Martensitic steels have become very important engineering materials in modern society. Crucial parts of everyday products are made of martensitic steels, from surgical needles and razor blades to car components and large-scale excavators. Martensite, which results from a rapid diffusionless phase transformation, has a complex nature that is challenging to characterize and to classify. Moreover the possibilities for modeling of this phase transformation have been limited, since its thermodynamics and kinetics are only reasonably well understood. However, the recent development of characterization capabilities and computational techniques, such as CALPHAD, and its applicability to ferrous martensite has not been fully explored yet. In the present work, a thermodynamic method for predicting the martensite start temperature (Ms) of commercial steels is developed. It is based mainly on information on Ms from binary Fe-X systems obtained from experiments using very rapid cooling, and Ms values for lath and plate martensite are treated separately. Comparison with the experimental Ms of several sets of commercial steels indicates that the predictive ability is comparable to models based on experimental information of Ms from commercial steels. A major part of the present work is dedicated to the effect of carbon content on the morphological transition from lath- to plate martensite in steels. A range of metallographic techniques were employed: (1) Optical microscopy to study the apparent morphology; (2) Transmission electron microscopy to study high-carbon plate martensite; (3) Electron backscattered diffraction to study the variant pairing tendency of martensite. The results indicate that a good understanding of the martensitic microstructure can be achieved by combining qualitative metallography with quantitative analysis, such as variant pairing analysis. This type of characterization methodology could easily be extended to any alloying system and may thus facilitate martensite characterization in general. Finally, a minor part addresses inverse bainite, which may form in high-carbon alloys. Its coupling to regular bainite is discussed on the basis of symmetry in the Fe-C phase diagram. / <p>QC 20120824</p> / Hero-m

High carbon bainitic steel plates could surpass quench and tempered martensitic counterparts for fabrication of ammunition- and blast-resistant armours. Mechanical properties, microstructure and reaction kinetics of a commercially available carbide-free nanoscale bainite alloy were characterized. Based on the initial characterization and a comprehensive review of the literature a new alloy with lower carbon, higher silicon and cobalt additions was designed and processed into hot-rolled plates (10x10mm and 300x300mm) using CanmetMATERIALS pilot-scale facilities. The heat treated plates achieved strength above 2 GPa with elongation of 14%. Thorough analysis with electron backscattered diffraction revealed that the microstructure consisted of bainitic ferrite laths, islands of retained austenite, areas of mixed martensite-austenite (MA). Transmission electron microscopy confirmed the fine scale of bainitic ferrite and the presence of thin films of retained austenite encompassing bainite laths. Dilatometric study of the new alloy revealed that forming bainite at higher transformation temperatures, 275°C versus 250°C and 225°C, led to faster overall reaction kinetics and higher final fractions of bainite within 18 hours of isothermal holding. Although it is expected that the fraction of bainite increases at lower temperatures, substantial prolonged holding time is required for completion of the reaction. Microstructural features and particularly bainite lath thickness depended on bainite formation temperature. Ausforming, deformation of austenite at 600°C for 25-45% strain prior to decomposition to bainite, however led to a decrease in reaction rate and final fraction of bainite. Tensile testing of austempered specimens showed that higher transformation temperature yielded a stronger microstructure, which was attributed to the formation of thinner bainitic ferrite laths. Higher transformation temperatures led to an increase in ductility. Tensile testing of the ausformed specimens showed a reduction in both strength and ductility. A negative correlation was seen between the amount of MA areas in the microstructure and total elongation. / Thesis / Master of Science in Materials Science and Engineering (MSMSE) / This project has adopted the science of bainite transformation to develop a suitable alloy and processing method for the fabrication of very strong armour plates at a lower cost compared to commercially available grades. The pilot-scale casting and processing facility at CanmetMATERIALS centre was used to produce full sized, 1ft (304.8mm) by 1ft (304.5mm), prototype armour plates. The plates were subsequently characterized using a variety of techniques to determine interplay between processing parameters, microstructure and the ensuing final performance. The optimized alloy, tailored processing parameters, and characterization information constitute the contribution of the present work to the current state of research.

