Orientador: Paulo Roberto Mei / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-18T15:15:33Z (GMT). No. of bitstreams: 1 Bueno_JulianaCristina_M.pdf: 6612143 bytes, checksum: ff1f20ccef9c00e4455c0b43362c43ce (MD5) Previous issue date: 2005 / Resumo: Neste trabalho foi estudada uma liga inoxidável Fe-Mn-Si-Cr-Ni-Co com efeito de memória de forma (EMF) e os objetivos principais foram otimizar a técnica de coloração por ataque químico (color etching) para identificação e análise das fases presentes na microestrutura, o que permitiu a determinação da dureza da martensita-? e da austenita-? através da técnica de nanoindentação. O desenvolvimento deste processo também permitiu a quantificação das fases e e g por microscopia óptica. A técnica de coloração por ataque químico consiste na utilização de reagentes específicos que resultam em uma microestrutura composta por várias colorações, o que permite identificar fases por microscopia óptica. Os resultados de dureza obtidos por nanoindentação foram de 7,0 GPa para a martensita-? e de 3,0 GPa para a austenita-?. Já para a fração volumétrica da martensita-?, os resultados obtidos por microscopia óptica variaram de 33 a 40 % para amostras no estado deformado. Para amostras de tamanho de grão 123 ?m e 3º ciclo de treinamento, os resultados foram coerentes com os obtidos por difração de raios X de trabalhos anteriores para a mesma liga / Abstract: In this work a Fe-Mn-Si-Cr-Ni-Co stainless alloy with shape memory effect (SME) was studied and the main objectives were to optimize the technique of coloration by chemical attack (color etching) for identification and analysis of the phases in the microstructure, allowing the determination of the ?-martensite and the -austenite hardness by nanoindentation technique. The development of this process also allowed the quantification of the ?- and ?- phases by optical microscopy. The technique of coloration by chemical attack consists in the use of specific reagents to identify phases by color using optic microscopy. The hardness obtained was 7.0 GPa for ?-martensite and 3.0 GPa for ?-austenite. The volume fraction of the ?-martensite, measured with optical microscopy varied from 33 to 40 % for samples in the deformed state. For samples with grain size of 123 ?m and after the 3º training cycle, the results were coherent with the obtained by X ray diffraction of previous works for the same alloy / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica

abstract: Ultra High Performance (UHP) cementitious binders are a class of cement-based materials with high strength and ductility, designed for use in precast bridge connections, bridge superstructures, high load-bearing structural members like columns, and in structural repair and strengthening. This dissertation aims to elucidate the chemo-mechanical relationships in complex UHP binders to facilitate better microstructure-based design of these materials and develop machine learning (ML) models to predict their scale-relevant properties from microstructural information.To establish the connection between micromechanical properties and constitutive materials, nanoindentation and scanning electron microscopy experiments are performed on several cementitious pastes. Following Bayesian statistical clustering, mixed reaction products with scattered nanomechanical properties are observed, attributable to the low degree of reaction of the constituent particles, enhanced particle packing, and very low water-to-binder ratio of UHP binders. Relating the phase chemistry to the micromechanical properties, the chemical intensity ratios of Ca/Si and Al/Si are found to be important parameters influencing the incorporation of Al into the C-S-H gel. ML algorithms for classification of cementitious phases are found to require only the intensities of Ca, Si, and Al as inputs to generate accurate predictions for more homogeneous cement pastes. When applied to more complex UHP systems, the overlapping chemical intensities in the three dominant phases – Ultra High Stiffness (UHS), unreacted cementitious replacements, and clinker – led to ML models misidentifying these three phases. Similarly, a reduced amount of data available on the hard and stiff UHS phases prevents accurate ML regression predictions of the microstructural phase stiffness using only chemical information. The use of generic virtual two-phase microstructures coupled with finite element analysis is also adopted to train MLs to predict composite mechanical properties. This approach applied to three different representations of composite materials produces accurate predictions, thus providing an avenue for image-based microstructural characterization of multi-phase composites such UHP binders. This thesis provides insights into the microstructure of the complex, heterogeneous UHP binders and the utilization of big-data methods such as ML to predict their properties. These results are expected to provide means for rational, first-principles design of UHP mixtures. / Dissertation/Thesis / Doctoral Dissertation Engineering 2020

Determination of mechanical properties of very thin films is rather difficult task as all of currently using testing techniques have some weakness. This master’s thesis deals with microcompressive test and bulge test. Finite element simulations of the two methods were carried out in order to better understanding of experimental record. Microcompression combines the sample preparation with the use of focused ion beam (FIB) with a compression test carried out using nanoindenter. Cylindrical specimens (pillars) were prepared from Al film deposited on Si substrate using FIB. Experimentally measured data on pillars needs correction to obtain undistorted material properties of Al thin film. A necessary correction using FE modeling is suggested in the thesis. Second part of the work is focused on modeling of bulge test. Pressure is applied on freestanding SiNx film while deflection of the film is measured. Stress state in the film is biaxial making determination of mechanical properties of the film more complicated. The goal is to present how to model the whole problem. In addition, preparation of the specimens was simulated to estimate residual stress in the film. The paper contributes to a better characterization of very thin surface layers and determination of their mechanical properties.

