A avaliação da integridade estrutural de dutos pelo uso de corpos-de-prova laboratoriais depende da escolha de corpos-de-prova de geometrias que representem condições de restrições plásticas na frente da trinca, similares às encontradas nas condições operacionais dos dutos. O Núcleo de Ensaios de Materiais e Análise de Falhas, NEMAF do SMM, EESC-USP vem realizando pesquisas para o desenvolvimento de corpos-de-prova e metodologias experimentais que melhor represente esta situação. Entretanto, no caso de dutos existem situações onde a geometria e o tamanho do corpo-de-prova são limitados pelas dimensões do duto. Este trabalho apresenta o desenvolvimento e aplicação de espécimes SE(T) em aço API 5L X70, avaliando a influência da geometria e dimensões do corpo-de-prova na tenacidade à fratura do citado aço, sendo este utilizado na fabricação de dutos para transporte de gás e petróleo. Para isto, foram obtidas curvas de resistência à propagação dúctil de trincas, curvas J-R\'s, utilizando a metodologia do espécime único (single specimen) em conjunto com a técnica da variação da flexibilidade elástica (unloading elastic compliance), medida na boca da trinca (CMOD) que fornece ao mesmo tempo a área plástica abaixo da curva de carregamento versus deslocamento e o tamanho da trinca, segundo a norma de ensaios ASTM E1820-05. Foram ensaiados corpos-de-prova SE(T) com trincas rasa (a/W=0,2) e profunda (a/W=0,5) e razão W/B de 2,5 e 1,0, com a finalidade de garantir que o ensaio seja realizado em dominância de um estado plano de deformação como recomendado pela referida norma, para outros tipos de corpos-de-prova. Dos resultados observou-se que, independente do tamanho de trinca inicial adotado, não foram observadas diferenças significativas nas curvas J-R. Este fato pode ser comprovado nos casos de W/B = 2,5 e 1,0, sendo obtidas curvas J-R similares para cada caso, independente do valor de a/W. Entretanto, na grande maioria dos CDP\'s, foi obtida uma propagação dúctil de trinca anômala, ou seja, trincas que apresentam um tunelamento acentuado, decorrente de um elevado estado de tensão plana próximo das laterais, mesmo com o entalhe lateral de 20% da espessura. Os corpos-de-prova com W/B = 1,0 foram capazes de produzir curvas J-R, sem que as trincas apresentassem tunelamento e que os valores médios de trinca (ai e af) medidos conforme a norma (ASTM, 2005), são bastante próximos dos valores obtidos pelo método da variação de flexibilidade elástica. As razões para este fato são discutidas em detalhes. De um modo geral as delaminações, quando existente, não permitem uma correta medição do tamanho de trinca. Ainda, contrário à observação de outros pesquisadores, neste trabalho, foi observado que em vários casos as delaminações induziram fratura instável. / The evaluation of pipes´ structural integrity from laboratories specimens depends on choosing the right specimen geometry that is able to present the conditions of plastic constrain at the crack tip, similar to the one found in the pipes´ operational conditions. The NEMAF Group from SMM, EESC-USP has been performing studies in this area, trying to develop specimen´s geometry that is able to represent this situation, as well as the necessary experimental methodologies to evaluate the fracture toughness of pipes. However, in some cases, the pipe size is a limiting factor in determining the specimen size and geometry. In this work is presented the development and application of specimens SE(T), evaluating the influence of the geometry and dimensions of the specimens on the fracture toughness of API 5L X70 steel, regularly used in the pipes for gas and petroleum transportation. Therefore, the resistance curves to ductile crack propagation, J-R`s curves, using the single specimen methodology, together with the variation of the elastic compliance technique (multiple unloading), measure at the crack mouth (CMOD) that provides both the plastic area under the load x displacement curve and crack size, according to the ASTM E1820-05 standard. The SE(T) specimens with shallow (a/W=0.2) and deep (a/W=0.5) cracks and W/B ratio of 2.5 and 1.0 trying to reduce the amount of plastic deformation and a straight crack front, as well as a dominance of a plane strain state at the crack tip, as recommended by the ASTM E1820-05 standard for other specimens type. From the results it was observed that, independent of the initial a/W, no significant differences were observed in the J-R curves. This fact is verified in both cases, this is, W/B = 2.5 and 1.0. However, in the great majority of CDP\'s with W/B = 2.5, it was obtained an anomalous crack propagation during testing, in other words, they presented an accentuated tunneling due to a high plane tension state near the CDP´s lateral faces, even with the side groove of 20% thickness. The specimens with W/B = 1.0 were capable to produce J-R curves with straight crack fronts, this is, without tunneling, allowing the measurement of medium values of the crack (ai e af) according to the ASTM E1820-05 standard. The reasons for this fact are discussed in details in this work. In general, the split, when present, did not allow a correct crack size measurement. Still, contrary to the other researchers\' observation, in this work, it was observed that in several cases the splits were able to induced unstable fracture.