Oriented needle-shaped or rod-shaped quartz precipitates occur in clinopyroxenes have been commonly observed in eclogites or garnet peridotites from the high pressure or ultra-high pressure (HP/UHP) metamorphic belts, and their occurrence has been used as an indicator of UHP metamorphism. However, the origin of those quartz precipitates and their crystallographic orientation relationships with clinopyroxene hosts are still not clear. In order to understand the formation mechanisms and environments of the quartz precipitates, the present study has used electron backscattered diffraction (EBSD) analysis, petrographic and scanning electron microscopy, and electron microprobe analysis to study textural features, mineral assemblages, mineral compositions, and crystallographic orientation relationships of mineral precipitates in the omphacite from Xitieshan, North Qaidam UHP metamorphic belt. The results show that the oriented rod-like precipitates in the omphacite hosts are mainly composed of quartz + edenite, and the rods are 5~20

abstract: This report will review the mechanical and microstructural properties of the refractory element rhenium (Re) deposited using Laser Additive Manufacturing (LAM). With useable structural strength over 2200 °C, existing applications up to 2760 °C, very high strength, ductility and chemical resistance, interest in Re is understandable. This study includes data about tensile properties including tensile data up to 1925 °C, fracture modes, fatigue and microstructure including deformation systems and potential applications of that information. The bulk mechanical test data will be correlated with nanoindentation and crystallographic examination. LAM properties are compared to the existing properties found in the literature for other manufacturing processes. The literature indicates that Re has three significant slip systems but also twins as part of its deformation mechanisms. While it follows the hcp metal characteristics for deformation, it has interesting and valuable extremes such as high work hardening, potentially high strength, excellent wear resistance and superior elevated temperature strength. These characteristics are discussed in detail. / Dissertation/Thesis / Ph.D. Materials Science and Engineering 2012

Knowledge of the full 5-degree Grain Boundary Character Distribution (GBCD) is vital to understanding properties, such as gas diffusivity, that are dominated by grain boundary character. Surface characterization techniques, such as Electron Backscattered diffraction (EBSD), can provide only 4 of the 5 GB characteristics (the rotation between the neighboring grains, and the trace of the GB on the surface). The inclination of the GB in the direction normal to the surface is not known. A previous study indicated that the GB inclination could be recovered by correlating the Electron Backscattered patterns (EBSPs) of sample points near the GB with EBSPs taken from the centers of the neighboring grains. The resultant transition curve could be compared with theoretical curves obtained from MonteCarlo simulations of electron yield from the two grains. However, a practical method based upon this study was never implemented. Here, a few microscopy and image filters have been applied to the EBSPs to improve the image quality. Also, several experiments have been conducted to verify and validate the interaction volume of the materials used to produce theoretical transition curves, in order to receive more accurate results. In this work, it is hypothesized that transition curves obtained from considering individual band intensities from the EBSPs will give more informative transition curves. The filtered EBSPs from the band intensities coupled with the accurate interaction volume values, should give us more reliable and repeatable transition curves, and that a more detailed comparison of the experimental and simulated transition curves will give higher fidelity results, in terms of GB inclination determination.

This study focuses on the laser powder bed fusion processing of NiTi alloys and the feasibility of fabricating very thin stent structures for biomedical applications. A comprehensive correlation between the process and the material’s-structure and properties is established to facilitate the fabrication of NiTi alloys with tailored properties. In the first step, the impact of LPBF processing parameters and post-treatments on evolving the microstructure, texture, superelasticity, and asymmetry is examined. Subsequently, the feasibility of manufacturing very thin mesh structured stents is scrutinized followed by in-depth investigations into differently designed stents considering properties such as surface characteristics, mechanical properties, superelasticity, and recoverability. The obtained results and the represented discussions offer imperative insights, helping to better understand the complexity of the LPBF process and the present challenging aspects. Moreover, detailed contributions are made with the goal of paving the road ahead for the production of patient-specific NiTi stents with enhanced properties. / Thesis / Doctor of Philosophy (PhD)