In this study, the time-dependent deformation behavior of several model bulk metallic glasses (BMGs) was studied. The BMGs were obtained in different structural states by thermal relaxation below their glass transition temperature, cryogenic thermal cycling, and chemical rejuvenation by micro-alloying. The creep behavior of Zr52.5Ti5Cu17.9Ni14.6Al10 BMG in different structural states was investigated as a function of peak load and temperature. The creep strain rate sensitivity (SRS) indicated a transition from shear transformation zone (STZ) mediated deformation at room temperature to diffusion dominated mechanisms at high temperatures. The relaxation enthalpy of Zr47Cu46Al7 BMG was found to increase significantly with the addition of 1 at% Ti, namely for Zr47Cu45Al7Ti1. Comparison of their respective free volumes indicated that chemical rejuvenation had a more pronounced effect compared to cryogenic thermal rejuvenation. Micro-pillar compression tests supported the improved plasticity with increase in free volume from the rejuvenation effect. Effect of chemistry change on mechanical response and time-dependent deformation was investigated for topologically equivalent Pt-Pd BMGs, where the Pt atoms were systematically replaced with Pd atoms (Pt42.5-xPdx)Cu27Ni9.5P21: x=0, 7.5, 20, 22.5, 35, 42.5). The hardness and reduced modulus increased while the degree of plasticity decreased with increase in Pd-content, which was attributed to the increase in stiffer 3-atom cluster connections. STZ volume was calculated for all the BMGs using cooperative shear model (CSM) for fundamental understanding of the underlying deformation mechanisms.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第19893号 / 工博第4209号 / 新制||工||1651(附属図書館) / 32970 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 白井 泰治, 教授 松原 英一郎 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

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<p>  </p> <p>Aluminum (Al) possesses a plenitude of remarkable properties, such as strong corrosion resistance, high thermal and electrical conductivity, and high specific strength. However, Al and its alloys are still remarkably weaker than most high strength steels and susceptible to drastic softening at high temperatures, preventing many applications where its low density would be beneficial. Severe plastic deformation can yield ultra-fine grained Al alloys with similar strengths as steels, although they are highly unstable even at room temperature. Nanotwinned (NT) metals have demonstrated concomitant strength and ductility, enabled by twin boundaries which simultaneously act to inhibit dislocation motion and generate partial dislocations that aid in plasticity. In spite of having a high stacking fault energy, nanotwins have been introduced into Al alloys using transition metal solutes during magnetron sputtering. This thesis aims to explore the impact Zr has on the microstructure, deformation, and thermal stability of nanotwins in NT Al.</p> <p>Our studies identify how Zirconium (Zr) aids in the formation of a significant volume fraction of 9R phase and an abundance of finely spaced incoherent twin boundaries, leading to a maximum hardness of 4.2GPa. They further uncover through <em>in-situ</em> micropillar compression that NT Al-Zr alloys are highly deformable and reach a flow stress of ~1.1GPa. Constant strain rate nanoindentation tests demonstrate the enhanced strain rate sensitivity in NT Al-Zr alloys. Zr is also identified to be a remarkable thermal stabilizer when incorporated into NT Al-Co alloys, with no apparent softening up to 450 °C (0.78 T­m). The influence of substrate texture on nanotwinned Al-Zr alloys microstructure was also thoroughly explored.</p>

