Resumo: Neste trabalho foi feita uma análise detalhada dos micromecanismos de iniciação da fratura em amostras entalhadas para cinco aços e duas ligas de alumínio. Com esse objetivo foram obtidas curvas de transição frágil-dúctil e de tenacidade à fratura em função do raio da raiz do entalhe, e realizados ensaios interrompidos antes da fratura da amostra. Análises fractográficas e micrográficas das regiões de iniciação das fraturas foram realizadas por microscopia eletrônica de varredura. A variação dos micromecanismos de iniciação em função da variação da capacidade plástica local na raiz dos entalhes, como induzida pela variação da temperatura de ensaio e pela variação do raio da raiz, foi analisada. De um modo geral, três tipos de micromecanismos de iniciação foram observados. Um frágil, em que a iniciação envolve a nucleação de uma microtrinca à frente do entalhe e sua subsequente propagação instável. Dois dúcteis, um pela ruptura por cisalhamento localizado ao longo de linhas de cisalhamento máximo formadas na raiz do entalhe, e outro pela formação de microcavidades cuja ligação entre si e a ponta do entalhe envolve um processo misto de cisalhamento localizado e de coalescência de microcavidades. Aspectos de modelos que relacionam tenacidade com a microestrutura foram discutidos com base nos micromecanismos observados. / Abstract: In this study a detailed analysis of the micromechanisms of the fracture initiation in notched specimens was made, for five steels and two aluminum alloys. With that purpose brittle/ductile transition and fracture toughness x r1/2 curves were obtained, and interrupted tests before the fracture of the sample were used. Fractographic and micrographic analysis of the fracture initiation areas were accomplished by scanning electron microscopy. The variation of the initiation micromechanisms in function of the variation of the local plastic capacity in the notch root, as induced by the variation of the test temperature and by the variation of the notch root radius, was analyzed. In a general way, three types of initiation micromechanisms were observed. A brittle one, where the initiation involves the microcrack nucleation ahead of the notch and its subsequent unstable propagation. Two ductile, one by localized shear rupture along the maximum shear lines formed in the notch root, and other by microvoids nucleation whose link to each other and the notch tip involves a mixed process of localized shear and microcavoid coalescence. Aspects of relating models of fracture toughness with microstructure were discussed, based in the observed micromechanisms. / Orientador: Fathi Aref Ibrahim Darwish / Coorientador: Luís Rogério de Oliveira Hein / Banca: Valdir Alves Guimarães / Banca: Marcelo dos Santos Pereira / Banca: Luiz Carlos Pereira / Banca: Marcos Venicius Soares Pereira / Doutor

Carbon capture and storage (CCTS) is a transitional technology offering a nearterm method of mitigating climate change. Pipelines are considered to be the most suitable systems for CCTS; however, structural integrity of pipeline has to be guaranteed in order for this technology to become a practical technical solution. The investigation detailed here is based on a systematic experimental approach to investigate the structural integrity of API X100, X60 and X70 steels exposed in simulated flue-gas under dynamic conditions. A core of the structured experiments through some methods such as aging test, tensile properties, fracture toughness, residual stress and engineering critical assessment was accomplished in parent material and exposed samples on flue-gas. The temperature range of evaluation for tensile test covers -70C to 21C while fracture toughness was over the range -196C to 21C. Tensile properties of virgin material show that steels meet standard specification while aging samples do not show significant scatter compared with parent steels. Ovalisation of the fracture surface and splitting phenomenon was observed which is related with steel anisotropy. Fracture toughness obtained from experiment was compared with that calculate by two existing correlations. However both correlations did not predict the level of fracture toughness expected indicating the methods used in this work has limited applicability under the test conditions used here. Residual stress (RS) induced in API X100 steel by cold rolling method was characterised using two complementary techniques known as Neutron Diffraction (ND) and Incremental Hole Drilling (IHD). The RS distribution shows good agreement for both techniques used but reproducibility of them depends on their own inaccuracies. An Engineering Criticality Assessment (ECA) was performed based in Failure Assessment Diagram (FAD) approach using all the experimental data obtained by a leak-before-break method under three operational pressures. The results showed the effect on the integrity of material under the presence of a flaw length assessed. Overall, the thesis presents a combined engineering critical assessment which involved the examination of materials used to transport flue-gas and established a methodology to determine fracture toughness alongside with the FAD to assess the integrity of pipelines.

