Orientador: Michelli Leali Costa / Resumo: Dentre os setores de aplicações comerciais de materiais compósitos avançados, destaca-se o setor aeroespacial com larga aplicação desses materiais. Entre as técnicas de união aplicadas aos compósitos termoplásticos está a soldagem com grandes vantagens em relação aos outros processos de uniões tais como, redução de custo, agilidade de processamento, redução de elementos acumuladores de tensão, preparações mais simplórias das superfícies a serem soldadas. Mesmo com essas vantagens e, embora o processo já seja utilizado nos setores industriais, a soldagem de compósitos tem como desafio a melhoria de sua resistência, a aplicação do processo para reparos ou processamentos em campo, além da necessidade de avaliação dos efeitos das condições climáticas em juntas soldadas, as quais podem estar submetidas quando em operação em uma aeronave, por exemplo. Mediante a isso, esse trabalho visa produzir e estudar juntas soldadas por resistência elétrica e por tocha acetilênica em compósito PEI/fibra de vidro. Os compósitos obtidos foram submetidos ao condicionamento higrotérmico seguido de ensaios mecânicos de LSS (Lap Shear Strength) e ENF (End-Notched Flexure). O mecanismo de fratura das juntas soldadas foi avaliado por microscopia. A partir das análises e dos resultados obtidos, foi observado que os valores de resistência ao cisalhamento em modo II dos compósitos soldados por resistência elétrica (3270,9 J/m²) são similares aos descritos na literatura para os compósitos PEI/fibra de vid... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Among the commercial application sectors of advanced composite materials, the aerospace sector with wide application of these materials stands out. Among the joining techniques applied to thermoplastic composites is welding with great advantages over other joining processes such as cost reduction, processing agility, reduction of stress accumulators, little or no preparation required of the surface to be processed. Even with these advantages, and although the process is already used in the industrial sectors, composite welding has the challenge of improving its resistance, the application of the process for field repairs or processing, and the need to evaluate the effects of weather conditions. welded joints, which may be subjected when operating in an aircraft, for example. Therefore, this work aims to produce and study joints welded by electric resistance and acetylene torch in PEI / fiberglass composite. The composites obtained were subjected to hygrothermal conditioning followed by mechanical tests of LSS (Lap Shear Strength) and ENF (End-Notched Flexure). The fracture mechanism of the welded joints was evaluated by microscopy. From the analyzes and results obtained, it was observed that the shear strength values in mode II of the composites welded by electric resistance (3270.9 J / m²) are similar to those described in the literature for PEI / fiberglass composites. However, for the composites welded by the oxyacetylene process, a reduction of approximately 20% in the va... (Complete abstract click electronic access below) / Mestre

In this work, Slow Strain Rate Test (SSRT) testing, Light Optical Microscopy (LOM) and Scanning Electron Microscopy (SEM) were used to study the effect of micro-structure, corrosive environments and cathodic polarisation on stress corrosion cracking (SCC) of two grades of high strength steels, Type A and Type B. Type A is manufactured by quench and tempered (Q&T) method. Type B, a normalize steel was used as reference. This study also supports electrochemical polarisation resistance method as an effective testing technique for measuring the uniform corrosion rate. SSRT samples were chosen from base metal, weld metal and Heat Affected Zone (HAZ). SSRT tests were performed at room temperature under free corrosion potential and cathodic polarisation using 4 mA/cm2 in 1 wt% and 3.5 wt% NaCl solutions. From the obtained corrosion rate measurements performed in 1 wt% and 3.5 wt% NaCl solutions it was observed that increased chloride concentration and dissolved oxygen content enhanced the uniform corrosion for all tested materials. Moreover, the obtained results from SSRT tests demonstrate that both Q&T and normalized steels were not susceptible to SCC in certain strain rate(1×10-6s-1) in 1 wt% and 3.5 wt% NaCl solutions under free corrosion potential. It was con-firmed by a ductile fracture mode and high reduction in area. The weld metal of Type A with acicular ferrite (AF), pro-eutectoid (PF) and bainite microstructure showed higher susceptibility to hydrogen assisted stress corrosion cracking compared to base metal and HAZ. In addition, typical brittle intergranular cracking with small reduction in area was observed on the fracture surface of the Type A due to hydrogen charging.