Metal-organic frameworks (MOFs) are an emerging class of materials exhibiting desirable properties and functionalities for a variety of applications, including catalysis, molecular separation, gas storage, and mechanical reinforcement. However, the majority of MOFs exist as particulate powders, limiting their transportability and applicability in practical fields. Polymers, on the other hand, are one of the most widely used materials in the world owing to their facile processability and low production cost. Combining MOFs and polymers to form MOF-polymer composites can potentially maintain the merits of both materials while overcoming drawbacks of each individual component. Specifically, MOFs are promising candidates as mechanical reinforcers for polymers because of their low density, high specific modulus, and controllable dimensions. Herein, we aim to provide a comprehensive investigation into the chemistry and mechanical properties of MOF-polymer composites. Various governing parameters, including particle aspect ratio (AR), MOF-particle interface, and intrinsic mechanical properties of MOFs, were thoroughly studied to construct an optimal pathway for fabricating mechanically reinforced MOF-polymer composites. Chapter 1 presents an introduction to MOFs, polymer composites, and mechanical properties and characterizations of polymeric materials. It serves as a foundation of this dissertation and outlines essential concepts for the scientific background. The primary factors that impact the mechanical properties of polymer composite are highlighted, leading to the following three research chapters. Comprehensive background on various characterization techniques that aim at mechanical properties is covered in detail. Chapter 2 focuses on the role of MOF AR on the mechanical properties of MOF-polymer composites. PCN-222, a Zr-MOF with porphyrin linkers, was synthesized with AR ranging from 3.4 to 54. The crystallinity and chemical structure of the MOFs remained consistent for different ARs, ensuring that the AR was the only variable in determining the mechanical reinforcement. Fabricated through the doctor-blade technique, the MOF-PMMA composite films showed homogeneous MOF distribution and alignment. Tensile tests revealed that Young's modulus of the composites increased with MOF AR, exhibiting a good agreement with a modified Halpin-Tsai model. Both storage and loss moduli were also enhanced following increased MOF AR. In addition, the thermal stability was also improved with the addition of MOF particles. In Chapter 3, the authors extend the understanding of mechanical properties of MOF-polymer composites to the interfacial properties between the two materials. Pristine MOFs often lack strong interactions with a polymer matrix due to the difference in chemical/physical properties. The authors developed a three-step synthetic route to grow PMMA on the surface of PCN-222. Owing to an efficient surface-initiated polymerization technique, the PMMA was successfully grafted with high molecular weight and grafting density. The molecular weight of PMMA could be controlled by simply varying polymerization time. The PMMA-grafted PCN-222 was manufactured along with PMMA matrix to form composite films. Mechanical analysis proved that the mechanical reinforcement was improved with increasing grafted molecular weight. Chapter 4 presents an experimental approach to unveil the structure-mechanical property of MOF single crystals, which provides insights on designing MOFs with desired mechanical strength. Zeolitic imidazolate frameworks (ZIFs), a subdivision of MOFs, were chosen as the template owing to their facile synthesis, structural diversity, and high crystallinity. Two types of micron-sized ZIFs, ZIF-8 with Zn2+ node and ZIF-67 with Co2+ node, were synthesized to compare the effect of metal-linker bond. Moreover, the linker composition was varied to examine the difference in crystal structure and defect level. The mechanical properties of these ZIF samples were revealed by nanoindentation on single particles. Overall, the stronger metal-linker bond and high crystallinity were able to yield the highest elastic modulus and hardness. Finally, Chapter 5 offers a comprehensive review on polymer-grafted MOF particles regarding the synthesis and applications associated with surface-anchored polymers. Various polymerization techniques were summarized, and their adjustment and limitations with respect to MOFs were highlighted. The novel and unique applications arisen from polymer-grafted MOFs and Mixed Matrix Membranes were thoroughly discussed. / Doctor of Philosophy / Polymer composites, a combination of polymer matrix and particle fillers, have shown great applicability in nearly every aspect of our daily lives. For example, rubber tires, composed of synthetic polymeric rubber and inorganic particle fillers (e.g., carbon black and glass fiber), have been a great booster for modern society owing to their durability and mechanical strength. Aircraft are also made of roughly 50% composite materials, because of their lightweight and high mechanical strength. Herein, we present a novel type of polymer composite using metal-organic frameworks (MOFs) as mechanical reinforcers. Thanks to the low density, high modulus, and tunable geometry, MOFs can be ideal candidates for mechanically reinforced polymer composites. In this dissertation, several fundamental parameters that impact the mechanical properties of MOF-polymer composites are discussed. The intent of this work is to provide mechanistic insights on the development of outstanding lightweight composites with efficient mechanical reinforcement.

<p>  </p> <p>Molecular crystals are used in a wide variety of applications, from pharmaceuticals and sweeteners to energetic materials. Understanding their chemical and mechanical properties provides insight into their performance and use. These properties are especially critical for energetic material systems, which may be sensitive to impact and require specific handling and storage practices. The mechanical properties of energetic molecular crystals are typically determined using nanoindentation by measuring elastic modulus, hardness, yield point, and fracture behavior. Reports of the properties and mechanical behavior of as-grown molecular crystals are limited due to the relative difficulty of performing good quality measurements. This work’s contributions include the first known measurements of elastic and plastic properties for crystals of DAAF, CL-20, NTO, ETN, and R-salt.</p> <p>When studying molecular crystalline systems, some important assumptions and behaviors typical to metallic and ionic systems begin to break down. The energetic material diaminoazoxyfurazan (DAAF) exhibits highly irregular mechanical behavior, which is likely explained by a complex combination of chemical and material attributes. This work investigates and compares the irregular mechanical response in DAAF—including high variance in mechanical properties, broad range of load-depth behavior, and non-conforming indentation impression geometries—to other energetic molecular crystals. The yield points (i.e., onset of plasticity) for several energetic materials, whose elastic modulus values range from 9.6 to 25.5 GPa, are also compared to identify the parameters that govern the onset of plasticity. This includes an investigation into yield point dependence on (or independence from) elastic modulus, hardness, near-neighbor spacing, and activation volume. When these materials reach the onset of plasticity, the maximum shear stress in each material ranges from 2-7% of their elastic modulus value. Analysis of the yield behavior in these materials suggests that there is not a strong correlation between yield stress and hardness, thus establishing that the mechanisms governing dislocation nucleation are not controlled by hardness, and vice-versa. By recognizing and accounting for the added complexities associated with inherently non-spherical molecules in a crystal lattice, this work advances the comprehension of mechanical response in molecular crystal systems.</p>

<p>An investigation of the influence of three alloying elements Chromium, Phosphorus, and Nitrogen with the solute types of oversized substitutional, undersized substitutional, and interstitial on the irradiation induced microstructural evolution and hardening</p>