Made available in DSpace on 2017-07-21T19:25:52Z (GMT). No. of bitstreams: 0 Previous issue date: 2016-03-10 / This work aimed at study the correlation of variables in a plasma immersion ion implantation (PIII) system, as well as their synergistic combination for the nitriding of the UNS S32750 super duplex stainless steel ( SD 2507). The research comprised two phases, as follows. (i) Study of the system. The interconnection of variables, namely voltage (V), pulse width (L), frequency (f) and current (I), were systematically analyzed with respect to the cathode heating. A mathematical formulation was proposed for the ion average energy and the substrate temperature, which took into consideration the energy conservation in the system, and the basic theories for plasma and sheaths and the ion interaction with matter. Hereafter, such model is thought to be experimentally demonstrated, allowing inferring the actual PIII fraction of energy that is converted to heat. (ii) N-PIII of the SD. Mirror-like samples were nitrided under different V, f and L combinations, leading to the temperatures 295, 325, 355 and 400 oC. The surface characterization methods were the optical, field emission electron, and atomic force microscopies, X-ray diffraction, energy dispersive X-ray spectroscopy, backscattered electron diffraction, and instrumented indentation. The austenite and ferrite fraction in the as received material amounted to 43,7 % and 56,3 %, respectively. After nitriding, the modified layers were 0,5-1,5 m thick. Up to 355 ºC, the expanded phase N was produced in originally austenite grains, whereas Fe2-3N e Fe4N precipitates were formed in ferrite grains. The hardness profiles were similar among different temperatures and between the two phases in the same sample. However, in ferritic regions, the mechanism for plastic deformation changed from ductile to brittle. In the 400 ºC treatments, only N was formed. Finally, a correlation for the production of the expanded phase in PIII and the mean pulse energy Ei was attained, given by and . Where IN and I are the integrated intensities of diffraction peaks for austenite and expanded austenite, respectively. / O objetivo deste trabalho foi estudar o comportamento de um sistema de implantação iônica por imersão em plasma (PIII: “plasma immersion ion implantation”), em função de suas variáveis, bem como a influência destas na nitretação de superfícies do aço super duplex UNS S32750 (ou SD 2507). O trabalho foi dividido em dois momentos, como segue. (i) Estudo do sistema. O comportamento das variáveis associadas à implantação iônica, especificamente tensão (V), largura de pulsos (L), frequência (f) e corrente (I), foi sistematicamente analisado com relação ao aquecimento do cátodo. Com base na conservação de energia, física de plasmas e bainhas catódicas e interação de íons com a matéria, propôs-se uma formulação matemática relacionado a energia média dos íons à temperatura do substrato, a qual poderá, futuramente, ser posta à prova experimental, mensurando-se a fração de energia que é, de fato, transformada em calor. (ii) Nitretação por PIII do SD. Amostras com superfície especular foram nitretadas sob diferentes combinações de V, f e L, em temperaturas de 295, 325, 355 e 400 oC. As superfícies foram caracterizadas por métodos de microscopia (ótica, eletrônica com efeito de campo, de força atômica), difração de raios X, espectroscopia de raios X por energia dispersiva, difração de elétrons retroespalhados, e indentação instrumentada. O SD apresenta estrutura cristalina de austenita e ferrita na proporção de 43,7/56,3. A nitretação produziu camadas modificadas com espessura de 0,5 a 1,5 m. Observou-se, nos tratamentos até 355 ºC, a formação da fase expandida N nos grãos que originalmente eram austenita, e de precipitados de nitretos -Fe2-3N e -Fe4N em grãos de ferrita. Embora não houve diferenças significativas nos perfis de dureza, tanto entre as temperaturas quanto entre as fases em uma mesma amostra, o mecanismo de deformação plástica nas regiões ferríticas transitou de dúctil para frágil. Nas nitretações em 400 ºC, houve apenas a formação de N. Finalmente, determinou-se que a obtenção da fase expandida por PIII no SD se relaciona com a energia média por pulso Ei por e . Onde I e I são as intensidades integradas dos picos de difração da austenita expandida e da austenita, respectivamente.