Classical fatigue models teach that there is an intrinsic fatigue limit for steels, representing a level of stress that is too low for regular crack growth where every cyclic load propagates a fatigue crack through the material. Modern application with extreme lifetimes has shown that fatigue will still take place in steels with stress levels well below the expected fatigue limit. This relatively new area of study has been named Very High Cycle Fatigue, or VHCF, and describes fatigue failures with a number of load cycles exceeding 107. Fractography of steels that has suffered VHCF tends to reveal an especially rough crack surface adjacent to where the fatigue crack originates, which is typically some form of defect in the bulk of the steel. This area is believed to be critical for VHCF and has been referred to in a number of ways by different studies, but will herein be called Fine Granular Area, or FGA. The aim of this study is to try and get a better understanding of VHCF. This was done by fractography analysis of test specimens of high strength tool steel that suffered fatigue failure at lifetimes ranging from about 106 cycles to 1,9x109 cycles. The lower lifetimes were achieved using hydraulic testing equipment, while the specimens in the VHCF range suffered fatigue failure in ultrasonic testing equipment allowing the application of a cyclic stress at a rate of 20 000 Hz. The resulting fracture surfaces were then investigated using a scanning electron microscope, or SEM, taking special note of the fatigue initiating defects and, in the case of VHCF, the rough area found adjacent to it. In combination with the SEM an elemental analysis of the fatigue initiating defects as well as the bulk of the material was done using energy-dispersive X-ray spectroscopy, or EDS. This was done to find out what the defects consisted of; confirming that they were slags and checking that the composition of the material of the bulk of the specimen matches what was expected. Using light optical microscopy in combination with acid etching of the surface of samples cut out of the test specimens the structure of the steel was investigated. Calculating the local stresses at the location of the fatigue initiating defect was done using FEM in combination with displacement amplitude gathered from the ultrasonic testing equipment. The data gathered was then measured and compared to that of previous studies, using models of prediction and seeing how they match the experimental results. The results suggest that the stress intensity factor at the internal slags is critical for VHCF and that with lower stress intensity factors one can expect longer lifetimes. Another observation is a relatively consistent stress intensity factor at the edge of the FGA combined with the original defect, likely signifying the transition from the creation of FGA to traditional crack propagation. There also seems to be a connection between the size of the FGA and the number of cycles to failure, with larger FGA with increasing lifetimes. The most glaring shortcoming of this study is the amount satisfactory tests conducted, and thus amount of data points, is very low due to the majority of specimens suffered failure at the threading used to connect them to the ultrasonic testing equipment at lifetimes far too low to be relevant. / Klassiska utmattningsmodeller lär ut att det finns en utmattningsgräns för stål, vilket representerar en spänningsnivå som är för låg för regelbunden sprickväxt där varje cyklisk belastning sprider en utmattningsspricka genom materialet. Moderna applikation med extrema livstider har visat att utmattning fortfarande äger rum i stål med spänningsnivåer långt under den förväntade utmattningsgränsen. Detta relativt nya studieområde har fått namnet Very High Cycle Fatigue, eller VHCF, och beskriver utmattningsfall med ett antal belastningscykler som överstiger 107. Fraktografi av stål som har drabbats av VHCF tenderar att ha en särskilt gropig sprickyta som ligger intill där utmattningssprickan har sitt ursprung, vilket typiskt är någon form av defekt i stålets bulk. Detta område tros vara kritiskt för VHCF och har hänvisats till på ett antal sätt av olika studier, men kommer här att kallas Fine Granular Area eller FGA. Syftet med denna studie är att försöka få en bättre förståelse för VHCF. Detta gjordes genom fraktografianalys av testprover av verktygsstål med hög hållfasthet som drabbades av utmattningsbrott vid livstider från cirka 106 cykler till 1,9x109 cykler. De lägre livslängderna uppnåddes med hjälp av hydraulisk testutrustning, medan proverna i VHCF-området drabbades av utmattningsbrott i