Alguns espelhos usados em câmeras de satélite devem apresentar qualidade superficial elevada. Eles são normalmente fabricados em ZERODUR®, um material vitrocerâmico, por meio de processos abrasivos. Observou-se que a qualidade da superfície do material deteriora-se algum tempo após a usinagem, necessitando assim de retrabalho. A causa mais influente desse fenômeno é o crescimento de trincas devido à corrosão sobtensão. Estas trincas são geradas pelas condições impostas nos processos convencionais de lapidação e polimento. Este trabalho apresenta um estudo sobre a usinabilidade do ZERODUR® utilizando torneamento de ultraprecisão com ferramenta de diamante de ponta única como uma alternativa a estes métodos tradicionais. Amostras de ZERODUR® foram submetidas a testes de indentação e riscamento a fim de se estudar as propriedades mecânicas do material, a transição dúctil-frágil e os mecanismos de remoção de material. Com base nesses testes, foi delineado um experimento fatorial do tipo 23 para avaliar a influência das seguintes variáveis de usinagem: profundidade de corte, nos níveis 0,4 e 0,2 \'mü\'m, taxa de avanço, nos níveis 0,3 e 0,1 \'mü\'m/rev e ângulo de saída da ferramenta, nos níveis -5º e -20º. As amostras do experimento foram usinadas em um torno de ultraprecisão com a ferramenta de diamante de ponta única. A qualidade superficial de cada combinação foi avaliada por microscopia eletrônica de varredura e perfilometria óptica interferométrica. Os resultados dos experimentos foram analisados estatisticamente, por meio de análise de variância (ANOVA). Para os intervalos das variáveis testadas verificou-se que o ângulo de inclinação da ferramenta é o que mais afeta a qualidade superficial. Ângulos com inclinações mais negativas (-20º) proporcionaram as melhores qualidades superficiais (em torno de 200 nm). Nos resultados não houve evidência de que o corte do material tenha ocorrido dentro do regime dúctil. Porém, a rugosidade superficial encontrada em algumas combinações de corte sugere que o torneamento de ultraprecisão pode ser uma alternativa ao processo lapidação que antecede o polimento. Este trabalho de caráter exploratório contribui com estimativas de alguns parâmetros ótimos para usinagem do ZERODUR®, fornecendo subsídios para pesquisas futuras sobre este tema. / Some mirrors used in satellite cameras must present a high surface quality. They are usually made of ZERODUR®, a brittle glass ceramic, by means of abrasive processes. It was observed that the surface quality of the material deteriorates some time after the machining, thus requiring rework. The most influential cause of this phenomenon is the crack growth due to stress corrosion. These cracks are generated by the conventional machining processes of lapping and polishing. This work presents a study on the machinability of ZERODUR® using ultraprecision turning with single-point diamond tool as an alternative to these traditional methods. ZERODUR® samples were subjected to indentation and nano-scratching tests in order to study the ductile-brittle transition and material removal mechanisms. After that, a \'2 POT.3\' factorial experiment was designed in order to assess the influence of three machining parameters on the resulting surface roughness, which are: depth of cut (tested at levels 0,4 and 0,2 \'mü\'m), feed rate (tested at levels 0,3 and 0,1 \'mü\'m/rev) and rake angle of the cutting tool (tested at levels -5º e -20º). The samples were turned with single-point diamond tool using different combinations of the parameters at the levels described above. The surface quality of each sample was evaluated using an interferometric optical profiler and a scanning electron microscope (SEM). The results of the experiments were statistically evaluated by means of Analysis Of Variance (ANOVA). For the ranges tested, it was found that the rake angle of the tool was the most influential parameter. The angle of -20º provided the best values for surface quality, which were around 200 nm. There was no evidence that the cut of the material occurred in the ductile regime, however, the obtained surface roughness showed that the ultraprecision turning may be a feasible alternative for the lapping process of optical components. This exploratory research contributes to the existing knowledge by providing estimates for optimal parameters of ZERODUR® machining, furnishing empirical basis for future research in this field.