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.

Lors d’un recuit inter-critique d’un acier dit « Medium Manganèse », dont la teneur en Mn est située entre 4 et 12 %, avec une microstructure initiale complètement martensitique, la formation de l’austénite obéit à un mécanisme spécifique qui porte le nom d'ART - « Austenite Reverted Transformation » (transformation inverse de l’austénite). L’objectif de ce travail de thèse était d’étudier et de modéliser les évolutions microstructurales en lien avec les propriétés mécaniques lors d’un recuit ART. Il a été déterminé que la microstructure finale se compose de phases de nature (ferrite, austénite résiduelle et martensite de trempe) et morphologie (en forme d’aiguille et polygonale) différentes. Une attention particulière a été accordée aux cinétiques de dissolution des carbures et de formation de l’austénite. Une vision complète de ces processus a été construite. En outre, le mécanisme de stabilisation de l’austénite résiduelle à la température ambiante a été étudié et discuté. Enfin, des essais de traction ont été réalisés afin d’évaluer le comportement mécanique de l’acier après différents recuits ART et établir le lien avec la microstructure. Une analyse plus détaillée du comportement de chaque constituant de la microstructure a été effectuée. A l'issue de cette thèse, un modèle complet est disponible pour calculer les courbes de contrainte vraie - déformation vraie d’un acier Medium Mn / During the intercritical annealing of fully martensitic Medium Mn steel, containing from 4 to 12 wt.% Mn, the formation of austenite happens through the so-called “Austenite Reverted Transformation” (ART) mechanism. In this PhD work, the evolution of both microstructure and tensile properties was studied as a function of holding time in the intercritical domain. The microstructure evolution was studied using a double experimental and modeling approach. The final microstructure contained phases of different natures (ferrite (annealed martensite), retained austenite and fresh martensite) and of different morphologies (lath-like and polygonal). A particular attention was paid to the kinetics of austenite formation in connection with cementite dissolution and to the morphology of the phases. A mechanism was proposed to describe the formation of such microstructure. The critical factors controlling thermal austenite stability, including both chemical and size effects, were determined and discussed, based on the analysis of the retained austenite time-evolution. At last, tensile properties of the steel were measured as a function of holding time and the relation between microstructure and mechanical behavior was analyzed. Advanced analysis of the individual behavior of the three major constituents was performed. As a final output of this work, a complete model for predicting the true-stress versus true-strain curves of medium Mn steels was proposed

Shape memory alloys (SMAs) operating as solid-state actuators pose economic and environmental benefits to the aerospace industry due to their lightweight, compact design, which provides potential for reducing fuel emissions and overall operating cost in aeronautical equipment. Despite wide applicability, the implementation of SMA technology into aerospace-related actuator applications is hindered by harsh environmental conditions, which necessitate extremely high or low transformation temperatures. The versatility of the NiTi-based SMA system shows potential for meeting these demanding material constraints, since transformation temperatures in NiTi can be significantly raised or lowered with ternary alloying elements and/or Ni:Ti ratio adjustments. In this thesis, the expansive transformation capabilities of the NiTi-based SMA system are demonstrated with a low and high-temperature NiTi-based SMA; each encompassing different stages of the SMA development process. First, exploratory work on the NiTiSn SMA system is presented. The viability of NiTiSn alloys as low-temperature SMAs (LTSMAs) was investigated over the course of five alloy heats. The site preference of Sn in near-equiatomic NiTi was examined along with the effects of solution annealing, Ni:Ti ratio adjustments, and precipitation strengthening on the thermomechanical properties of NiTiSn LTSMAs. Second, the thermomechanical processability of NiTiHf high-temperature SMA (HTSMA) wires is presented. The evolution of various microstructural features (grain size reduction, oxide growth, and nano-precipitation) were observed at incremental stages of the hot rolling process and linked to the thermal and mechanical responses of respective HTSMA rods/wires. This work was carried out in an effort to optimize the rolling/drawing process for NiTiHf HTSMAs.