European iron production is to a large extent dependant on massive Kiruna type apatite-iron ore deposits. In this contribution, high-temperature magnetite samples from apatite-iron-oxide deposits are investigated by means of Electron Backscattered Diffraction. However, the origin of Kiruna-type deposits is still unresolved. Although magmatic processes are likely, it is not clear how small-scale processes can form giant Kiruna-type deposits. The sample suite consists of magnetite samples from six global apatite-iron-oxide deposits: the famous Kiirunavaara deposit and the Malmberget deposit, both located in northern Sweden, the Grängesberg deposit in south-central Sweden, the iconic El Laco deposit in north-eastern Chile, the Bafq deposit in central Iran, and the Varena deposit in south Lithuania. Fe-O systematics has been conducted to complement existing δ18O and δ56Fe isotope data and ensure magmatic origin of the samples from the Malmberget deposit (n=6) and the Varena deposit (n=2). This is the first effort to characterise magnetite samples from apatite-iron-oxide deposits utilising EBSD. In total, twelve EBSD maps have been produced. Evaluation of the EBSD data have been performed to quantify the preferred orientation of the magnetite crystals. Four deposits, with Kiirunvaara being the prime example, shows no preferred alignment of the magnetite crystals. Whereas the El Laco samples exhibits a strong preferred alignment of {111}. The EBSD data from magnetite samples in equilibrium with a magmatic source indicate that apatite-iron-oxide deposits are formed in both intrusive and extrusive environment and that magmatic crystal accumulation is a key process in aggregating magnetite to form large and even giant Kiruna-type deposits. / Europeisk järnmalmsproduktion är i stor utsträckning beroende av massiva apatit-järnmalmsfyndigheter av Kiruna-typ. I det här arbetet, undersöks magnetitprover av hög-temperaturs ursprung från olika apatit-järnmalmsfyndigheter med Elektron Bakåtspridande Diffraktion. Bildningsmekanismen av apatit-järnmalmsfyndigheter av Kiruna-typ är än idag oklar. Bevisen indikerar magmatiska bildningsprocesser, det är dock fortfarande oklart hur småskaliga magmatiska processer bildar gigantiska apatit-järnmalmsfyndigheter av Kiruna-typ. Provserien består av magnetitprover från sex globala apatit-järnmalmsfyndigheter: den världsberömda Kiirunavaara fyndigheten och Malmberget fyndigheten, båda lokaliserade i Norrbotten, Sverige, Grängesberg fyndigheten i Bergslagen, Sverige, den ikoniska El Laco fyndigheten i nordöstra Chile, Bafq fyndigheten i centrala Iran, och Varena fyndigheten i södra Litauen. För att fastställa ett magmatiskt ursprung och komplettera befintlig δ18O och δ56Fe isotopdata har Fe-O-systematik utförts på magnetitproverna från Malmberget (n=6) och Varena (n=2). Det här är den första dokumenterade EBSD-undersökningen av magnetitprover från apatit-järnmalmsfyndigheter. Totalt tolv EBSD-kartor har producerats. Utvärdering av EBSD-data har utförts för att kvantifiera den föredragna riktningen på magnetitkristallerna. I fyra fyndigheter, med Kiirunvaara som typexempel, uppvisar magnetitkristallerna ingen föredragen riktning, medan magnetitproverna från El Laco uppvisar en tydlig föredragen riktning längs {111}. EBSD-data från magnetitprover i jämnvikt med en magmatiskkälla påvisar att apatit-järnmalmer bildas i både intrusiva miljöer och extrusiva miljöer och att magmatisk ackumulation är en nyckelprocess för att aggregera magnetitkristaller och bilda stora till gigantiska apatit-järnmalmsfyndigheter av Kiruna-typ.