Alguns espelhos usados em câmeras de satélite devem apresentar qualidade superficial elevada. Eles são normalmente fabricados em ZERODUR®, um material vitrocerâmico, por meio de processos abrasivos. Observou-se que a qualidade da superfície do material deteriora-se algum tempo após a usinagem, necessitando assim de retrabalho. A causa mais influente desse fenômeno é o crescimento de trincas devido à corrosão sobtensão. Estas trincas são geradas pelas condições impostas nos processos convencionais de lapidação e polimento. Este trabalho apresenta um estudo sobre a usinabilidade do ZERODUR® utilizando torneamento de ultraprecisão com ferramenta de diamante de ponta única como uma alternativa a estes métodos tradicionais. Amostras de ZERODUR® foram submetidas a testes de indentação e riscamento a fim de se estudar as propriedades mecânicas do material, a transição dúctil-frágil e os mecanismos de remoção de material. Com base nesses testes, foi delineado um experimento fatorial do tipo 23 para avaliar a influência das seguintes variáveis de usinagem: profundidade de corte, nos níveis 0,4 e 0,2 \'mü\'m, taxa de avanço, nos níveis 0,3 e 0,1 \'mü\'m/rev e ângulo de saída da ferramenta, nos níveis -5º e -20º. As amostras do experimento foram usinadas em um torno de ultraprecisão com a ferramenta de diamante de ponta única. A qualidade superficial de cada combinação foi avaliada por microscopia eletrônica de varredura e perfilometria óptica interferométrica. Os resultados dos experimentos foram analisados estatisticamente, por meio de análise de variância (ANOVA). Para os intervalos das variáveis testadas verificou-se que o ângulo de inclinação da ferramenta é o que mais afeta a qualidade superficial. Ângulos com inclinações mais negativas (-20º) proporcionaram as melhores qualidades superficiais (em torno de 200 nm). Nos resultados não houve evidência de que o corte do material tenha ocorrido dentro do regime dúctil. Porém, a rugosidade superficial encontrada em algumas combinações de corte sugere que o torneamento de ultraprecisão pode ser uma alternativa ao processo lapidação que antecede o polimento. Este trabalho de caráter exploratório contribui com estimativas de alguns parâmetros ótimos para usinagem do ZERODUR®, fornecendo subsídios para pesquisas futuras sobre este tema. / Some mirrors used in satellite cameras must present a high surface quality. They are usually made of ZERODUR®, a brittle glass ceramic, by means of abrasive processes. It was observed that the surface quality of the material deteriorates some time after the machining, thus requiring rework. The most influential cause of this phenomenon is the crack growth due to stress corrosion. These cracks are generated by the conventional machining processes of lapping and polishing. This work presents a study on the machinability of ZERODUR® using ultraprecision turning with single-point diamond tool as an alternative to these traditional methods. ZERODUR® samples were subjected to indentation and nano-scratching tests in order to study the ductile-brittle transition and material removal mechanisms. After that, a \'2 POT.3\' factorial experiment was designed in order to assess the influence of three machining parameters on the resulting surface roughness, which are: depth of cut (tested at levels 0,4 and 0,2 \'mü\'m), feed rate (tested at levels 0,3 and 0,1 \'mü\'m/rev) and rake angle of the cutting tool (tested at levels -5º e -20º). The samples were turned with single-point diamond tool using different combinations of the parameters at the levels described above. The surface quality of each sample was evaluated using an interferometric optical profiler and a scanning electron microscope (SEM). The results of the experiments were statistically evaluated by means of Analysis Of Variance (ANOVA). For the ranges tested, it was found that the rake angle of the tool was the most influential parameter. The angle of -20º provided the best values for surface quality, which were around 200 nm. There was no evidence that the cut of the material occurred in the ductile regime, however, the obtained surface roughness showed that the ultraprecision turning may be a feasible alternative for the lapping process of optical components. This exploratory research contributes to the existing knowledge by providing estimates for optimal parameters of ZERODUR® machining, furnishing empirical basis for future research in this field.