A solution-hardening of AISI 316L stainless-steel powder was conducted. The expansion of the crystal lattice and a strong increase in the nanoindentation hardness confirm the successful diffusion of carbon and nitrogen in the interstices. A multiphase state of the powder feedstock with phase fractions of the metastable S-phase (expanded austenite) mainly at the particle’s edge, and the initial austenitic phase within the core was found. Thermal spraying using high velocity oxy-fuel (HVOF) and atmospheric plasma spraying (APS) prove the sufficient thermal stability of the Sphase. Microstructural investigations of the HVOF coating reveal the ductility of the S-phase layer, while the higher heat load within the APS cause diffusion processes with the initial austenitic phase. The lattice expansion and the nanoindentation hardness decrease during thermal spraying. However, the absence of precipitates ensures the sufficient heat stability of the metastable S-phase. Even though further efforts are required for the thermochemical treatment of powder feedstock, the results confirm the feasibility of the novel powder treatment approach.

Les liaisons bimétalliques en acier inoxydable (LBM inox) permettent, au sein des réacteurs nucléaires français actuels, de connecter les gros composants en acier ferritique faiblement allié (cuve, pressuriseur, générateur de vapeur) à la tuyauterie du circuit primaire en acier austénitique inoxydable. De par leurs microstructure et propriétés mécaniques hétérogènes, ces liaisons sont des zones dites "sensibles" pour l'intégrité des structures et il est donc indispensable de caractériser leur tenue mécanique dans les situations de fonctionnement nominal et accidentelles. Ce travail de thèse a pour objectif d'évaluer le risque d'amorçage fragile de la LBM inox dans le haut de la transition fragile-ductile à l'aide d'un critère adapté. Les microstructures au voisinage de l'interface entre l'acier ferritique et le beurrage austénitique ont tout d’abord été caractérisées, et un liseré martensitique d’épaisseur variable ainsi qu’une couche entièrement austénitique ont été observés. Ces deux couches, qui sont le siège d’une intense précipitation de carbures pendant le traitement thermique de détensionnement, forment ensemble une couche dure de martensite et d’austénite carburées potentiellement fragile. Le comportement mécanique de l’ensemble de la LBM inox a ensuite été étudié à 20°C et à -175°C, et des lois de comportement élasto-plastiques isotropes ont été identifiées pour les différentes couches macroscopiques à partir d’essais de traction sur des éprouvettes multi-matériaux travers-joint à diamètre variable. Le comportement mécanique de la couche dure a, quant à lui, été caractérisé à partir d’essais in-situ sur des micro-éprouvettes usinées au FIB et testées à l’aide d’une micro-machine de traction développée dans cette thèse. Une étude des mécanismes de rupture de la LBM inox dans le domaine de la transition fragile-ductile a par ailleurs été réalisée à partir d’essais sur éprouvettes CT et a mis en évidence une fragilité de l’interface MA (entre martensite et austénite) liée à un mécanisme de rupture intergranulaire amorcée sur les carbures et systématiquement activé pour des fronts de préfissure traversant la couche dure. Une modélisation par éléments finis des essais a permis d’analyser les champs de contrainte sur l’interface MA et d’identifier un modèle de Weibull linéique à 3 paramètres basé sur une contrainte seuil et une distance seuil pour les éprouvettes CT. Finalement, l’effet du vieillissement thermique sur les LBM inox a été étudié à partir d’un traitement thermique de 10 000h à 400°C et un durcissement des couches austénitiques résultant d’un mécanisme de décomposition spinodale de la ferrite résiduelle a été mis en évidence à partir d’essais de traction. L’analyse des mécanismes de rupture à l’état vieilli a également montré que ce durcissement provoque une augmentation d’environ 30°C de la température de transition associée à la rupture intergranulaire de l’interface MA. / Stainless steel dissimilar metal welds (SS DMW) are widely used within the French nuclear power plants where they connect the main components (pressure vessel, pressurisor, steam generator) made of low-alloy ferritic steel to the primary circuit pipes made of austenitic stainless steel. Because of their heterogeneous microstructure and mechanical properties, these junctions are critical components for the structure integrity and their fracture resistance has to be demonstrated for all the nominal or accidental operating conditions. This PhD work aims at building a model to evaluate the risk of brittle fracture of the SS DMW in the upper shelf of the brittle-to-ductile transition range. The observation of the microstructures around the fusion line revealed a martensitic layer and a fully austenitic zone, which undergo an important carbides precipitation during the post-weld heat treatment and form a narrow hard layer of carburized martensite and austenite. The mechanical behavior of the SS DMW was then characterized at 20°C and -175°C and isotropic elastoplastic constitutive laws were determined for each macro/mesoscopic layer of the weld from tensile tests on crossweld specimens with variable diameters. The mechanical behavior of the narrow hard layer was also studied with micro tensile tests on specimens extracted by FIB micro processing and tested using an in-situ tensile testing device developed during the PhD. Furthermore, fracture toughness tests were carried out on CT specimens in the brittle-to-ductile temperature range and helped identify the MA interface (between martensite and austenite) as the weakest region in the SS DMW because of an intergranular fracture mechanism initiated at the carbides-rich interface. This mechanism was consistently observed for specimens with fatigue precrack fronts in the hard layer. The stress distributions on the MA interface calculated from the FE numerical simulation of these tests were then analysed and a 1D 3 parameters Weibull model based on a threshold stress and a threshold length was identified for the CT specimens. Finally, the effect of thermal ageing on the SS DMW was explored with a thermal ageing treatment of 10000h at 400°C and a hardening of the austenitic layers was measured by tensile tests and was associated to a spinodal decomposition mechanism of the residual ferrite. The fracture mechanisms of the SS DMW were also analysed in the aged state and showed that this hardening caused an increase of the transition temperature associated with the intergranular fracture of the MA interface by about 30°C.