To fully exploit the strengths of La2Zr2O7 pyroclores and promote them as a next-generation thermal barrier coating (TBC), the improvements of their thermally insulating property and fracture toughness are studied in this thesis. A strong phonon scattering source, rattlers, is found in Y3+-doped La2Zr2O7 pyrochlores. Rattlers dramatically flatten k (thermal conductivity)-T curves, or even make k approach the amorphous limit. The presence of rattlers is strongly dependent on (1) oversized atomic cages that are formed in pyrochlores; and (2) the occupation of smaller guest ions in those oversized cages. To maximize the rattling effect, In3+/Sc3+ ions that are much smaller than Y3+ are introduced to the La2Zr2O7 lattice. As envisaged, the smaller ions in the oversized lattice voids make k glass-like at a much lower doping content. Nevertheless, they are still not effective in reducing the high temperature plateau kmin. Instead, oxygen vacancies are very effective in reducing kmin, because they generate an electrostatic repulsion force among cations surrounding them, resulting in stronger lattice anharmonicity and weaker bonds. The plateau kmin is reduced dramatically by the filling of the B-sites in La2Zr2O7 with a 21% larger (and 50% heavier) Ce4+ guest ion rather than a 96% heavier (but similar-sized) Hf4+ ion, suggesting that a large absolute size of substitutional atoms is more effective in reducing kmin than a heavy absolute mass. This is because: (1) kmin is proportional to (E/M)0.5 (where E is the elastic modulus and M is the average atomic mass); (2) a larger size of guest ions tends to produce a weaker ionic bond and consequently, a lower E; and (3) the changing extent of E by introducing larger guest ions is much greater than that of M induced by adding heavier ones. Lastly, the fracture toughness (KIc) has been increased by dispersing the tetragonal 3 mol% Y2O3-stabilized zirconia (t-3YSZ) particulates in the La2Zr2O7 (LZ) matrix. The tendency of the dispersive t-3YSZ second phases transforming to monoclinic (m) phases strongly depends on the volume fraction introduced. For samples made from equilibrium route, they are toughened by phase transformations within the dispersive t-3YSZ second phases and a crack shielding effect arising from the residual compressive stress within the LZ matrix. An anticipated increase of KIc from ferroelastic toughening together with the residual compressive stress toughening highlights a potential to improve coating durability by depositing t’-3YSZ/LZ composite TBCs by the non-equilibrium route.