Made available in DSpace on 2017-07-21T20:42:39Z (GMT). No. of bitstreams: 1 Hudison.pdf: 7678712 bytes, checksum: 77d524c573ba60402f77fbda4e17c5e9 (MD5) Previous issue date: 2013-03-25 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / In the present study was investigated the API 5L X70 steel mechanical behavior through tensile and instrumented impact tests. Results from the instrumented Charpy impact test have allowed quantify the forces, energies and deflections of the specimens. It was used to obtain the fracture mechanics parameters such as the dynamic fracture toughness JId, the stress intensity factor for dynamic loading KId, as also range the ductile brittle transition temperature. Simultaneously was evaluated the mechanisms that induce to the delamination phenomenon as well as the investigation of their influence on the absorbed energy during the impact test. It was also analyzed the microtexture and mesotexture of different samples from the brittle, ductile and mixed regions from the ductile brittle transition temperature curve. Results have shown that the longitudinal direction was slightly superior mechanical properties when compared to the transverse direction. The dynamic fracture toughness JId was higher for the L-T specimen orientation when compared to the T-L orientation and it tends to increase with increasing temperature for both directions. The stress intensity factor values for dynamic loading was close to in both L-T and T-L orientations. The microtexture has revealed that deformation process from the impact test preserves some of its characteristics from the prior processing such as phase transformations and recrystallization components. While the mesotexture feature has shown higher energy values in the ductile brittle transition temperature curve, it is resulted from the formation of deformation substructure. Results obtained by scanning electron microscopy and light microscopy have shown that the main factors that may be contributing to the formation of crack-divider type delaminations are banded microstructure and elongated ferrite grains. While the microtexture from the edges delamination has shown that propagation mechanism is intergranular. Taylor factor mapping has shown that the mechanism responsible for the formation of delamination is accompanied by low plastic deformation. / No presente trabalho foi investigado o comportamento mecânico do aço API 5L X70 através de ensaios de tração e impacto instrumentado. O ensaio de impacto Charpy instrumentado permitiu quantificar as forças, energias e deflexões dos corpos de prova. Com a utilização destes dados foram obtidos parâmetros da mecânica da fratura, tais como, a tenacidade à fratura dinâmica JId, o fator de intensidade de tensão para carregamento dinâmico KId, além da faixa de valores da temperatura de transição dúctil frágil. Concomitantemente foram avaliados os mecanismos que contribuem na formação do fenômeno conhecido como delaminação, bem como a investigação de sua influência sobre a energia absorvida durante o ensaio de impacto. Foram também analisadas a microtextura e mesotextura de diferentes amostras retiradas da região frágil, dúctil e mista, da curva de transição dúctil frágil do material. Os resultados mostraram que o material possui propriedades mecânicas de impacto ligeiramente superiores na direção longitudinal à laminação comparado à direção transversal. Os valores encontrados para a tenacidade à fratura dinâmica JId são superiores para corpos de prova com orientação L-T quando comparados para a orientação T-L, e tendem a aumentar com o aumento da temperatura para ambas orientações. Os valores encontrados para o fator de intensidade de tensão para carregamento dinâmico foram próximos para ambas as orientações L-T e T-L. A microtextura revelou que após a deformação no ensaio de impacto o aço preserva algumas das características do seu histórico de processamento tais como componentes de transformações de fase e recristalização. Enquanto que o estudo da mesotextura mostrou que maiores valores de energia na curva de transição dúctil frágil resultam na formação de uma subestrutura de deformação. Resultados obtidos por microscopia eletrônica de varredura e microscopia ótica mostraram que os principais fatores que podem estar contribuindo para formação de delaminações do tipo trinca divisora são a microestrutura bandeada e grãos alongados de ferrita. Enquanto que a microtextura nas bordas da delaminação mostrou que o seu mecanismo de propagação é intergranular. O mapeamento do fator de Taylor mostrou que o mecanismo responsável pela formação da delaminação é acompanhado por pouca deformação plástica.