ultraljudstestutrustning som klarar att applicera en cyklisk stress med en frekvens på 20 kHz. De resulterande sprickytorna undersöktes sedan med hjälp av ett svepelektronmikroskop, eller SEM, med särskild fokus på utmattningsinitierande defekter och, i fallet med VHCF, det grova området som hittades intill det, FGA. I kombination med SEM utfördes en elementanalys av utmattningsinitierande defekter liksom huvuddelen av materialet med energidispersiv röntgenspektroskopi, eller EDS. Detta gjordes för att ta reda på vad inneslutningarna bestod av för att bekräfta att de var slagg samt kontrollera att sammansättningen av materialet i huvuddelen av provet matchar det som förväntades. Med användning av optisk ljusmikroskopi i kombination med syraetsning av ytan på prover som skars ut ur testproverna undersöktes stålets struktur. Beräkning av de lokala spänningarna på platsen för den utmattningsinitierande defekten gjordes med hjälp av FEM i kombination med förskjutningsamplituden som samlats från ultraljudsutrustningen. De insamlade uppgifterna mättes sedan och jämfördes med tidigare studier genom att använda diverse modeller och se hur de matchar de experimentella resultaten. Resultaten antyder att stressintensitetsfaktorn vid inneslutningarna är kritisk för VHCF och att man med lägre stressintensitetsfaktorer kan förvänta sig längre livstid. En annan observation är en relativt konsekvent stressintensitetsfaktor vid kanten av FGA, vilket sannolikt markerar övergången från skapandet eller utbredning av FGA till traditionell sprickutbredning. Det verkar också finnas en koppling mellan storleken på FGA och antalet cykler till fel, med större FGA med ökande livslängd. Den mest uppenbara bristen i denna studie är mängden tillfredsställande tester som genomförts. Därmed är mängden datapunkter mycket låg, detta på grund av att majoriteten av proverna misslyckades vid gängningen som användes för att ansluta dem till ultraljudstestutrustningen vid livstider alltför låga för att vara relevanta.

Este trabalho discutiu a relação entre o espaçamento inter-estrias , isto é, a taxa de propagação da trinca microscópica SL (local) e SP (projetada) e a taxa de propagação macroscópica , da/dN, obtido após o ensaio de propagação de trinca por fadiga. Corpos de prova compacto C(T) foram extraídos na orientação LT do centro de uma placa laminada de liga de alumínio SAE-AMS 7475 T7351 onde posteriormente foram realizados ensaios de fadiga sob carga ou &#916K constantes, à temperatura ambiente de acordo com a Norma ASTM-E647 (1993). Para o ensaio sob carga constante foram obtidos os dados do estágio II e III da curva da/dN vs. &#916K. Para o ensaio de fadiga sob &#916K constante, quatro níveis de &#916K foram utilizados com taxas de crescimento de trinca variando entre 0,15 à 2,4 &#956m/ciclo. Adicionalmente foram realizados ensaios de tenacidade à fratura, KIC nas direções LT e TL conforme a Norma ASTM-E1820 (1999). A análise fratográfica por microscopia eletrônica de varredura foi conduzida no ensaio de fadiga a &#916K constante para determinar os espaçamentos inter-estrias. As taxas de propagação macroscópica e microscópica foram comparadas e boas correlações foram obtidas para um intervalo entre 0,1 a 1,0 &#956m/ciclo. Através da técnica proposta por Berkovitz (1995), o espectro de carregamento foi estimado através da técnica de parametrização do fator K e os resultados foram comparados ao espectro de carregamento real imposto pela máquina de ensaio. Utilizando o espaçamento inter-estrias local, SL, e para valores de &#916K menores que 23 MPam 1/2 (região de Paris), a estimativa de carregamento exibiu um erro menor que 15%. As vidas estimadas em propagação fornecidas pelas taxas microscópicas de propagação de trinca foram comparadas à vida real de propagação obtida a partir da taxa de propagação de trinca macroscópica e o erro absoluto entre ambos os valores foi menor que 15,7 %. Estes resultados sugerem que a vida em fadiga e o espectro de carga podem ser adequadamente estimados utilizando o espaçamento inter-estrias local, SL. / This work discusses the relationship between striation spacing, i.e. the microscopic crack propagation rate, SL (local) e SP (projected), as measured in post-mortem fractographic inspection of fatigue fractured surfaces, and the macroscopic crack propagation rate, da/dN, as monitored during fatigue crack growth tests. Compact tensile specimens C(T) were extracted in LT orientation from the core of a laminated plate of a SAE-AMS 7475-T7351 Al alloy and subsequently fatigue tested either at constant load or at constant &#916K, at room temperature, according to ASTM-E647. For