Aplicações de alto desempenho, como as de dutos utilizados no transporte de derivados de petróleo, exigem materiais com uma combinação excepcional de propriedades mecânicas, dentre as quais, elevada resistência mecânica, tenacidade e resistência à fadiga. O aço API 5L X70 com adição de nióbio apresenta-se, quando comparado com o API 5L X70 padrão, como sendo uma opção para a melhora em seu processo de fabricação, sendo sua composição química diferenciada, devido a um maior teor de nióbio. A Arcelor Mittal Tubarão tem mostrado interesse em fabricar aços API X70/X80, sem a adição de V e com adições de Nb acima do recomendado pela Petrobras. O objetivo principal deste trabalho é o estudo da resistência mecânica e de tenacidade à fratura de dois aços API 5L X70, com teores de Nb de 0,06% e Nb de 0,09% em peso, processados conforme processo HSM Arcelor Mittal Tubarão. Para o atendimento deste objetivo, serão executadas a caracterização microestrutural conforme norma ASTM E3, ensaios de tração conforme ASTM E8M e ensaios de tenacidade à fratura conforme a norma ASTM E1820 com obtenção das curvas J-R\'s. Foram retirados corpos de prova da região de material base, região da solda e zona termicamente afetada. A partir dos resultados obtidos observa-se que o processo de laminação controlada a quente da Arcelor Mittal, produziu microestruturas bastante similares para ambas as composições, produzindo parâmetros de resistência mecânica similares e que atenderam o especificado pela Norma API 5L X70, nível PSL2. As soldas se apresentaram, a partir de valores de dureza, ligeiramente superiores ao do metal base (overmatch), sendo o resultado de microestruturas bastante similares. Os ensaios para obtenção das curvas J-R foram capazes de apresentar resultados representativos da resistência à propagação dúctil de trinca, para as espessuras de tubos estudadas. Estes resultados indicaram elevada resistência a propagação dúctil de trinca em ambos os aços, sendo que, o MB do aço NNb apresentou resistência superior ao ANb. O MS apresentou curvas J-R bem inferiores às do MB e ZTA. Estas diferenças foram atribuídas a composição microestrutural de cada região. / High performance applications such as pipelines used to transport oil products require materials with an exceptional combination of mechanical properties, such as high mechanical strength, toughness and fatigue resistance. The API 5L X70 steel with enhanced niobium as an option to the production of this type of HSLA steel. Arcelor Mittal, Tubarão/Brazil has great interest in producing API 5L X70/X80 steels, without V and with Nb content above the recommended by Petrobras. Thus, the main objective of this thesis is the study of the mechanical strength and fracture toughness of API 5L X70 steel with Nb content of 0.06% Nb and 0.09% by weight processed as HSM Arcelor Mittal Tubarão process. To meet this goal, microstructural characterization following the ASTM E3, tensile tests following the ASTM E8M and Elastic Plastic Fracture toughness testing, according to ASTM E1820, were carried out. Specimens were taken from the base material region, weld bead and heat affected zone. From the results obtained it was observed that the controlled hot rolling process from ArcelorMittal, produced very similar microstructures for both compositions, as a consequence similar mechanical resistance and both met the criteria specified by the API Standard 5L X70, PSL2 level. The produced girth welds presented hardness values slightly higher than those from the base metal (overmatch), and resulted in very similar microstructures. The fracture toughness tests were able to provide valid JR curves that are representative results of resistance to ductile crack propagation for this pipe thickness. Both steels presented resistance to ductile crack propagation, and that the MB of the NNB steel showed superior resistance to the ANb steel. MS showed the lowest J-R curves, while MB and ZTA presented similar behavior. These differences were attributed to microstructural composition of each region.

