.br || repositorio@ufc.bropendoar:2024-09-11T18:55:04.917882Repositório Institucional da Universidade Federal do Ceará (UFC) - Universidade Federal do Ceará (UFC)false
dc.title.none.fl_str_mv Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
Synthesis and characterization of Fe-Mn-Si alloys with shape memory effect obtained by high energy mechanical milling
title Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
spellingShingle Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
Silva, Francisco Iran Sousa da
Ciência dos materiais
Ligas de aço
Moagem de alta energia
Ligas com memória de forma
Shape memory
Mechanical milling
title_short Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
title_full Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
title_fullStr Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
title_full_unstemmed Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
title_sort Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia
author Silva, Francisco Iran Sousa da
author_facet Silva, Francisco Iran Sousa da
author_role author
dc.contributor.none.fl_str_mv Vasconcelos, Igor Frota de
dc.contributor.author.fl_str_mv Silva, Francisco Iran Sousa da
dc.subject.por.fl_str_mv Ciência dos materiais
Ligas de aço
Moagem de alta energia
Ligas com memória de forma
Shape memory
Mechanical milling
topic Ciência dos materiais
Ligas de aço
Moagem de alta energia
Ligas com memória de forma
Shape memory
Mechanical milling
description This thesis presents studies on Fe-30Mn-6Si shape memory alloys produced by high energy mechanical milling. Elemental powders of iron, manganese and silicon were processed in a planetary mill with a rotational speed of 500 rpm with milling times of 1 to 10 h. X-ray diffractograms showed the evolution of the various crystallographic phases present in the material. A single FeMnSi austenitic phase with nanometric crystalline size is found at 4 h of milling time. This phase is stable up to 10 h of milling. Mössbauer spectra showed the existence of a ferromagnetic sextet and a paramagnetic singlet at the beginning of the milling process. During the course of grinding the sextet is replaced by the singlet. Only the paramagnetic singlet associated to the FeMnSi austenitic phase is seen from 4 h to 10 h. Scanning electron microscopy and granulometry results showed that the samples are not homogeneous and have particle sizes in the micrometer range. The powder sample milling for 4 h was compacted and sintered to produce cylinders with a height of 11 mm and a diameter of 8 mm. The sintered cylinders were subjected to compression deformation and subsequent heat treatment for shape recovery. X-ray diffraction results showed the presence of γ austenite phase and of a small fraction of ε martensite with HCP structure in the sintered cylinder. The diffractogram of the deformed sample showed that a large fraction of austenite was transformed into martensite. After heat treatment it was observed that part of the martensite phase was transformed back into austenite. The Mössbauer spectra of these samples showed that the Fe atoms are found in more than one paramagnetic environment, which is consistent with the results of X-ray diffraction. Scanning electron microscopy revealed the presence of pores created by the cylinder manufacturing process. Values of hardness can be associated to the porosity of the samples. Corrosion tests showed that the deformed sample showed the best corrosion performance, which is attributed to the higher presence of martensite in this sample. Deformation and shape recovery tests led to an elastic recovery of 5.3% after removal of the compressive load and a plastic recovery of 0.9% after the heat treatment, resulting in a total recovery of 6.2%. These results provide evidence that the shape memory effect occurs both after mechanical relief as well as after heat treatment. The plastic recovery effect is associated with ε − γ transformation observed by X-ray diffraction. The plastic recovery around 0.9% after the heat treatment obtained in this study is consistent with results previously reported for FeMnSi alloys with similar chemical composition.
publishDate 2018
dc.date.none.fl_str_mv 2018-12-11T11:36:54Z
2018-12-11T11:36:54Z
2018
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 SILVA, F. I. S. da. Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia. 2018. 93 f. Tese (Doutorado em Engenharia e Ciência de Materiais)-Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2018.
http://www.repositorio.ufc.br/handle/riufc/37974
identifier_str_mv SILVA, F. I. S. da. Síntese e caracterização de ligas Fe-Mn-Si com efeito memória de forma obtidas por moagem mecânica de alta energia. 2018. 93 f. Tese (Doutorado em Engenharia e Ciência de Materiais)-Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2018.
url http://www.repositorio.ufc.br/handle/riufc/37974
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
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dc.format.none.fl_str_mv application/pdf
dc.source.none.fl_str_mv reponame:Repositório Institucional da Universidade Federal do Ceará (UFC)
instname:Universidade Federal do Ceará (UFC)
instacron:UFC
instname_str Universidade Federal do Ceará (UFC)
instacron_str UFC
institution UFC
reponame_str Repositório Institucional da Universidade Federal do Ceará (UFC)
collection Repositório Institucional da Universidade Federal do Ceará (UFC)
repository.name.fl_str_mv Repositório Institucional da Universidade Federal do Ceará (UFC) - Universidade Federal do Ceará (UFC)
repository.mail.fl_str_mv bu@ufc.br || repositorio@ufc.br
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