Abstract From the largest discontinuities to the smallest of the elements, various factors can threaten structural integrity. Susceptibility to these factors elevates with higher yield strengths. As-quenched low-carbon steels with a martensitic or martensitic-bainitic microstructure are modern ultra-high-strength structural steels. They can possess sufficient toughness, formability, and weldability, and are typically used in weight-critical and high-performance structures. Common problems with as-quenched steels with a yield strength of 900 MPa or more are that they do not obey the conventional correlation between the fracture toughness reference temperature T₀ and the impact toughness transition temperature T₂₈ᴊ used in many standards and structural integrity assessment procedures, and a lack of design rules in general. This thesis studies the relationship between the T₀ and T₂₈ᴊ to provide additional knowledge for future standardisation, the microstructural features governing the toughness at these temperatures on both global and local scale, and whether hydrogen embrittlement is present at subzero temperatures. It uses steels produced via laboratory rolling and quenching as well as from pilot-scale and full-scale industrial production, studying them with standardised toughness tests, microstructural characterisation, fractography, and cohesive zone modelling. As-quenched steels have a distinct correlation between T₀ and T₂₈ᴊ. An improved general T₀ – T₂₈ᴊ correlation applies to a wide range of steels. T₂₈ᴊ correlates closely with a dynamic reference toughness, which can be used together with the fraction of detrimental {100} cleavage planes near the main fracture plain to effectively estimate the transition temperatures. On a local scale, centreline segregation decreases the effective coarse grain size, which more than compensates for the harmful effects associated with the higher hardness and inclusion content of the centreline, resulting in increased fracture toughness. Hydrogen embrittlement causes a decrease in fracture toughness and local deformability, thereby increasing T₀ while leaving T₂₈ᴊ unaffected. Overall, the results show that high toughness demands good control of effective coarse grain size and hydrogen content. / Tiivistelmä Tekijät suurimmista epäjatkuvuuskohdista aina pienimpään alkuaineeseen voivat uhata rakenteellista eheyttä, minkä lisäksi alttius näille kasvaa materiaalin myötölujuuden kasvaessa. Modernit karkaistun tilan ultralujat matalahiiliset rakenneteräkset voivat silti omata riittävän sitkeyden, muovattavuuden ja hitsattavuuden. Tyypillisiä käyttökohteita näille ovat painon suhteen kriittiset ja korkean suorituskyvyn rakenteet. Yleinen ongelma myötölujuudeltaan noin ja yli 900 MPa karkaistun tilan teräksillä on se, että ne eivät noudata perinteistä murtumissitkeyden referenssilämpötilan T₀ ja iskusitkeyden transitiolämpötilan T₂₈ᴊ välistä korrelaatiota, jota käytetään useissa standardeissa ja suunnitteluohjeissa, jotka eivät myöskään vielä salli näin lujien terästen käyttöä. Tämä väitöstyö tutkii transitiolämpötilojen T₀ ja T₂₈ᴊ välistä suhdetta edistääkseen näiden terästen sisällyttämistä standardeihin, haurasmurtuma-sitkeyteen vaikuttavia mikrorakenteellisia tekijöitä sekä yleisellä että paikallisella tasolla, ja vetyhaurautta matalissa lämpötiloissa. Koeteräkset ovat laboratoriovalmisteisia, tuotantokokeita ja tuotantolaatuja. Niitä tutkitaan standardisoiduilla sitkeyskokeilla, mikrorakenteen karakterisoinnilla, fraktografialla ja koheesiovyöhykettä hyödyntävällä mallinnuksella. Tulokset osoittavat karkaistun tilan terästen omaavan erityisen korrelaation T₀ ja T₂₈ᴊ välillä. Muokattu, ultralujat teräkset huomioiva yleinen T₀ – T₂₈ᴊ -korrelaatio soveltuu laajalti eri terästyypeille. T₂₈ᴊ korreloi läheisesti dynaamisen referenssisitkeyden kanssa, jonka avulla yhdessä haitallisten {100} lohkomurtumatasojen osuuden kanssa voidaan estimoida joukko transitiolämpötiloja. Paikallisella tasolla keskilinjasuotauma pienentää efektiivistä karkeiden rakeiden kokoa, mikä suotauman suurista sulkeumista ja kovuudesta huolimatta parantaa murtumissitkeyttä. Vetyhauraus taas huonontaa sitkeyttä ja paikallista muodonmuutoskykyä myös matalissa lämpötiloissa nostaen T₀ lämpötiloja. Kokonaisuutena erinomainen transitiolämpötilasitkeys vaatii efektiivisen karkearaekoon ja vetypitoisuuden minimointia.