Les fils composites Cu/Nb étudiés ici sont d'excellents candidats pour les bobines non destructives générant des champs magnétiques pulsés intenses (B ≥ 100T). Ils sont fabriqués par Accumulative Drawing and Bundling (ADB) et sont constitué de renforts continus de Nb dans une matrice multi-échelles de Cu. Ces travaux rentrent dans le cadre du projet METAFORES (ANR-12-BS09-0002), visant l’évaluation des effets de taille et d’architecture sur les propriétés des conducteurs Cu/Nb. L’objectif principal consiste donc à caractériser leur microstructure et leurs propriétés à chaque étape de la fabrication par différentes techniques de caractérisation. Des essais mécaniques et électriques montrent une augmentation de la limite d’élasticité avec l’affinement de la microstructure tout en conservant une conductivité électrique adéquate. Les études de la texture globale par DRX ont mis en évidence trois composantes de texture de fibre dont deux pour la matrice de Cu (<111> et <100>) et une composante unique <110> pour le Nb. On retrouve ces trois composantes de texture dans les analyses locales (EBSD), cependant les proportions relatives des composantes du Cu varient en fonction du nombre de cycles ADB.Les essais de déformation in-situ sous neutrons ont mis en évidence des comportements élasto-plastique et purement élastique des familles de grains {111} du Cu et {110} du Nb respectivement, quels que soient les échantillons. Pour la famille {200} du Cu, le comportement mécanique varie en fonction du nombre de cycles ADB. Tous ces résultats viendront nourrir les simulations effectuées dans le cadre du projet METAFORES (Thèse de Tang Gu, ENSAM-Paris/Mines ParisTech). / High strength and high conductivity Cu/Nb composites studied here are very good candidates for the design of magnets generating high pulsed magnetic fields (B ≥ 100T). They are fabricated by Accumulative Drawing and Bundling (ADB) and are constituted with a multi-scale Cu matrix embedding continuous Nb filaments that are distributed in a controlled manner. This study is performed within the framework of the METAFORES project (ANR-12-BS09-0002) aiming at assessing size and architecture effects on properties of these Cu/Nb conductors. The main purpose is therefore to characterize the microstructure and properties of these conductors at different stages of the fabrication process. Mechanical and electrical results show an increase in yield strength while maintaining adequate electrical conductivity. Global texture studies confirm three fiber texture components: two for the Cu matrix (<111> and <100>) and a single component <110 > for Nb. These three texture components are also observed at the local scale analysis (EBSD); however the volume fractions of the Cu components locally depend on the number of ADB cycles.In-situ deformation tests under neutrons reveal elasticplastic and purely elastic behaviors of the {111} Cu and {110} Nb grains family respectively, whatever the samples. However, for the {200} Cu grains family, mechanical behavior strongly depends on the number of ADB cycles. These results will feed the simulations conducted in the METAFORES project (Thesis of Tang Gu, ENSAM-Paris / Mines ParisTech).