Objetivo: Analisar a influência da matriz orgânica, do conteúdo inorgânico e do tratamento térmico (TT) sobre diferentes propriedades de compósitos experimentais, tais como o grau de conversão (GC), tenacidade à fratura (KIC), resistência à flexão (RF) e módulo de elasticidade (ME). Métodos: Para o experimento foram analisadas seis formulações de compósitos experimentais com proporções molares de Bis-GMA:TEGDMA de 5:5 e 7:3, a carga utilizada foi o vidro de bário, nas concentrações de 30, 50 e 70% em peso, e os fotoiniciadores a amina e canforoquinona. O GC foi analisado através da espectroscopia no infra-vermelho (FTIR) (n=5). A KlC foi avaliada pelo método single-edge notched beam (SENB). As imagens das superfícies de fratura foram capturadas por um estereomicroscópio e a KlC calculada (n=10). A análise da RF e ME foi realizada através do teste dos três pontos (n=10). Para todos os fatores de variação estudados, metade dos espécimes imediatamente após à confecção receberam TT em estufa convencional, a 170º C por 10 minutos e a outra metade não. Após 24 horas, as amostras foram destinadas de acordo com os ensaios realizados. Os dados foram analisados utilizando ANOVA/Tukey para o grau de conversão, tenacidade à fratura e resistência à flexão, e, Kruskal-Wallis para o módulo de elasticidade (=5%). Resultados: Na análise do GC (%) foi observada significância estatística para os três fatores de variação analisados individualmente (monômero, carga e TT), como também, para a interação monômero x TT (p<0,001). Para a KIC e RF, as alterações significantes foram observadas apenas nos três fatores de variação (monômero, carga e TT) analisados individualmente (p<0,001). Para o ME, os fatores individuais (monômero, carga e TT), a interação carga x TT apresentaram significância estatística (p<0,001), bem como a interação monômero x carga (p=0,001). Conclusões: A matriz orgânica e o conteúdo inorgânico dos compósitos experimentais influenciaram o GC, a KIC, a RF e ME, e o TT promoveu melhorias nas propriedades estudadas. / Objective: To analyze the influence of organic matrix, the inorganic content and thermic treatment (TT) on different properties of experimental composites, such as the degree of conversion (DC), fracture toughness (KIC), flexural strength (FS) and elastic modulus (EM). Methods: This experiment analyzed six formulations of experimental composites with 5:5 and 7:3 molar proportions of Bis-GMA: TEGDMA. The load used was barium glass at concentrations of 30, 50 and 70% by weight and the photoinitiators, camphorquinone and amine. GC was analyzed by infrared spectroscopy (FTIR) (n=5). The KIC was evaluated by a \"single-edge notched beam\" (SENB). The images of the fracture surfaces were captured by a stereomicroscope and KIC calculated (n=10). The analysis FS and EM were performed by testing three points (n=10). For all the variation factors studied, half of the specimens immediately after the preparation received TT in conventional oven at 170º C for 10 minutes and the other half not. After 24 hours, the samples were designed according to the tests. Data were analyzed using ANOVA/Tukey the degree of conversion, fracture toughness and flexural strength, and Kruskal-Wallis test for the elastic modulus (=5%). Results: Analysis of GC (%) statistical significance was observed for the three variation factors analyzed individually (monomer, filler and TT), as well as for the interaction monomer x TT (p <0.001). For KIC and FS, significant changes were observed only in the three variation factors (monomer, filler and TT) analyzed individually (p<0.001). For EM, the individual factors (monomer, filler and TT) TT x filler interaction showed statistical significance (p <0.001), as well as the monomer x filler interaction (p = 0.001). Conclusions: The organic matrix and inorganic content of experimental composites influenced the GC, KIC, FS and EM, and the TT caused improvements in the properties studied.