De récents travaux consacrés à l’étude des propriétés des matériaux aux petites échelles ont souligné des différences exceptionnelles dans le comportement mécanique des nano-objets par rapport aux matériaux massifs. Dans le cas du silicium, une transition fragile-ductile à température ambiante a été observée lorsque la taille des échantillons est réduite. Cependant, les défauts et les mécanismes à l’origine de ce changement de comportement n’ont pas été clairement identifiés. Ce travail repose sur l’étude post mortem de nanopiliers déformés, en utilisant différentes techniques de microscopie électronique. Les nanopiliers étudiés ont été préparés par gravure plasma et déformés en compression à température ambiante. Les résultats obtenus durant cette thèse, confirment la différence de comportement des nano-objets par rapport au matériau massif. Par ailleurs, une grande variété de défauts produits lors de la compression a été observée. L’orientation cristallographique de l’axe de sollicitation semble avoir un impact important sur les mécanismes à l’origine du comportement ductile observé. La comparaison entre images HRTEM expérimentales et simulées témoigne de la propagation simultanée de dislocations partielles et parfaites dans les plans {111}. De plus, des événements plastiques ont également été observés dans des plans {115}. Divers mécanismes de déformation possibles impliqués lors de la compression des piliers sont décrits à partir des observations microscopiques. Un modèle tenant compte de l’influence sur la mobilité des dislocations des interactions entre systèmes de glissement est proposé afin d’expliquer la transition fragile-ductile observé aux petites échelles / Several recent works devoted to the study of the properties of materials at small scales have revealed exceptional differences in the mechanical behavior of nano-objects as compared to bulk material. In the case of silicon, a brittle-ductile transition at room temperature has been observed when the sample size decreases. However, the extended defects and mechanisms behind this behavioral change have not been clearly identified. This work is based on the post mortem study of deformed nanopillars, using different electron microscopy techniques. The studied nano-pillars of 100 nm in diameter were prepared by plasma etching (RIE) and deformed in compression at room temperature. The results obtained during this thesis confirm the difference in the behavior of nano-objects compared to bulk material. Moreover, a large variety of defects produced during plastic deformation has been observed. The crystallographic orientation of the deformation axis seems to have a significant impact on the mechanisms behind the observed ductile behavior. The comparison between experimental and simulated HRTEM images notably evidences the simultaneous propagation of partial and perfect dislocations in {111} planes. In addition, unexpected plastic events have also been observed in {115} planes. Various possible deformation mechanisms involved during the nano-compression of the pillars are described, based on the microscopic observations. Finally, a model considering the influence of interactions between various activated systems on the mobility of dislocations is proposed to explain the brittle-ductile transition observed at small scales in silicon

No description available.

In the present thesis the crack propagation in the ductile-brittle transition region is studied on two scales with deterministic models. In the macroscopic model the ductile failure is described by a non-local Gurson-model whereas the discrete void microstructure is resolved around the crack tip in the microscopic model. The failure by cleavage is not evaluated by means of a post-processing criterion but is modeled equivalently using a cohesive zone model on both scales. Thus, cleavage is not a priori identified with unstable crack propagation but the transition between stable and unstable mode of propagation is a result of the simulation. The problem of handling completely failed material within the framework of non-local damage models is pointed out. A method to overcome this problem is proposed and successfully applied. The case of contained plastic yielding at the crack tip is addressed with a modified-boundary layer model. The macroscopic simulations reproduce many features which are known from experiments like the formation of stretch zones, cleavage after initial ductile tearing, pop-ins with crack arrest, among others. The microscopic simulations substantiate the understanding of the macroscopically observed behavior. Systematic parameter studies are performed. Starting with considerations on the limit cases like pure ductile failure or the lower-ductile brittle transition region allows to separate the effects of the different constitutive parameters. Based on these results, a methodology is proposed to extract the macroscopic material parameters from experiments. This scheme is successfully applied to experimental data from literature. The results show that the behavior of a low-constraint specimen can be reliably predicted with the parameters extracted from a high-constraint specimen. / In der vorliegenden Arbeit wird die Rissausbreitung im spröd-duktilen Übergangsbereich auf zwei Skalen mittels deterministischer Modelle untersucht. Das duktile Versagen wird im makroskopischen Modell durch ein nichtlokales Gurson-Modell beschrieben, während im mikroskopischen Modell die Porenmikrostruktur im Bereich um die Rissspitze diskret aufgelöst wird. Das mögliche Versagen durch Spaltbruch wird nicht, wie üblich, nachträglich durch ein spannungsbasiertes Kriterium bewertet. Stattdessen wird