constant amplitude loading fatigue tests, da/dN- &#916K data points were obtained for Regions II and III of crack growth curve. For constant &#916K fatigue tests, four &#916K levels were selected to give crack growth rates typically ranging from 0.15 to 2.4 &#956m/cycle. Additionally, KIC fracture toughness tests were performed in both LT and TL directions, according to ASTM E1820. SEM fractographic analysis was conducted on constant &#916K fatigue specimens, in order to determine striation spacing created during the fatigue test. Macro- and microscopic crack growth rates were compared and good correlation have been obtained for data within the range from 0,1 to 1,0 &#956m/ciclo. Using the technique proposed by Berkovitz, loading history was estimated by the K-factor parametrization and the results were compared to the true loading spectrum imposed by the testing machine. Using the local striation spacing SL and for &#916K values lower than 23 MPam 1/2 (Paris region), the estimated loading exhibits an error less than 15%. Propagation life estimated by local striation spacing (microscopic crack growth rate) was compared to the true propagation life obtained from macroscopic crack growth rate values and the absolute difference between them was less than 15,7%. These results suggest that both life and loading history can be adequately estimated using the local SL striation spacing values.

[pt] O uso de todos os tipos de amianto na construção civil tem diminuído drasticamente devido a problemas sérios de saúde associados a sua manipulação. De fato é previsto banir totalmente o seu uso, dentro de um curto espaço de tempo, nos países desenvolvidos bem como nos em desenvolvimento. Na necessidade de se encontrar um substituto adequado para o amianto, tem-se pesquisado compósitos de argamassa reforçada com fibras vegetais e polpas celulósicas. Devido ao processo de polpação, que remove as impurezas não celulósicas, como a lignina e a hemicelulose, diminuindo o ataque às fibras, sem a necessidade de recorrer a modificações na matriz cimentícia, as polpas celulósicas podem ser o substituto ideal para o amianto. Assim sendo, o principal objetivo desta dissertação é determinar experimentalmente as características mecânicas e os parâmetros de fratura de compósitos de matriz cimentícia reforçada por polpa de bambu refinada e sem refino. As polpas celulósicas foram utilizadas nas porcentagens de 8 e 14 por cento em relação à massa do cimento, porcentagens estas que, conforme a literatura, são associadas à otimização da energia absorvida no ensaio de flexão. A avaliação do comportamento mecânico dos compósitos considerados neste trabalho foi realizada através de ensaios de compressão e impacto, bem como de flexão em três pontos em espécimes não entalhados e em outros contendo entalhes de raios de curvatura diferentes. Propriedades mecânicas, tais como módulo de elasticidade, resistência à compressão, ao impacto e à flexão, bem como integral J na carga máxima, são apresentadas e discutidas em termos de aspectos microestruturais e fractográficos dos corpos de prova ensaiados. / [en] As handling and manipulation of asbestos pose grave health hazards, its use in civil construction has been drastically dwindling and will in fact be completely prohibited, in a few years, in developed countries. With the need arising to find an adequate substitute, vegetable fibers and cellulosic pulps have been considered to be viable alternatives. Taking into account the fact that the process for pulp production entails the removal of impurities, such as lignin and hemicellulose, cellulosic pulps seem to be the ideal substitute to asbestos, as their use does not necessitate modifications in the cementitious matrix. Accordingly, the purpose of this work is to experimentally determine basic mechanical characteristics and pertinent fracture parameters of bamboo pulp reinforced cement. Refined and non-refined pulps were used in the proportions of 8 and 14 percent of the weight of dry cement. These percentages were adopted as they imply, according to literature, in optimizing the energy absorbed by the composite in bend loading. Evaluation of the mechanical behavior of the composites considered in this work was realized by means of compression and impact testing. Three point bend tests were also carried out using unnotched as well as notched specimens of different notch root radii. Mechanical properties such as modulus of elasticity, compressive, impact and bend strengths, and J integral at maximum load are presented and discussed in terms of pertinent microstructural and fractographic aspects of test specimens.