Diante da evolução da composição das resinas compostas e do lançamento de compósitos do tipo bulk fill, faz-se necessário o estudo do desempenho dessa nova classe de materiais. Para isso, o presente estudo teve como objetivo avaliar propriedades como grau de conversão (GC) , dureza Knoop (KHN), resistência à flexão (RF) e tenacidade à fratura (KIC) de sete compósitos bulk fill (EverX Posterior, EXP; Filtek Bulk Fill Flow, FBFF; Fill-Up!, FU; SonicFill, SF; Surefil SDR, SDR; Tetric EvoCeram Bulk Fill, TECBF; Venus Bulk Fill, VBF) e um compósito nanohíbrido convencional (Charisma Diamond, CD). De forma complementar, foi realizado tratamento térmico a 170 °C por 10 minutos para melhor compreensão do comportamento desses materiais quanto ao potencial de conversão e à indução de tensões na interface carga/matriz. A avaliação do GC (n=3) foi realizada através de espectroscopia FTIR, a leitura da dureza Knoop foi realizada nas superfícies do topo e da base (n=3), e os ensaios de RF de três pontos (n=10) e KIC (n=10) em máquina de ensaios universais. Os resultados obtidos foram submetidos à analise de variância (complementados pelo teste de Tukey) ou teste Kruskal-Wallis, com nível de significância de 5%. A análise do GC (%) revelou diferença entre os materiais testados, sendo que todas as resinas bulk fill apresentaram valores maiores que a resina convencional: SF (75,7) > VBF (66,7) = EXP (66,4) = SDR (62,8), sendo esta também semelhante a FU (60,0); FU, TECBF (56,6), FBFF (56,6) e CD (54,5) apresentaram conversão semelhante. Os valores de KHN variaram de acordo com o material e com a superfície: apenas SF apresentou KHN semelhante (na superfície do topo) a CD, entretanto não foi possível realizar a leitura da superfície da base deste último material; SF, TECBF e FBFF apresentaram valores de KHN diferentes nas superfícies topo e base; EXP, FU, SDR e VBF mantiveram os valores de dureza do topo semelhantes à superfície da base. Para a RF (MPa), os resultados variaram de acordo com o material: EXP (122,54) = SF (101,09) = CD (99,15), sendo estes dois últimos semelhantes a FU (83,86) e TECBF (82,71), os quais não diferiram da resina SDR (65,18); esta última também mostrou comportamento semelhante a FBFF (60,85) e VBF (59,90). Quanto ao KIC (MPa.mm0,5), EXP (3,35) apresentou o maior valor, semelhante a SF (2,42), que por sua vez também foi igual ao compósito convencional CD (2,01); CD apresentou KIC semelhante a SDR (1,74); SDR = VBF (1,59) = TECBF (1,57); TECBF, FU (1,54) e FBFF (1,37) apresentaram valores semelhantes. Na dependência do material, o tratamento térmico aumentou os valores dos parâmetros estudados, apontando limitações da reação de polimerização dos compósitos estudados. Com base nos resultados obtidos, podese concluir que: resinas bulk fill apresentam elevado GC, superior à resina convencional estudada; a nova classe de materiais restauradores é capaz de polimerizar em profundidade e alguns materiais apresentam KHN semelhantes no topo e na base de espécimes de 4 mm de profundidade; RF e KIC variaram de acordo com o material, e o compósito EXP apresentou os maiores valores para ambos os testes. / Facing the evolution of the resin composites and the release of the bulk-fill composite type, it is necessary to study the performance of this new class of materials. For this, the present study aimed to evaluate properties such as degree of conversion (DC), Knoop hardness (KHN), flexural strength (FS) and fracture toughness (KIC) of seven bulk-fill composites (EverX Posterior, EXP; Filtek Bulk Fill Flowable, FBFF; Fill-Up!, FU; SonicFill, SF; Surefil SDR, SDR; Tetric EvoCeram Bulk Fill, TECBF; Venus Bulk Fill, VBF) and a conventional nanohybrid composite (Charisma Diamond, CD). Complementarily, heat treatment was performed at 170 °C for 10 minutes for better understanding the behavior of these materials. Evaluation of DC (n=3) was performed by FTIR spectroscopy, the evaluation of Knoop hardness was made on the top and bottom surfaces (n=3), and three point bending test (n=10) and KIC (n=10) were evaluated on a universal testing machine. The results were submitted to analysis of variance (complemented by Tukey test) or Kruskal-Wallis test with 5% significance level. Analysis of DC (%) revealed differences between tested materials, and all bulk-fill resins had higher values than the conventional resin: SF (75.7) > VBF (66.7) = EXP (66.4) = SDR (62.8), which was also similar to FU (60.0); FU, TECBF (56.6), FBFF (56.6) and CD (54.4) showed similar conversion. KHN values showed variations according to the material and the surface: only SF showed a similar KHN (on the top surface) to CD, however it was not possible to read the bottom surface of this latter material; SF, TECBF and FBFF presented different