der Spaltbruch auf beiden Skalen durch ein Kohäsivzonenmodell abgebildet. Somit wird die Spaltbruchinitiierung nicht a priori mit instabiler Rissausbreitung gleichgesetzt. Vielmehr ist die Stabilität der Rissausbreitung ein Ergebnis der Simulationen. Außerdem wird das Problem der der Handhabung vollständig ausgefallenen Materials im Rahmen nichtlokaler Schädigungsmodelle herausgestellt. Es wird eine Methode vorgestellt, dieses Problem zu behandeln und erfolgreich angewendet. In den Simulationen wird der Fall vollständig eingebetteten, plastischen Fließens untersucht. Die Simulationen mit dem makroskopischen Modell geben viele Effekte wieder, die aus Experimenten bekannt sind. Dazu zählen die Ausbildung von Stretchzonen, die Spaltbruchinitiierung nach anfänglichem, duktilem Reißen oder lokale Instabilitäten mit Rissarrest. Die mikroskopischen Simulationen tragen zum Verständnis des makroskopisch beobachteten Verhaltens bei. In der vorliegenden Arbeit werden systematische Parameterstudien durchgeführt. Zunächst werden Grenzfälle wie das rein duktile Versagens oder der Spaltbruch in Abwesenheit der Mikroporen untersucht, um die Einflüsse der einzelnen Materialparameter abzugrenzen. Ausgehend von diesen Ergebnissen wird eine Prozedur vorgeschlagen, die Materialparameter des makroskopischen Modells Schritt für Schritt aus Experimenten zu bestimmen. Diese Prozedur wird erfolgreich auf experimentelle Daten aus der Literatur angewendet. Die Ergebnisse zeigen, dass es das entwickelte Modell erlaubt, das Verhalten einer Bruchmechanikprobe mit geringer Dehnungsbehinderung an der Rissspitze mit denjenigen Materialparametern vorherzusagen, die an Proben mit einer hohen Dehnungsbehinderung ermittelt wurden.

Bulk metallic glasses (BMGs) are a new class of structural materials and exhibit unique combinations of mechanical properties. As a result, their mechanical behavior has been an active area of scientific pursuit in the recent past and considerable emphasis has been paid to understand plastic deformation in them. It is now well accepted that shear transformation zones (STZs), aided by free volume, are the fundamental carriers of plasticity. At a microscopic level, deformation at low temperatures and high stresses tends to localize into shear bands. Most BMGs posses high fracture toughness despite high yield strengths and poor global ductility. However, the micro-mechanisms of fracture and fatigue in this new class of materials are not fully understood yet. The overall objective of this study is to provide insights into the fracture and fatigue response of amorphous alloys, which is important both from scientific and technological perspectives. The key questions we seek to answer through this study are the following. Do amorphous alloys undergo a ductile-brittle transition (DBT), and if so what are the reasons for it? What are the parameters that influence fatigue crack initiation in amorphous alloys and whether fatigue life can be improved by surface treatments? A related question is whether the BMGs are susceptible to deformation-induced crystallization (DIC). A Zr-based BMG, Zr41.2Ti13.75Cu12.5Ni10Be22.5 was utilized to conduct this study. By comparing the fracture and fatigue behaviors in the as-cast and annealed states {annealing was carried out below the glass transition temperature (Tg) because of established embrittlement effects}, we seek to provide answers for the questions posed above. We begin by examining the influence of temperature on the toughness of BMGs. Impact toughness measurements show that the annealed samples, which are brittle at room temperature, recover the lost toughness beyond a critical temperature (TDB) and exhibit a sharp DBT. However, the hardness remains unaffected across the TDB. Fractography reveals nano-scale patterning and cleavage fracture in the brittle state, while the formation of thick vein-patterns and shear fracture are characteristics of the ductile state of the annealed samples. We explore various micro-mechanistic possibilities for explaining the features of this transition, including a critical Poisson’s ratio-toughness correlation. Next, to understand the origins of fatigue crack initiation, we study the un-notched fatigue response of as-cast and sub-Tg annealed Zr-based BMG specimens. Because of embrittlement and nano-crystallization at the crack initiation region, the annealed specimens exhibit a lower fatigue life than the as-cast specimens. Shot-peening of the as-cast specimens did not exhibit significant improvement in their fatigue performance because of competing effects between the compressive residual stress field (CRSF) and deformation-induced softening. To further investigate surface and repeated loading effects, the tribological response of the as-cast Zr-based BMG was compared with specimens annealed above and below the Tg. A good correlation between the hardness (increasing as a function of the annealing temperature) and wear rate was obtained. The formation and peeling of the oxide layer formed during testing was the primary wear mechanism in all the specimens. Lastly, crystallization was observed within the deformed region of the as-cast Zr-based BMG repeatedly scratched with a sharp diamond indenter. But, transmission electron microscopy (TEM) does not reveal any evidence of crystallization within the indents formed within an electron transparent film formed by laser deposition of the as-cast Zr-based BMG. Absence of crystallization in deformed regions obtained by designing critical experiments, which avoid artifacts generated during sample preparation, suggests that the occasional observation of DIC might be an exception rather than the rule in BMGs.