Durante os anos desde 1910, diversos trabalhos científicos foram desenvolvidos, tornando o processo de têmpera bem estabelecido nas plantas industriais. Atualmente, existem diferentes tipos de têmpera e mais técnicas estão sendo desenvolvidas para aumentar as propriedades de componentes de aço. Um deles é o de têmpera intensiva, que pode ser considerado como um processo relativamente novo. O método de têmpera intensiva visa otimizar o processo produtivo, ao mesmo tempo em que diminui consideravelmente o custo da etapa de tratamento térmico. Além disso, atualmente o uso de soluções ambientalmente amigáveis torna este processo bem menos agressivo ao planeta. Neste trabalho realizou-se a têmpera intensiva e a têmpera convencional em corpos de prova preparados para teste de tenacidade à fratura. Trata-se, porém, de um método alternativo de teste, relativamente recente, no qual são considerados parâmetros de fratura dúctil e fratura frágil para o cálculo de K1C. Estes ensaios de tenacidade foram feitos a partir de ensaios de tração em corpos de prova com pré-trinca. Embora as tensões residuais compressivas tenham atingido os valores mais altos na têmpera intensiva, os resultados de tenacidade à fratura foram mais positivos para as amostras com têmpera convencional. A junção e aplicação desses métodos pode trazer um novo parâmetro de fabricação e análise de materiais metálicos, em especial aços-mola, que foi o objeto de estudo deste trabalho. / Since the beginning of 20th Century, several scientific works were developed and conventional quenching process became well established into the industrial area. Nowadays new quenching process were introduced increasing mechanical properties of the heat treated components. Intensive quenching is one of these process which optimize the heat treatment process using also quenchants considered nontoxic to the environment. In this work it was made comparative studies in the SAE 5160 samples which were submitted to conventional quenching and intensive quenching. Toughness fracture were evaluated using an alternative test where are analyzed ductile fracture and brittle fracture parameters to calculate KIC. In this method tensile test are performed in pre-cracked samples. Residual stresses were also measured and although intensive quenching promoted highest compressive stresses in the surface, KIC obtained in such samples presented low values compared with conventional quenching. The presented method of analysis will bring a new parameter for production and analysis for metallic materials, particularly spring steel, where compressive stress and toughness are important as properties for suspension components.

Raloxifene is an FDA-approved selective estrogen receptor modulator (SERM) that improves tissue quality by binding to collagen and increasing the bound water content in the bone matrix in a cell-independent manner. In this thesis, active tissue formation was induced by non-invasive external tibial loading in female mice and combined with raloxifene treatment to assess their combined effect on bone morphology and mechanical properties. Thermoregulation is an important factor that could have physiological consequences on research outcomes, and was introduced as an additional experimental factor in this study. We hypothesized that by removing the mild cold stress under which normal lab animals are housed, a metabolic boost would allow for further architectural and mechanical improvements as a result of the combination of tibial loading and raloxifene treatment. Ten week old female C57BL/6J mice were treated with raloxifene, underwent tibial loading to a strain level of 2050με and were housed in thermoneutral conditions (32°C) for 6 weeks. We investigated bone morphology through microcomputed tomography (μCT) and mechanical properties via four-point bending and fracture toughness testing. Results indicated a combined improvement by external loading and raloxifene on geometry, particularly in the cancellous region of the bone, and also in bone mechanics leading to greater improvements than either treatment individually. Temperature did not have a robust impact on either bone architecture or mechanical integrity.

Indiana University-Purdue University Indianapolis (IUPUI) / Raloxifene is an FDA-approved selective estrogen receptor modulator (SERM) that improves tissue quality by binding to collagen and increasing the bound water content in the bone matrix in a cell-independent manner. In this thesis, active tissue formation was induced by non-invasive external tibial loading in female mice and combined with raloxifene treatment to assess their combined effect on bone morphology and mechanical properties. Thermoregulation is an important factor that could have physiological consequences on research outcomes, and was introduced as an additional experimental factor in this study. We hypothesized that by removing the mild cold stress under which normal lab animals are housed, a metabolic boost would allow for further architectural and mechanical improvements as a result of the combination of tibial loading and raloxifene treatment. Ten week old female C57BL/6J mice were treated with raloxifene, underwent tibial loading to a strain level of 2050µε and were housed in thermoneutral conditions (32°C) for 6 weeks. We investigated bone morphology through microcomputed tomography (µCT) and mechanical properties via four-point bending and fracture toughness testing. Results indicated a combined improvement by external loading and raloxifene on geometry, particularly in the cancellous region of the bone, and also in bone mechanics leading to greater improvements than either treatment individually. Temperature did not have a robust impact on either bone architecture or mechanical integrity.