KHN values on the top and bottom surfaces; EXP, FU, SDR and VBF maintained top and bottom similar hardness values. For FS (MPa), the results varied according to the material: EXP (122.54) = SF (101.09) = CD (99.15), the latter two being similar to FU (83.86) and TECBF (82.71), which did not differ from SDR resin (65.18); the latter showed similar behavior to FBFF (60.85) and VBF (59.90). As for KIC (MPa.mm0.5), EXP (3.35) had the highest value, similar to SF (2.42), which in turn was also equal to the conventional composite CD (2.01); CD presented KIC similar to SDR (1.74); SDR = VBF (1.59) = TECBF (1.57); TECBF, FU (1.54) and FBFF (1.37) were similar. Depending on the material, heat treatment increased the values of the parameters, pointing limitations of polymerization reaction of the studied composites. Based on these results, it can be concluded that: bulk fill resins have high DC, higher than the conventional resin studied; the new class of restorative materials is capable of polymerizing in depth and some materials exhibited similar KHN at the top and bottom surfaces of 4 mm depth specimens; FS and KIC varied according to the material, and the EXP composite showed the highest values for both tests.

Os aços de alta resistência e baixa liga (ARBL) são amplamente empregados nas indústrias automotiva, petrolífera e naval por apresentarem boas propriedades mecânicas e boa soldabilidade. A seleção do processo de soldagem utilizado para a fabricação de componentes depende de vários fatores, entre eles a qualidade do cordão de solda e a capacidade de produção, ambas obtidas ao se utilizar a soldagem a laser, processo que vem sendo cada vez mais utilizado nas indústrias. As propriedades dos cordões de solda são afetadas pelo processo de soldagem e pelos parâmetros do processo, e o conhecimento do desempenho mecânico do cordão de solda é essencial para garantir a confiabilidade da união soldada. A caracterização mecânica de cordões de solda é complexa devido aos diversos fatores que podem afetá-lo, como as alterações metalúrgicas, diferentes propriedades mecânicas nas regiões do cordão de solda, presença de descontinuidades, tensão residual e complexo estado de tensão devido à geometria da junta. O presente trabalho obteve uniões entre chapas de aço ARBL pelo processo a laser em duas condições diferentes: com alto aporte térmico e baixo aporte térmico. A utilização de diferentes aportes térmicos gerou cordões de solda com microestruturas distintas, e avaliou-se, deste modo, o comportamento mecânico associando-o à microestrutura gerada. Para a avaliação da microestrutura utilizou-se da microscopia óptica e eletrônica de varredura, e para a caracterização mecânica empregou-se a aferição da dureza, ensaio de tração, ensaio de tenacidade à fratura, avaliada pelo CTOD, e ensaio de propagação da trinca por fadiga. Devido às alterações metalúrgicas causadas pelos diferentes aportes térmicos verificou-se diferente comportamento mecânico entre os cordões de solda em função da microestrutura obtida. / High-strength low-alloy steels (HSLA) are widely used in the automotive and oil industries due to their good mechanical properties and good weldability. The selection of the welding process used to manufacture components depends on several factors, including the quality of the weld bead and the production capacity, both obtained when using laser welding, a process, which is being increasingly used in the industries. The weld beads properties are affected by the welding process and by its parameters, and the knowledge of the weld bead mechanical performance is essential to ensure the reliability of the welded joint. The weld beads mechanical characterization is complex due to various factors that may affect it, such as metallurgical changes, different mechanical properties in the regions of the weld bead, presence of discontinuities, residual stress and complex state of tension due to the geometry of the joint. The present work obtained the joining of HSLA steel sheets by laser process in two different conditions, with high heat input and low heat input. The use of different heat inputs produced weld beads with different microstructures; therefore, the welded joints were evaluated according to their mechanical behavior, relating it with the microstructural generated. For the microstructure evaluation, optical microscopy and scanning electron microscopy were used, and for the mechanical characterization hardness determination, tensile test, fracture toughness test (evaluated by CTOD) and fatigue crack propagation were performed. Due to the metallurgical changes caused by the different heat inputs, a different mechanical behavior was observed between the weld beads as a function of the microstructure obtained.

