Orientador: Itamar Ferreira / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-18T17:02:04Z (GMT). No. of bitstreams: 1 Uehara_AndreYugou_M.pdf: 4445631 bytes, checksum: ba69e40eee3a8de5233ab826f19564d7 (MD5) Previous issue date: 2011 / Resumo: Este trabalho tem por objetivo investigar a etapa de decapagem ácida e os processos de desidrogenação e retrabalho realizados durante a zincagem de parafusos quanto à fragilização por hidrogênio. Parafusos fabricados conforme a norma JIS B 1127 (1995), cementados, de 6 mm de diâmetro e 16 mm de comprimento de rosca foram organizados em 39 diferentes grupos. A decapagem foi avaliada quanto ao volume de ácido clorídrico (700 ml, 900 ml e 1000 ml) e presença, ou ausência, de inibidor para este ácido, utilizando tempos de decapagem de 15, 30, 45 e 60 minutos para cada condição de volume de ácido e inibidor utilizados. A desidrogenação foi avaliada utilizando parafusos decapados (solução: 1000 ml de ácido, ausência de inibidor e decapados por 15, 30, 45 e 60 minutos) e desidrogenados a uma temperatura de 1000C e tempo total de processo de 1, 2 e 3,5 horas. O retrabalho foi avaliado utilizando parafusos de 8 ?m de espessura de camada zincada, retrabalhados por 4 minutos em 700 ml de ácido, ausência de inibidor e 300 ml de água, avaliando as hipóteses do retrabalho único e duplo sem desidrogenação e do retrabalho único seguido de desidrogenação (1000C - 2 horas). Ensaios de pré-carregamento para a detecção da fragilização por hidrogênio foram realizados em parafusos que sofreram as preparações citadas, sendo o torque de ruptura avaliado nestes parafusos, assim como naqueles obtidos após o tratamento térmico. Análises química e metalográfica e ensaios de microdureza Vickers e tração, além de análise fratográfica por microscopia eletrônica de varredura (MEV) também foram realizados. A análise metalográfica revelou uma matriz ferrítica composta por grãos equiaxiais com carbonetos esferoidizados para o fio máquina, enquanto que o parafuso possui estrutura ferrítico-perlítica no núcleo e martensita revenida na camada cementada. Os ensaios de microdureza e de tração revelaram que o fio máquina e o parafuso possuem níveis de resistência mecânica dentro do esperado conforme as condições utilizadas, enquanto que não houve diferenças significativas entre os valores de torque de ruptura obtidos em ambas as situações analisadas. A etapa de decapagem ácida revelou que, nos grupos que não utilizaram inibidor, o número de falhas aumenta num primeiro momento com o aumento do tempo de decapagem, reduzindo após um determinado tempo de decapagem relacionado ao volume de ácido utilizado. O número de falhas sofre grande redução com a utilização do inibidor, porém mesmo a baixas concentrações de ferro, a utilização de maiores volumes de ácido associado a maiores tempos de decapagem aumentam o risco de fragilização. Apenas houve falha para a desidrogenação realizada a 1000C, por 1 hora, revelando a importância de adequados controles de temperatura, procedimentos de homogeneização e parâmetros de temperatura e tempo. Não houve falhas para o retrabalho revelando a importância de adequados procedimentos de retrabalho (tempo e solução) e de desidrogenação, enquanto que a análise da superfície de fratura revelou apenas os micromecanismos de fratura intergranular e dimples, sendo este último mais freqüentemente associado a regiões mais próximas ao núcleo, além da presença de trincas secundárias / Abstract: The main aim of this work is to investigate the effects on hydrogen embrittlement of bolts due to acid pickling, baking, and strip processes performed during zinc plating. Carburized bolts type "hexagon flange head tapping screws", with 6 mm of diameter and 16 mm of thread length were organized into 39 different groups. Acid pickling was evaluated using volumes of hydrochloric acid of 700 ml, 900 ml, and 1000 ml, presence, or absence, of acid inhibitor, and pickling periods of 15, 30, 45, and 60 minutes for each condition of acid volume and inhibitor used. Baking was evaluated using 1000C, and periods of 1, 2, and 3.5 hours for bolts that were subjected to acid pickling with a solution of 1000 ml of acid, absence of inhibitor, and pickling periods of 15, 30, 45, and 60 minutes. Strip was evaluated using bolts with zinc layer thickness of 8 ?m, stripped for 4 minutes in a solution of 700 ml of acid, absence of inhibitor, and 300 ml of water, performing the hypotheses of single and double strip without baking, and single strip followed by baking (1000C - 2 hours). Preloading tests for the detection of