Ce travail de thèse concerne l’acier 16MND5 des cuves des Réacteurs à Eau Préssurisée (REP).L’étude vise à caractériser de manière quantitative la microstructure et à comprendre l’effet desparamètres influents (vitesse de refroidissement, température de revenu …) sur sa formation. D’unpoint de vue expérimental, l’étude est menée grâce à l’utilisation des techniques d’observationcomme la métallographie, le MET, MEB et l’EBSD, et la réalisation de traitements thermiquescontrôlés (dilatométrie notamment).Ces observations visent à identifier les différents constituants de l’acier et de déterminer lesgrandeurs quantitatives les caractériser (tailles, fractions volumiques des différentes phases ainsique leurs orientations cristallographiques).Nous avons dans un premier temps caractérisé de manière complète et quantitative, lamicrostructure de l’acier 16MND5 à l’état de réception (trempé et revenu). L’étude a permis demontrer qu’il existe un gradient de microstructure entre la peau interne et le coeur de l’épaisseur dela virole. La microstructure à coeur est constituée de ferrite proeutectoïde, de bainite et d’amas decarbures, tandis qu’en peau interne on est en présence de bainite et d’amas de carbures.Une campagne d’essais de dilatométrie a été réalisée afin de simuler la microstructure brute detrempe de l’acier 16MND5 et d’observer l’effet de la vitesse de refroidissement, des températuresde transformation sur la microstructure des aciers de cuve. Ces essais ont révélé que lamicrostructure de l’acier 16MND5 après refroidissement est constituée de bainite, d’îlots demartensite et d’austénite résiduelle (M-A) enrichie en carbone. Ce sont ces îlots M-A qui donnentnaissance aux amas de carbures lors du revenu final.L’effet de la composition chimique de cet acier a été étudié grâce à l’utilisation d’une tôle ayant unecomposition chimique plus riche en carbone et en éléments d’alliages. Ce travail a montré quel’augmentation des teneurs en carbone et en éléments d’alliages modifiaient la morphologie et lacristallographie de la ferrite.L’étude des comportements mécaniques des constituants présents en peau interne, quart épaisseur etmi épaisseur a été réalisée grâce à des essais de résilience sur des éprouvettes de mini charpy. Cetteétude a permis de montrer qu’à basse température (-120°C) la peau interne présente de meilleurespropriétés de résilience que le quart et la mi épaisseur de la virole. Des examens de la surfacelatérale des éprouvettes de Charpy ont montré que la présence de ferrite proeutectoïde favorise lagermination de micro-fissures de clivage. / Reactor pressure vessel is the second security barrier of the nuclear reactor and it is elaboratedwith a low carbon steel ( C-0.16%). Due to the large size of the ferrule there is temperatureand cooling rate gradient, which lead to microstructure gradient. To develop predictive modelit is necessary to well describe the microstructure which depend to the processing parameters.We focuse our work in investigating the effect of the processing parameters (cooling rate,chemical composition...) on the final microstructure during phase transformation.To get these informations and better describe the microstructure, we have used someexperimental technics like SEM, EBSD, TEM and Optical Microscopy. The steel used is alow carbon steel with a composition of C-0.16%, Mn-1.32%, Ni-0.72%, Mo-0.49%, Si-0.23%, Cr-0.23%, P-0.010%, S-0.004%. The material has been tempered in the range 635°C-660°C after cooling. Three positions have been chosen for examinations, because the coolingrate is not the same between the center and the edge of the material. The results of theobservations made in the different scale, indicate that the microstructure is mainly baniticwith bainitic ferrite and cementite precipitates. Examinations of the precipitates withextractive replicas in TEM reveal that morphology of cementite particles is complex they arecylinder-shaped particles, short bars particles and skeletal particles. OrientationsRelationships (OR) have been determined between ferrite and cementite particles with thinfoils in TEM by using Selected Area Diffraction, in a large number areas the Isaichev andBagaryatskii OR have been observed, a little Pitsch Petch OR have been obtained. The EBSDmap shows that the bainitic ferrite morphologies are both lath like and polygon. Themisorientations inside the laths are very small (0.5° misorientation point to point) andbetween laths we have the range 49-60° misorientation. The profile of misorientationsbetween point to point indicates higher frequency for the range 49-60°. Charpy test have beenperformed to analyze the effect of the microstructure on the fracture energy at lowtemperature. The results show that the fracture energy decreases when the content ofproeutectoid ferrite is high.