Os aços ARBL tem cada vez mais destaque na produção de auto-peças. Os atrativos são elevados limites de escoamento e resistência, resistência química, boa soldabilidade e estampabilidade. Estes atrativos fazem dos aços ARBL itens importantes no desenvolvimento de novos produtos, projetos de redução de custo e melhoria de processos. As inovações tecnológicas e a exigência de produtos cada vez mais robustos em sua aplicação têm levado a indústria a buscar em outros tipos de materiais as propriedades que possam satisfazer as especificações de projetos. O objetivo deste trabalho é entender a microestrutura e o comportamento mecânico da região soldada de dois aços ARBL e compara-los ao aço SAE1010AA visando a produção de aro para rodas de caminhão e ônibus. O processo de soldagem utilizado é conhecido como soldagem por resistência, onde a união das extremidades do blank é feita por aquecimento através de uma diferença de potencial sem adição de material. Os aços ARBL utilizados são o RD480 produzido pela CSN e o S275JR produzido pela CST. As uniões soldadas são caracterizadas por meio de ensaios de tração, tração com entalhe, impacto e avaliação da tenacidade à fratura através de medidas de CTOD. Os resultados obtidos nos ensaios mecânicos e as análises de microetrutura mostraram que os aços ARBL estudados possuem características mecânicas que os tornam ótimas opções na substituição do aço SAE1010AA na produção de aros para rodas sem câmara. Este trabalho teve o apoio da IOCHPE MAXION, divisão de rodas e chassis. / The HSLA steels have been increasingly highlighted in the production of automotive parts. Their attractives are high yield and ultimate strengths, chemical resistance, weldability and formability. These features make the HSLA steels an important item in the development of new products, design for cost reduction and process improvement. The technological innovations and product requirements have lead the industries to seek for new materials with properties that could meet the design specifications. The objective of this work is to understand the microstructure and the mechanical behavior of the weld zone of two types of HSLA steels and compare with the current steel (SAE1010AA) used in the manufature of rim wheels for truck and bus. The welding process used is this study is known as Flash weld, which is commonly used in the manufacture of wheel rims. The chosen HSLA steels are the RD480 (From CSN Inc.) and S275JR (From CST Inc.). The welded joints are characterized by means of notched and unotched tensile tests, impact tests and fracture toughness evaluation through CTOD measurements. The results obtained in mechanical testing and analysis showed that microetrutura studied HSLA steels have mechanical properties that make them great options in replacing steel SAE1010AA in the production of wheel rims to tubeless. This work was supported by IOCHPE-MAXION, division of wheels and chassis.