hydrogen embrittlement were conducted in bolts that were subjected to the preparations mentioned, while torsional tests were also conducted at these bolts, as well as in those obtained after heat treatment. Chemical and metallographic analysis, Vickers microhardness and tensile tests, and fractographic analysis using scanning electron microscopy (SEM) were also conducted. Metallographic analysis revealed a ferritic matrix composed of equiaxed grains with spheroidized carbides for the wire, while the bolts showed a ferritic-pearlitic microstructure at the center and tempered martensite at the hardened layer. Microhardness and tensile tests revealed that wire and bolts have strength levels as expected according to the conditions used, while no significant differences between the breaking torque values were obtained in both situations analyzed. Acid pickling revealed that in the groups, which did not use inhibitor, the number of failures increases at a first stage with increasing pickling periods, however it starts to decrease after a certain pickling period related to the volume of acid used. The number of failures is greatly reduced with the use of the inhibitor, but even at low concentrations of iron, the use of larger amounts of acid associated with longer pickling periods increases the risk of hydrogen embrittlement. Failures were observed only at 1000C - 1 hour as baking parameters, showing the importance of proper temperature controls, homogenization procedures, and temperature and time parameters. There were no failures related to strip, revealing the importance of adequate procedures for strip (period and solution used) and baking procedures as observed. The fracture surface analysis revealed only intergranular and dimples micromechanisms of fracture, where the latter being more often associated with regions closer to the core of the bolts, also showing the presence of secondary cracks / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica

Many experiments demonstrate that the effects of hydrogen solutes decrease macroscopic fracture stresses and strains in ductile materials. Hydrogen-related failures have occurred in nearly all industries involving hydrogen-producing environments. The financial losses incurred from those failures reaches millions if not billions of dollars annually. With the ever-urgent needs for alternative energy sources, there is a strong push for a hydrogen economy from government and private sectors. Safe storage and transportation of hydrogen increases the momentum for studying hydrogen-related failures, especially in ductile materials. To quantify ductile material damage with the effects of hydrogen embrittlement, it is necessary to add hydrogen effects into the void nucleation, void growth, and void coalescence equations. In this research, hydrogen-enhanced void nucleation is our focus, with hydrogen-enhanced void growth and void coalescence t be studied in the future. Molecular Dynamic (MD) and Monte Carlo (MC) simulations with Embedded Atom Method (EAM) potentials were performed to study how hydrogen affects dislocation nucleation, dislocation structure formation and nanovoid nucleation at nickel grain boundaries. The results were inserted into the continuum void nucleation model by Horstemeyer and Gokhale, and the relationships between stress triaxiality-driven void nucleation, grain boundary hydrogen concentrations and local grain geometries were extracted. MD and MC simulations with EAM potentials were also performed to study how hydrogen interstitials affect the dislocation nucleation, dislocation structure formation and subsequent anovoid nucleation of single crystal nickel in different hydrogen-charging conditions. Evolutions of dislocation structures of nickel single crystal with different hydrogen concentrations were compared. The effects of nanovoid nucleation stress and strain at different hydrogen concentrations were quantified. The results were also inserted into the Horstemeyer and Gokhale model and the relationship between stress triaxiality-driven void nucleation and hydrogen concentration caused by stress gradient, which showed similar trends as the grain boundary studies. From nanoscale studies and existing experimental observations, a continuum void nucleation model with hydrogen effects was proposed and used in a continuum damage model based upon Bammann and coworkers. The damage model was implemented into user material code in FEA code ABAQUS. Finite element analyses were performed and the results were compared to the experimental data by Kwon and Asaro.