O desenvolvimento dos veículos atuais vem sendo impulsionado pela necessidade de redução de massa associada com o aumento da segurança para os passageiros. Na procura de novos materiais e processos para atender estas exigências, os aços bifásicos ferrítico-martensíticos ou DP vêm se destacando entre os aços avançados de alta resistência (AHSS), por apresentar elevada resistência mecânica e boa ductilidade. Da mesma forma, a soldagem a laser vem se mostrando promissora para junção desta classe de materiais. Este processo permite unir os aços DP com boa qualidade metalúrgica sem significativas distorções dimensionais. Embora os aços DP apresentem boa soldabilidade, um amolecimento localizado na zona afetada pelo calor (ZAC) também é observado, especialmente no aço DP1000, que apresenta elevada fração de martensita. Desta forma, esta Tese propõe a soldagem a laser do aço DP1000 de espessura 1,80 mm, seguida de uma sistemática caracterização microestrutural, visando a produção de juntas soldadas suficientemente resistentes. Para isto, foram produzidos cordões numa chapa de aço DP1000, variando a potência nominal de soldagem entre 0,4 e 2,0 kW e a velocidade de soldagem entre 20 e 150 mm/s. A caracterização microestrutural foi conduzida com o auxílio das técnicas de microscopia óptica (MO), microscopia eletrônica de varredura (MEV), difração de raios X (DRX) e difração de elétrons retroespalhados (EBSD). As juntas soldadas mais representativas foram submetidas a ensaios de dureza Vickers e tração uniaxial. Os resultados mostram que é possível produzir juntas soldadas resistentes no aço DP1000. Todavia, é fundamental que a combinação de parâmetros gere soldas com penetração total e mínima largura de ZAC, limitando a quantidade de amolecimento da martensita prévia e a fração volumétrica de austenita retida. Na presente Tese, os melhores resultados foram obtidos para uma potência de 2,0 kW e velocidade de 150 mm/s. / The development of modern vehicles has been driven by the need of mass reduction associated with the increase of the safety of passengers. In the search for new materials and processes to meet these requirements, ferritic-martensitic dual-phase (DP) steels are potential candidates among advanced high-strength steels (AHSS), because of their high mechanical strength and good ductility. In that sense, laser beam welding has been shown promising for joining this class of materials. This process allows joining DP steels with good metallurgical quality without large dimensional distortions. Although DP steels show good weldability, a localized softening in the heat affected zone (HAZ) is also observed, especially in DP1000 steel which contains large amounts of martensite. Thus, laser beam welding has been performed in DP1000 steel with thickness of 1.80 mm, followed by a systematic microstructural characterization, aiming at the production of resistant welded joints. For this, bead-on-plate welds were carried out in DP1000 steel, varying the welding power between 0.4 and 2.0 kW and the welding speed between 20 and 150 mm/s. The microstructural characterization was conducted with the aid of light optical microscopy (LOM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and electron backscattered diffraction (EBSD). The most representative welded joints were tested for Vickers hardness and uniaxial tensile test. Results show that it is possible to produce sound and resistant welded joints in DP1000 steel. However, it is critical that the combination of parameters allows the obtainment of welds with full penetration and minimum HAZ width, limiting the amount of softening of prior martensite and the volume fraction of retained austenite. In the present Thesis, this was achieved using a power of 2.0 kW and a welding speed of 150 mm/s.

Technological advances results in the fact that quite a large number of electronic equipment interacts with its environment leading to the malfunction of the devices. This brings about the necessity of using proper electromagnetic (EM) wave absorbers/shields to avoid such interactions. In order to absorb EM waves in a large frequency band from several MHz to GHz, barium hexaferrite (BaHF) ceramics which are produced as textured ceramics as well as in multilayered form can be used. Textured ceramics are processed by tape casting using templated grain growth (TGG) phenomenon. In order to obtain textured ceramics, BaHF powders and platelets are required as raw materials in such a way that during sintering small size powders are directioned by large platelet surfaces. In this study, ferrite powders were synthesized by mixed oxide technique while the platelets were produced by both molten salt synthesis (MSS) and reactive templated grain growth (RTGG) methods. In the case of platelet synthesis by MSS, effects of calcination temperature and time as well as type and composition of the flux on the formation and morphology of platelets were investigated based on the XRD and SEM results. Studies have shown that KCl flux led to the formation of sharper platelet morphology, while NaCl resulted in more round shapes. However, extent of BaHF formation in the case of NaCl was higher when compared to KCl flux due to its higher wettability characteristic, and hence faster interaction with the raw materials. Since the aspect ratio of the synthesized platelets was only ca. 2-4, these platelets were not efficient for further TGG studies. Alternatively, BiFeO3 (BiF) particles having ~30-40 &mu / m average size were synthesized as seed crystals for the synthesis of BaHF platelets by RTGG method. After the washing of these platelets with dilute HNO3, pure BaHF powders and platelets were directed by tape casting which was followed by sintering using TGG phenomenon. Degree of achieved texturing in the processed ceramics was studied using Rietveld analysis, pole figure measurement and electron backscattered diffraction (EBSD).