Bei der Beurteilung der Sicherheit bestehender Konstruktionen aus altem Baustahl (i. A. Flussstahl) und der Entscheidung über notwendige Instandsetzungs- und Verstärkungsmaßnahmen ist der Nachweis ausreichender Werkstoffzähigkeit (der Sicherheit gegen ein sprödes Versagen) von wesentlicher Bedeutung. Die in DIN EN 1993-1-10 normativ geregelten Nachweismethoden zur Beurteilung der Sprödbruchgefährdung wurden basierend auf umfangreichen bruchmechanischen Untersuchungen entwickelt. Sie gelten für Schweißkonstruktionen und „Stähle aus neuerer Zeit“ mit in der Regel hohen Zähigkeitswerten. Die Quantifizierung der Zähigkeit in Werkstoffnormen erfolgt durch Kerbschlagbiegeversuche. Die Beziehung zwischen der Übergangstemperatur der Kerbschlagarbeit und der Referenztemperatur der Bruchzähigkeit wird durch die modifizierte Sanz-Korrelation hergestellt, die nur für diese Stähle abgeleitet wurde. Das in der Norm verankerte Verfahren ist für alte Flussstahlkonstruktionen mit Lochschwächung durch Niet- und Schraubenverbindungen nicht geeignet. Einerseits unterscheiden sich Kerbwirkung und Eigenspannungszustand von geschweißten und genieteten Konstruktionen und damit die Zähigkeitsanforderungen wesentlich voneinander. Auf der anderen Seite unterliegen die Zähigkeitseigenschaften von Flussstählen deutlich größeren Streuungen. In der vorliegenden Arbeit werden experimentelle und rechnerische Untersuchungen zum Sprödbruchverhalten gelochter Konstruktionen aus altem Flussstahl vorgestellt. Wesentlicher Bestandteil sind dabei die umfangreichen Werkstoffanalysen zur Ermittlung der bruchmechanischen Werkstoffzähigkeit im spröd-duktilen Übergangsbereich nach dem Master-Curve-Konzept (ASTM E1921). Die Auswertungen belegen, dass in Abhängigkeit des Herstellungsverfahrens unterschiedliche Werkstoffgüten definiert werden können. Um den Einfluss des Stanzens von Löchern auf das Sprödbruchverhalten alter Flussstähle zu beurteilen, werden Gefügeuntersuchungen und Mikrohärtemessungen durchgeführt. Ausgehend von einer umfassenden Analyse typischer Konstruktionsformen bestehender Tragwerke des Stahlhochbaus erfolgen bruchmechanische FE-Berechnungen an Anschlüssen von Winkelprofilen zur Bestimmung der Zähigkeitsanforderungen. Die dabei gewonnenen Ergebnisse des Spannungsintensitätsfaktors werden durch Modifikation bekannter Lösungen aus der Fachliteratur für die weitere Anwendung aufbereitet. Darauf aufbauend wird für die untersuchten Konstruktionsdetails im Rahmen einer bruchmechanischen Sicherheitsanalyse ein praxisgerechtes Verfahren zur Beurteilung der Sprödbruchgefährdung genieteter und geschraubter Bauteile abgeleitet. Mit Hilfe statistischer Methoden werden Streuungen der Festigkeits- und Zähigkeitskennwerte der Flussstähle erfasst und nach der Verifizierung durch Bauteilversuche in ein semi-probabilistisches Nachweiskonzept überführt.

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.

Laser surface treatment of engineering ceramics offers various advantages in comparison with conventional processing techniques and much research has been conducted to develop applications. Even so, there still remains a considerable gap in knowledge that needs to be filled to establish the process. By employing a fibre laser for the first time to process silicon nitride (Si3N4) and zirconia (ZrO2) engineering ceramics, a comparison with the CO2 and a Nd:YAG lasers was conducted to provide fundamental understanding of various aspects of the laser beam-material interaction. Changes in the morphology, microstructure, surface finish, fracture toughness parameter (K1c) were investigated, followed by thermal finite element modelling (FEM) of the laser surface treatment and the phase transformation of the two ceramics, as well as the effects of the fibre laser beam parameter - brightness (radiance). Fibre and CO2 laser surface treatment of both Si3N4 and ZrO2 engineering ceramics was performed by using various processing gases. Changes in the surface roughness, material removal, surface morphology and microstructure were observed. But the effect was particularly more remarkable when applying the reactive gases with both lasers and less significant when using the inert gases. Microcracking was also observed when the reactive gases were applied. This was due to an exothermic reaction produced during the laser-ceramic interaction which would have resulted to an increased surface temperature leading to thermal shocks. Moreover, the composition of the ceramics was modified with both laser irradiated surfaces as the ZrO2 transformed to zirconia carbides (ZrC) and Si3N4 to silicon dioxide (SiO2) respectively. The most appropriate equation identified for the determination of the fracture toughness parameter K1c of the as-received, CO2 and the fibre laser surface treated Si3N4 and ZrO2 was K1c=0.016 (E/Hv) 1/2 (P/c3/2). Surfaces of both ceramics treated with CO2 and the fibre laser irradiation produced an increased K1c under the measured conditions, but with different effects. The CO2 laser surface treatment produced a thicker and softer layer whereas the fibre laser surface treatment increased the hardness by only 4%. This is inconsiderable but a reduction