"February, 2004." / Bibliography: leaves 231-249. / xxvii, 261 leaves : ill. (some col.), plates, photos (col.) ; 30 cm. / Title page, contents and abstract only. The complete thesis in print form is available from the University Library. / Examines ways of reducing the risk of hydrogen assisted cold cracking in pipeline construction by modifying the construction procedure to reduce residual stress and hydrogen concentration. A numerical model of the pipeline construction procedure capable of modelling the process in a transient sense was created. Experimental validation of the model involved using the "blind hole drilling" strain gauge method of residual stress measurement. The diffusion of hydrogen during welding was modelled using a scheme based on Fick's Second Law of Diffusion, finding that the parameters which dominate the rate of diffusion are the timing of the weldment process, joint geometry, pre-heating and post-heating. / Thesis (Ph.D.)--University of Adelaide, School of Mechanical Engineering, 2004

Orientadores: Célia Marina de Alvarenga Freire, Itamar Ferreira / Dissertação (mestrado - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-20T02:38:33Z (GMT). No. of bitstreams: 1 Carvalho_IcaroZanettide_M.pdf: 13083038 bytes, checksum: c152edb400a89f8aecfa16c8073e6488 (MD5) Previous issue date: 2012 / Resumo: O fenômeno da fragilização por hidrogênio no aço AISI 4340 foi investigado devido ao fato do mesmo ser um aço baixa liga de alta resistência bastante suscetível a este fenômeno. A análise foi feita por meio do ensaio de tenacidade à fratura por flexão baseado na norma ASTM E 399 - 09. A matéria prima utilizada foi fabricada segundo dois diferentes processos, sendo o primeiro pelo método convencional de fundição e o segundo pelo processo VAR (vacuum arc refining) de maneira a se obter uma liga com menores quantidades de impurezas. Corpos-de-prova foram retirados da posição L-C das ligas, temperados a 845 oC e revenidos a 3 diferentes temperaturas (350 oC, 400 oC e 500 oC). O carregamento de hidrogênio foi feito por meio de uma célula eletroquímica, onde os corpos-de-prova foram imersos numa solução de H2SO4 0,01 M com aplicação de uma densidade de corrente de 10 mA/cm2 e dois diferentes tempos de hidrogenação, de maneira a se obter dois níveis de contaminação. Após os ensaios, foram feitas fractografias dos corpos-de-prova ensaiados para cada condição de revenimento e contaminação por hidrogênio, sendo observadas as alterações nos micromecanismos de fratura para as diferentes condições. Os resultados obtidos no ensaio de tenacidade à fratura por flexão foram correlacionados ao micromecanismo de fratura em função da dureza e contaminação por hidrogênio. O aço AISI 4340 convencional nas condições de revenimento de 400 oC e 350 oC mostrou-se bastante susceptível à fragilização por hidrogênio, apresentando reduções da ordem de 10% e 20%, respectivamente, nos valores de tenacidade à fratura de corpos-de-prova contaminados. O mesmo não foi observado no aço AISI 4340 convencional temperado e revenido a 500 oC, que não sofreu fragilização devido à sua baixa dureza. O aço AISI 4340 VAR em todas as condições de revenimento apresentou-se muito menos susceptível ao fenômeno, não sendo evidenciadas variações expressivas nas tenacidades à fratura dos corpos-de-prova contaminados e nas superfícies de fratura resultantes / Abstract: The phenomenon of hydrogen embrittlement in AISI 4340 steel was investigated due to the fact that it is a high strength low alloy steel quite susceptible to this phenomenon. The analysis was done through the fracture toughness test by bending based on ASTM E 399-09. The material used was manufactured according two different processes, the first by conventional casting process and the second by VAR (vacuum arc refining) process in order to obtain an alloy with minor amounts of impurities. Specimens were removed from the position L-C of the alloy, quenched at 845 oC and tempered at 3 different temperatures (350 oC, 400 oC and 500 oC). The hydrogen loading was made by means of an electrochemical cell where the specimens were immersed in a solution of 0.01 M H2SO4 by applying a current density of 10 mA/cm2 and two different hydrogenation times, in order to obtain two levels of contamination. After the tests were performed fractographies of specimens tested for each condition of temper and contamination by hydrogen, with observed changes in the micromechanisms of fracture for the different conditions. The test results of fracture toughness by bending were correlated with the micromechanisms of fracture, the microstructure and hydrogen contamination. The conventional AISI 4340 steel under conditions of tempering of 400 °C and 350 °C proved to be very susceptible to hydrogen embrittlement, with reductions of 10% and 20%, respectively, on the values of fracture toughness of contaminated specimens. The same was not observed in conventional AISI 4340 quenched and tempered at 500 °C, which did not presented embrittlement due to its low hardness. The AISI 4340 VAR steel in all conditions of temper proved to be much less susceptible to the phenomenon, not showing significant variations in fracture toughness of the contaminated specimens and the resulting fracture surfaces / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica

This work deals with the damage due to the simultaneous presence of hydrogen in atomic form and stress – straining.<p>The aim of this work is twofold: to better understand the hydrogen embrittlement mechanisms and to translate the acquired knowledge into a more appropriate qualification test. <p>The phenomena of hydrogen entry and transport inside the metals, together with the different types of damages due to the presence of hydrogen, are presented.<p>The analysis of the most important models proposed up to now for hydrogen embrittlement (HE) indicated that the slow dynamic plastic straining is a key factor for the embritteling process. There is a synergistic effect of hydrogen – dislocations interactions: on one hand hydrogen facilitates the dislocations movement (according to the HELP mechanism) and on the other hand dislocations transport hydrogen during their movement when their velocity is lower than a critical value. <p>This work is focused on supermartensitic stainless steels, base and welded materials. The interest on these materials is due to their broad use in offshore oil production. <p>First, the material’s characterisation with regards to hydrogen content and localisation was performed. This was conducted in charging conditions that are representative of industrial applications.<p>Because of previous industrial experience it was necessary to find a more appropriate qualification test method to asses the risk of HE. <p>In this work we proposed the stepwise repeated slow strain rate test (SW R – SSRT) as a qualification test method for supermartensitic stainless steels. <p>This test method combines hydrogen charging, test duration, plastic, dynamic and slow strains. Thus, this test method is coherent with both the model HELP proposed for hydrogen embrittlement and the observations of industrial failures. <p>The stepwise repeated slow strain rate test (SW RSSRT) is interesting not only as a qualification test of martensitic stainless steels, but also as a qualification test of conditions for using these materials (type of straining, range of strain and stress, strain rate, hydrogen charging conditions, etc.).<p><p><p><p>Ce travail se rapporte à l’endommagement provoqué par la présence simultanée de l’hydrogène sous forme atomique et une contrainte (appliquée où résiduelle). <p>Ce travail a comme but une meilleure compréhension du mécanisme de la fragilisation par l’hydrogène (FPH) et la recherche d’un essai de qualification qui soit cohérent avec ce mécanisme. <p>Les phénomènes liés à l’entrée et au transport de l’hydrogène au sein des métaux, ensemble avec les différents types d’endommagements dus à la présence de l’hydrogène, sont présentés.<p>L’analyse des modèles proposés jusqu’au présent pour la fragilisation par l’hydrogène (FPH) suggère que la déformation lente plastique dynamique est le facteur clé pour le processus de la fragilisation. Il y a un effet synergétique des interactions entre l’hydrogène et les dislocations: d’un coté l’hydrogène facilite le mouvement des dislocations (d’après le modèle HELP) et d’un autre coté les dislocations transportent l’hydrogène pendant leur mouvement, pourvu que leur vitesse soit en dessous d’une valeur critique. <p>Le travail a été conduit sur des aciers supermartensitiques, matériau de base et soudé. L’intérêt pour ces matériaux réside de leur large utilisation dans la production du pétrole en offshore. <p>D’abord, le matériau a été caractérisé du point de vu de la teneur et de la localisation de l’hydrogène. Les essais ont été conduits dans des conditions représentatives pour les cas industriels. <p>L’expérience industrielle d’auparavant indique qu’il est nécessaire de trouver un test de qualification plus approprié pour estimer la susceptibilité à la fragilisation par l’hydrogène. <p>Dans ce travail on propose un essai de traction lente incrémentée (SW R – SSRT) comme méthode de qualification pour les aciers supermartensitiques. <p>L’essai combine le chargement en hydrogène, la durée d’essai, la déformation lente, plastique et dynamique. Donc, cette méthode d’essai est cohérente avec le modèle HELP proposé pour FPH et les observations des accidents industriels. <p>Cet essai est intéressant pas seulement comme essai de qualification pour les aciers supermartensitiques, mais aussi comme essai de qualification pour les conditions d’utilisation des ces matériaux (type de déformation, niveau de déformation et contrainte, vitesse de déformation, conditions de chargement en hydrogène, etc.).<p> <p><p><p><p><p><p><p> / Doctorat en sciences appliquées / info:eu-repo/semantics/nonPublished