Le but de la thèse est de déterminer l’historique de chargement d’une pièce rompue ou fissurée en service, par analyse des surfaces de fissuration. Pour les analyses de défaillances, les enjeux sont de définir le rôle du chargement dans la défaillance et de déterminer la fraction de durée de vie atteinte lors de la détection de la fissure. Un enjeu complémentaire est d’enrichir la base de données de chargements en service. L’organe choisi pour cette étude est l’essieu-axe ferroviaire. Ainsi, la sollicitation étudiée est en flexion rotative et les matériaux considérés sont les aciers A4T (25CrMo4) et A1N (C40). Suite à une revue bibliographique, quatre méthodes d’analyse quantitative des surfaces de fissuration ont été ciblées et testées, deux ont été retenues et développées. La première est basée sur la quantification des faciès de rupture (stries de fatigue, cupules, fissures secondaires…). La seconde s’appuie sur l’analyse des contraintes résiduelles (fractographie X) en profondeur pour déterminer l’épaisseur de matériau plastifié sous la surface de rupture. Cette profondeur correspond au sillage plastique induit par la propagation de la fissure et est fonction du chargement recherché. / The aim of the thesis is to determine the loading history of a broken or cracked piece in service, by analysing the cracking surfaces. For failure analyses, the issues are to define the role of the loading in the failure and to determine the fraction of lifespan reached when the crack is detected. An additional issue is to expand the in-service loadings database. The component chosen for this study is the railway axle. Thus, the studied stress is in alternate bending and the considered materials are the steels A4T (25CrMo4) and A1N (C40). Following a bibliographic review, four methods for quantitative analysis of cracking surfaces were targeted and tested, two of which were selected and developed. The first one is based on the quantification of fractographic features (fatigue striations, dimples, secondary cracks...). The second is based on the in-depth analysis of the residual stresses (X-ray fractography) to determine the thickness of plasticized material below the fracture surface. This depth corresponds to the plastic wake induced by the crack propagation and is a function of the sought loading.

Este trabalho discutiu a relação entre o espaçamento inter-estrias , isto é, a taxa de propagação da trinca microscópica SL (local) e SP (projetada) e a taxa de propagação macroscópica , da/dN, obtido após o ensaio de propagação de trinca por fadiga. Corpos de prova compacto C(T) foram extraídos na orientação LT do centro de uma placa laminada de liga de alumínio SAE-AMS 7475 T7351 onde posteriormente foram realizados ensaios de fadiga sob carga ou &#916K constantes, à temperatura ambiente de acordo com a Norma ASTM-E647 (1993). Para o ensaio sob carga constante foram obtidos os dados do estágio II e III da curva da/dN vs. &#916K. Para o ensaio de fadiga sob &#916K constante, quatro níveis de &#916K foram utilizados com taxas de crescimento de trinca variando entre 0,15 à 2,4 &#956m/ciclo. Adicionalmente foram realizados ensaios de tenacidade à fratura, KIC nas direções LT e TL conforme a Norma ASTM-E1820 (1999). A análise fratográfica por microscopia eletrônica de varredura foi conduzida no ensaio de fadiga a &#916K constante para determinar os espaçamentos inter-estrias. As taxas de propagação macroscópica e microscópica foram comparadas e boas correlações foram obtidas para um intervalo entre 0,1 a 1,0 &#956m/ciclo. Através da técnica proposta por Berkovitz (1995), o espectro de carregamento foi estimado através da técnica de parametrização do fator K e os resultados foram comparados ao espectro de carregamento real imposto pela máquina de ensaio. Utilizando o espaçamento inter-estrias local, SL, e para valores de &#916K menores que 23 MPam 1/2 (região de Paris), a estimativa de carregamento exibiu um erro menor que 15%. As vidas estimadas em propagação fornecidas pelas taxas microscópicas de propagação de trinca foram comparadas à vida real de propagação obtida a partir da taxa de propagação de trinca macroscópica e o erro absoluto entre ambos os valores foi menor que 15,7 %. Estes resultados sugerem que a vida em fadiga e o espectro de carga podem ser adequadamente estimados utilizando o espaçamento inter-estrias local, SL. / This work discusses the relationship between striation spacing, i.e. the microscopic crack propagation rate, SL (local) e SP (projected), as measured in post-mortem fractographic inspection of fatigue fractured surfaces, and the macroscopic crack propagation rate, da/dN, as monitored during fatigue crack growth tests. Compact tensile specimens C(T) were extracted in LT orientation from the core of a laminated plate of a SAE-AMS 7475-T7351 Al alloy and subsequently fatigue tested either at constant load or at constant &#916K, at room temperature, according to ASTM-E647. For constant amplitude loading fatigue tests, da/dN- &#916K data points were obtained for Regions II and III of crack growth curve. For constant &#916K fatigue tests, four &#916K levels were selected to give crack growth rates typically ranging from 0.15 to 2.4 &#956m/cycle. Additionally, KIC fracture toughness tests were performed in both LT and TL directions, according to ASTM E1820. SEM fractographic analysis was conducted on constant &#916K fatigue specimens, in order to determine striation spacing created during the fatigue test. Macro- and microscopic crack growth rates were compared and good correlation have been obtained for data within the range from 0,1 to 1,0 &#956m/ciclo. Using the technique proposed by Berkovitz, loading history was estimated by the K-factor parametrization and the results were compared to the true loading spectrum imposed by the testing machine. Using the local striation spacing SL and for &#916K values lower than 23 MPam 1/2 (Paris region), the estimated loading exhibits an error less than 15%. Propagation life estimated by local striation spacing (microscopic crack growth rate) was compared to the true propagation life obtained from macroscopic crack growth rate values and the absolute difference between them was less than 15,7%. These results suggest that both life and loading history can be adequately estimated using the local SL striation spacing values.

Plastic flow in bulk metallic glasses (BMGs) localizes into narrow bands, which, in the absence of a microstructure that could obstruct them, propagate unhindered under tensile loading. In constrained deformation conditions such as indentation and at notch roots, extensive shear band formation can occur. A key issue in the context of fracture of BMGs that is yet to be understood comprehensively is how their toughness is controlled by various state parameters. Towards this end, the change in fracture toughness and plasticity with short term annealing above and below the glass transition temperature, Tg, is studied in a Zr-based BMG. Elastic properties like shear modulus, Poisson's ratio as well as parameters defining the internal state like the fictive temperature, Tf, density, and free volume are measured and correlation with the toughness was attempted at. While the elastic properties may help in distinguishing between tough and brittle glasses, they fail to reveal the reasons behind the toughness variations. Spherical-tip nanoindentation and microindentation tests were employed to probe the size, distributions and activation energies of the microscopic plastic carriers with the former and shear band densities with the latter. Results indicate that specimens annealed at a higher temperature, Ta, exhibit profuse shear banding with negligible changes in the local yield strengths. Statistical analysis of the nanoindentation data by incorporating the nucleation rate theory and the results of the cooperative shear model (CSM), reveals that short term annealing doesn't alter the shear transformation zone (STZ) size much. However, density estimates indicate changes in the free volume content across specimens. A model combining STZ activation and free volume accumulation predicts a higher rate in the reduction of the cumulative STZ activation barrier in specimens with a higher initial free volume content. Of the macroscopic physical properties, the specimen density is revealed to be a useful qualitative measure of enhancement in fracture toughness and plasticity in BMGs. We turn our attention next to the brittle fracture in BMGs, with the specific objective of understanding the mechanisms of failure. For this purpose, mode I fracture experiments were conducted on embrittled BMG samples and the fracture surface features were analyzed in detail. Wallner lines, which result from the interaction between the propagating crack front and shear waves emanating from a secondary source, were observed on the fracture surface and geometric analysis of them indicates that the maximum crack velocity to be ~800 m/s, which corresponds