Submitted by ISABELA ATILIO null (isabelaatilio@hotmail.com) on 2017-10-31T16:58:11Z No. of bitstreams: 1 Dissertação Final - Isabela Atilio.pdf: 12968588 bytes, checksum: 24d1b58efcf37a8ffc0d9ed1afc4d7d4 (MD5) / Approved for entry into archive by LUIZA DE MENEZES ROMANETTO (luizamenezes@reitoria.unesp.br) on 2017-11-10T19:48:34Z (GMT) No. of bitstreams: 1 atilio_i_me_guara.pdf: 12968588 bytes, checksum: 24d1b58efcf37a8ffc0d9ed1afc4d7d4 (MD5) / Made available in DSpace on 2017-11-10T19:48:34Z (GMT). No. of bitstreams: 1 atilio_i_me_guara.pdf: 12968588 bytes, checksum: 24d1b58efcf37a8ffc0d9ed1afc4d7d4 (MD5) Previous issue date: 2017-09-18 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / O aumento da demanda por petróleo e seus derivados tem instigado o desenvolvimento de materiais para dutos com elevadas tenacidade à fratura e resistência mecânica, como os aços de alta resistência e baixa liga (ARBL) pertencentes às classes API. Aliada à utilização destes aços, a aplicação do processo de soldagem por resistência elétrica de alta frequência (HF/ERW) tem conquistado maior interesse no setor. Entretanto, defeitos nas juntas soldadas constituem uma das principais causas de falhas em dutos, principalmente quando associados às condições externas de operação, o que tem sido motivo para estudos relacionados à integridade estrutural destes tubos. O objetivo deste trabalho foi estudar a tenacidade à fratura de um tubo de aço API 5L X70 soldado pelo processo HF/ERW, a partir de dados obtidos com ensaios CTOD de espécimes de flexão por três pontos, tipo SE(B) “gull wing”. A metodologia proposta envolveu ensaios de CTOD a variadas temperaturas, incluindo a região de transição dúctil-frágil, a fim de avaliar a integridade estrutural do material em condições críticas de operação. Os ensaios foram realizados com base nas normas ASTM E1820 e BS7448, e consistiram na utilização de corpos de prova retirados diretamente da parede do tubo, com posterior planificação. De forma geral, as amostras de material base apresentaram uma boa tenacidade à fratura em todas as temperaturas de ensaio, o que não aconteceu com as amostras de material de solda, que apresentaram baixa tenacidade. Os resultados de tenacidade obtidos mostraram que a metodologia empregada para o estudo da integridade estrutural por meio de ensaios CTOD com amostras extraídas diretamente da parede do tubo, com posterior planificação, mostrou-se adequada. Embora as normas ASTM E1820 e BS7448 adotem diferentes parâmetros para a determinação do valor de CTOD, observou-se que os valores de CTOD foram bem próximos. / The increasing demand for oil and its products has driven the development of materials for ducts with high fracture toughness and high mechanical strength, such as high strength low alloy (HSLA) steels, appertaining to the API classes. In addition to the use of these steels, the application of the high frequency resistance welding process (HF/ERW) has gained greater interest in the sector. However, defects in the welded joints are one of the most causes of failures in pipelines, especially when they are associated with external operating conditions, which has been the reason for studies related to the structural integrity of these tubes. The aim of this work was to study the fracture toughness of an API 5L X70 steel tube welded by the HF/ERW process, from data obtained with CTOD tests bending specimens by three points, type SE (B) gull wing. The proposed methodology involved CTOD tests at various temperatures, including the ductile-brittle transition region, in order to assess the structural integrity of the material under critical operating conditions. The tests were performed based on the ASTM E1820 and BS7448 standards, and consisted of the use of specimens taken directly from the wall of the tube, with subsequent planning. In general, the base material samples showed good fracture toughness at all test temperatures, which did not occur with the samples of welded material, which presented low toughness. The toughness results obtained showed that the methodology used for the study of structural integrity by means of the CTOD tests with samples drawn directly from the wall of the tube, with subsequent planning, was adequate. Although the ASTM E1820 and BS7448 standards adopt different parameters for the determination of the CTOD value, it was observed that the CTOD values were very close.