in the crack lengths increased the K1c value under the applied conditions. This was through a possible transformation hardening which occurred within both engineering ceramics. Experimental findings validated the generated thermal FEM of the CO2 and the fibre laser surface treatment and showed good agreement. However, a temperature difference was found between the CO2 and fibre laser surface treatment due to the difference in absorption of the near infra-red (NIR) wavelength of the fibre laser being higher than the mid infra-red (MIR) wavelength of the CO2 laser. This in turn, generated a larger interaction zone on the surface that was not induced further into the bulk, as was the case with the fibre laser irradiation. The MIR wavelength is therefore suitable for Viability and Characterization of the Laser Surface Treatment of Engineering Ceramics 3 the surface processing of mainly oxide ceramics and surface treatments which do not require deep penetration. Phase transformation of the two ceramics occurred at various stages during the fibre laser surface treatment. The ZrO2 was transformed from the monoclinic (M) state to a mixture of tetragonal + cubic (T+C) during fibre laser irradiation and from T+C to T and then a partially liquid (L) phase followed by a possible reverse transformation to the M state during solidification. The Si3N4 transformed to a mixture of α-phase and β-phase (α→ α+β) followed by α+β and fully transforms from α+β → β-phase. What is more, is a comparison of the fibre laser-beam brightness parameter with that of the Nd:YAG laser. In particular, physical and microstructural changes due to the difference in the laser-beam brightness were observed. This research has identified the broader effects of various laser processing conditions, as well as characterization techniques, assessment and identification of a method to determine the K1c and the thermal FEM of laser surface treated engineering ceramics. Also, the contributions of laser-beam brightness as a parameter of laser processing and the influence thereof on the engineering ceramics have been identified from a fundamental viewpoint. The findings of this research can now be adopted to develop ceramic fuel cell joining techniques and applications where laser beam surface modification and characterization of engineering ceramics are necessary.

Le but de ce travail est d'étudier l'effet de la teneur en cuivre et de la valence des atomes de cuivre sur la structure et les propriétés mécanique du verre. Des verres de zinc- et plomb- cuivre borate ont été étudiés. Les changements structurels avec le remplacement de PbO ou ZnO par CuO sont observés par réflectance infrarouge et Raman. L'état d'oxydation, l'environnement du site et la liaison caractéristique d'ions de cuivre ont été étudiés par spectroscopie optique et de résonance de spin électronique. Les propriétés mécaniques ont été déterminées et corrélées à la structure du verre et à sa composition, en mettant l'accent sur les propriétés élastiques, le comportement d'indentation (dureté et micro-fissures), la ténacité et la dépendance à la température de l'élasticité. Le cuivre a une tendance à stabiliser le bore en coordinence trigonale et donne une structure de type métaborate plus homogène. L'ajout d'ions de cuivre au verre métaborate améliore les performances mécaniques (modules d'élasticité et dureté), et diminue la sensibilité à la température ainsi que le taux de ramollissement des verres au plomb. Toutefois, l'ajout d'ions de cuivre dans les verres au zinc a des effets opposés sur ces propriétés. Les changements chimiques à la surface des verres de borates de cuivre et de zinc après traitement thermique sont également étudiés. L'étude par nanoindentation et par rayage montre que la couche cristallisée améliore la résistance mécanique de la surface du verre. / The aim of this work is to study the effect of copper content and copper valence on the structural and mechanical properties of glass. Zinc- and lead- copper borate glasses were studied. Their structural changes with the substitution of CuO for ZnO or PbO are followed by Raman and reflectance infrared. The oxidation state, site environment and bonding characteristic of copper ions are studied by optical and electron spin resonance spectroscopy. The mechanical properties were determined and correlated to the glass structure and composition, with a particular emphasis on the elastic properties, sharp indentation behavior (hardness and micro-cracking), toughness and temperature dependence of elasticity. Copper tends to stabilize trigonal boron and gives a more homogeneous metaborate structure. Adding copper ions to the metaborate glass clearly improves the mechanical performance (elastic moduli and hardness), in the meantime decreases the temperature sensitivity and soften rate of lead borate glasses. However, adding copper ions in zinc borate glasses has opposite effects on these properties. The chemistry changes at zinc-copper-borate glass surface after heat-treatment are also studied. Investigation of the nanoindentation and scratch behavior show that the crystallized layer improves the mechanical resistant of glass surface.