to ~0.32 times the shear wave speed. Fractography reveals that the sharp crack nucleation at the notch tip occurs at the mid-section of the specimens with the observation of flat and half-penny shaped cracks. On this basis, we conclude that the crack initiation in brittle BMGs occurs through hydrostatic stress assisted cavity nucleation ahead of the notch tip. High magnification scanning electron and atomic force microscopies of the dynamic crack growth regions reveal highly organized, nanoscale periodic patterns with a spacing of ~79 nm. Juxtaposition of the crack velocity with this spacing suggests that that the crack takes ~10-10 s for peak-to-peak propagation. This, and the estimated adiabatic temperature rise ahead of the propagating crack tip that suggests local softening, are utilized to critically discuss possible causes for the nanocorrugation formation. The Taylor’s fluid meniscus instability is unequivocally ruled out. Then, two other possible mechanisms, viz. (a) crack tip blunting and resharpening through nanovoid nucleation and growth ahead of the crack tip and eventual coalescence, and (b) dynamic oscillation of the crack in a thin slab of softened zone ahead of the crack-tip, are critically discussed. One way of alleviating the fracture-related issues in BMGs is to impart a microstructure to it, which would either impede the growth of shear bands or promote the multiplication of them. One such approach is through the BMG composites (BMGCs) route, wherein a crystalline second phase incorporated in the BMG matrix. There is a need to study the effects of reinforcement content, size and distribution on the mechanical behavior of the BMGC so as to achieve an optimum combination of strength and ductility. For this purpose, an investigation into the microstructure and tensile properties of Zr/Ti-based BMG composites of the same composition, but produced by different routes, was conducted so as to identify “structure–property” connections in these materials. This was accomplished by employing four different processing methods—arc melting, suction casting, semi-solid forging and induction melting on a water-cooled copper boat—on composites with two different dendrite volume fractions, Vd. The change in processing parameters only affects microstructural length scales such as the interdendritic spacing, λ, and dendrite size, δ, whereas compositions of the matrix and dendrite are unaffected. Broadly, the composite’s properties are insensitive to the microstructural length scales when Vd is high (∼75%), whereas they become process dependent for relatively lower Vd (∼55%). Larger δ in arc-melted and forged specimens result in higher ductility (7–9%) and lower hardening rates, whereas smaller dendrites increase the hardening rate. A bimodal distribution of dendrites offers excellent ductility at a marginal cost of yield strength. Finer λ result in marked improvements in both ductility and yield strength, due to the confinement of shear band nucleation sites in smaller volumes of the glassy phase. Forging in the semi-solid state imparts such a microstructure.

Práce je zaměřena na šíření únavových trhlin v módech II, III a II + III v prahové oblasti v kovových materiálech. Byly provedeny experimenty pro ARMCO železo, titan, nikl a austenitickou ocel na třech druzích vzorků pro zatěžování trhliny ve smykových módech. Byl použit zvláštní způsob vytváření iniciační trhliny, který eliminoval efekt zavírání trhliny na začátku smykového zatěžování. Ve všech zkoumaných materiálech byly efektivní prahové hodnoty v módu II přibližně 1,7 krát nižší než v módu III. Měřením úhlů lokálních odklonů a natočení lomových faset s použitím stereofotogrammetrie v SEM bylo usuzováno na tendenci trhliny k vyhýbání do lokálního módu I. Nejmenší úhly byly zjištěny u ARMCO železa pro trhliny v módech II i III, středně velké úhly u titanu a niklu a největší úhly (vyhnutí do čistého módu I) byly pozorovány u austenitické oceli. Tyto rozdíly lze vysvětlit různým počtem dostupných skluzových systémů v krystalových mřížkách daných materiálů. Poměry mezi naměřenými prahovými hodnotami v módu I, II a III byly srovnány s předpověďmi teoretických modelů. Byl navržen analytický vztah pro efektivní prahové hodnoty v módu II, který byl v dobré shodě s experimentálními výsledky. Pomocí efektivních prahových hodnot bylo vyčísleno kritérium pro vyhýbání do módu I, které vedlo ke kritickému úhlu odklonu 40° souvisejícímu s přechodem z lokálního smykového módu do otevíracího módu.