In the present thesis the crack propagation in the ductile-brittle transition region is studied on two scales with deterministic models. In the macroscopic model the ductile failure is described by a non-local Gurson-model whereas the discrete void microstructure is resolved around the crack tip in the microscopic model. The failure by cleavage is not evaluated by means of a post-processing criterion but is modeled equivalently using a cohesive zone model on both scales. Thus, cleavage is not a priori identified with unstable crack propagation but the transition between stable and unstable mode of propagation is a result of the simulation. The problem of handling completely failed material within the framework of non-local damage models is pointed out. A method to overcome this problem is proposed and successfully applied. The case of contained plastic yielding at the crack tip is addressed with a modified-boundary layer model. The macroscopic simulations reproduce many features which are known from experiments like the formation of stretch zones, cleavage after initial ductile tearing, pop-ins with crack arrest, among others. The microscopic simulations substantiate the understanding of the macroscopically observed behavior. Systematic parameter studies are performed. Starting with considerations on the limit cases like pure ductile failure or the lower-ductile brittle transition region allows to separate the effects of the different constitutive parameters. Based on these results, a methodology is proposed to extract the macroscopic material parameters from experiments. This scheme is successfully applied to experimental data from literature. The results show that the behavior of a low-constraint specimen can be reliably predicted with the parameters extracted from a high-constraint specimen. / In der vorliegenden Arbeit wird die Rissausbreitung im spröd-duktilen Übergangsbereich auf zwei Skalen mittels deterministischer Modelle untersucht. Das duktile Versagen wird im makroskopischen Modell durch ein nichtlokales Gurson-Modell beschrieben, während im mikroskopischen Modell die Porenmikrostruktur im Bereich um die Rissspitze diskret aufgelöst wird. Das mögliche Versagen durch Spaltbruch wird nicht, wie üblich, nachträglich durch ein spannungsbasiertes Kriterium bewertet. Stattdessen wird der Spaltbruch auf beiden Skalen durch ein Kohäsivzonenmodell abgebildet. Somit wird die Spaltbruchinitiierung nicht a priori mit instabiler Rissausbreitung gleichgesetzt. Vielmehr ist die Stabilität der Rissausbreitung ein Ergebnis der Simulationen. Außerdem wird das Problem der der Handhabung vollständig ausgefallenen Materials im Rahmen nichtlokaler Schädigungsmodelle herausgestellt. Es wird eine Methode vorgestellt, dieses Problem zu behandeln und erfolgreich angewendet. In den Simulationen wird der Fall vollständig eingebetteten, plastischen Fließens untersucht. Die Simulationen mit dem makroskopischen Modell geben viele Effekte wieder, die aus Experimenten bekannt sind. Dazu zählen die Ausbildung von Stretchzonen, die Spaltbruchinitiierung nach anfänglichem, duktilem Reißen oder lokale Instabilitäten mit Rissarrest. Die mikroskopischen Simulationen tragen zum Verständnis des makroskopisch beobachteten Verhaltens bei. In der vorliegenden Arbeit werden systematische Parameterstudien durchgeführt. Zunächst werden Grenzfälle wie das rein duktile Versagens oder der Spaltbruch in Abwesenheit der Mikroporen untersucht, um die Einflüsse der einzelnen Materialparameter abzugrenzen. Ausgehend von diesen Ergebnissen wird eine Prozedur vorgeschlagen, die Materialparameter des makroskopischen Modells Schritt für Schritt aus Experimenten zu bestimmen. Diese Prozedur wird erfolgreich auf experimentelle Daten aus der Literatur angewendet. Die Ergebnisse zeigen, dass es das entwickelte Modell erlaubt, das Verhalten einer Bruchmechanikprobe mit geringer Dehnungsbehinderung an der Rissspitze mit denjenigen Materialparametern vorherzusagen, die an Proben mit einer hohen Dehnungsbehinderung ermittelt wurden.