Dovetail joints are commonly seen in a furniture frame construction because of their unique configuration and strength. The tensile strength of dovetail joints was experimentally and analytically investigated using fracture mechanics method in this study. Experimental results of the investigation of effects of geometry factors on the tensile strength of dovetail joints in southern yellow pine and red oak indicated that the tensile strength of red oak joints was about 2 times higher than the one of southern yellow pine joints. Statistical analysis results indicated that the tail angle and tenon length of dovetail joints had significant influences on their tensile strength, and the tenon width was not a significant factor on the joint tensile strength. The fracture behaviors of southern yellow pine and red oak materials were investigated in the radial-longitudinal crack propagation system using a compact tension test method. Effects of wood specific gravity on fracture toughness for two wood species were studied in terms of their three growth ring combinations; earlywood, earlywood and latewood interface, and latewood. Regression analysis results indicated that the fracture toughness of two evaluated wood species can be predicted based on their specific gravity values. Statistical analyses indicated that the latewood yielded the significantly higher fracture toughness value, followed by earlywood and latewood interface, then earlywood for both wood species. Proposed prediction equations for tensile strengths of dovetail joints based on fracture toughness values of wooden materials used for frame construction were validated experimentally.

Despite being one of the most important organs of vertebrates, the material properties of skin are also one of the most poorly understood. In the field of designing medical devices and surgical tools there are significant advantages to having a model that describes the interaction of forces between a blade tip and skin during surgical cutting. In general, skin can best be described as a composite layer consisting of a viscoelastic dermis with interwoven collagen and elastin fibers beneath a superficial epidermis. The purpose of this research is to study the fracture toughness of porcine skin during practical cutting applications, the behavior of skin under quasistatic loads, and viscoelastic behavior of skin during stress relaxation. To fully describe the mechanics of skin in this model tensile test are conducted to determine the material properties of skin. The fracture toughness of the material is calculated by measuring the energy release rate of the material during required during cutting with Number 11 scalpel blade with a tip radius of 12 [micro]m . These results are then compared to a finite element analysis with a debonding interface and a Mooney-Rivlin hyperelastic material model with viscoelastic relaxation in an effort to predict the loads required by tools during surgical applications. The main outcome of this research is the development of a testing protocol and material model of skin that can be used in finite element simulations of uniaxial loads and surgical cutting.

<p> The effects of small additions of Fe2O3, GeO2, Ta2O5, V2O5, TiO2, and SiO2 on the microstructure and fracture toughness of magnesia enriched doloma were investigated. Effects of up to 5% additive oxides on grain growth and sintering in MgO and CaO were determined in preliminary tests. One percent additions were made to 40%, 60% and 80% MgO dolomas and the fracture toughness at temperatures up to 1500°C determined using the single edge notched beam specimen. Fracture surfaces were studied on the scanning electron microscope to determine fracture mode. Silica and Ta2O5 doped material showed high toughness at 1500°C possibly due to microcracks, while TiO2 resulted in formation of a viscous grain boundary film producing high toughness at 1300°C followed by a rapid decline by 1500°C. In undoped samples increases in MgO resulted in the appearance of a toughness peak near 1300°C. This was attributed to grain boundary segregation of impurities.</p> / Thesis / Master of Engineering (MEngr)

Effective treatment of carbon fiber components to improve delamination resistance is vital to the application of such materials since delamination is one of the biggest concerns regarding the use of composites in the aerospace sector. Due to the significant application benefit gained from increased stiffness to density ratio with composite materials, innovative developments resulting in improved through-thickness strength have been on the rise. The inherent anisotropy of composite materials results in an added difficulty in designing structural elements that make use of such materials. Proposed techniques to improve the through-thickness strength of laminar composites are many and varied; however all share the common goal of improving inter-laminar bond strength. This research makes use of novel materials in the field of wet flocking and Z-pinning. Cellulose nanofibers (CNFs) have already demonstrated excellent mechanical properties in terms of stiffness and strength, originating at the nano-scale. These materials were introduced into the laminate while in a sol-gel suspension in an effort to improve load transfer between laminate layers. The effect of CNFs as lightweight renewable reinforcement for CFRPs will be investigated. Carbon nanotube (CNT) additives were also considered for their beneficial structural properties. / Master of Science