In the work, it is studied almost carbon-free corrosion-resistant Fe-Cr-Ni-based steel, with the additional alloying with cobalt, molybdenum, aluminum and titanium, with high ductility and processability in production of high-strength wire. / В настоящей работе проводятся исследования новой практически безуглеродистой коррозионно-стойкой стали на Fe-Cr-Ni основе, с дополнительным легированием кобальтом, молибденом, алюминием и титаном, обладающей высокой пластичностью и технологичностью при производстве высокопрочной проволоки.

A balance between strength and ductility has been one of the most important considerations in the steel industry. Austenitic steel or multi-phase steel with retained austenite has plasticity-enhancing mechanisms, which can make it achieve high strength and good formability. Due to the occurrence of twinning-based mechanisms in high Mn steels, they have improved strength without sacrificing ductility. However, high Mn steels with extraordinary mechanical properties has not been used in mass production because of its high material cost together with welding problems and so on. As a consequence, many researchers have attempted to decrease the Mn concentration of high Mn twinning-induced plasticity steels without significant sacrifice of the mechanical properties. In the present work, a novel medium Mn steel with high C is designed with the aim of obtaining comparable mechanical properties as high Mn TWIP steel. In addition to Mn, C is also common effective austenite stabilizing element. C and Mn both increase the SFE of austenite. It should be possible to substitute at least some of the Mn in high Mn steels with C and still retain the TWIP effect. If the reduction in Mn content is not compensated for by the addition of other alloying elements, the microstructure will additionally contain some ferrite or martensite. The problem with C concentration is that it will result in the formation of carbide during the cooling process. As long as the carbide formation is suppressed, the formation of ferrite/martensite in medium Mn steels can be inhibited by an increase in the C concentration. In such cases, a soft and formable austenitic microstructure can be achieved by quenching from high austenitization temperatures to retain austenite with appropriate mechanical stability. The precipitation and dissolution of cementite in austenitic medium Mn high C steels capable of deformation-induced twinning were analyzed based on the associated length changes. Al addition was found to significantly retard the kinetics of cementite precipitation, indicating its usefulness in the design of cementite-free austenitic medium Mn steels with high C concentrations. Furthermore, Al addition changes the morphology of intragranular cementite from plate-shaped to equiaxed. The tensile properties of alloy were also examined in the present study. The present contribution discusses the mechanical properties of a bulk medium Mn high C steel with special alloying additions to oppose the precipitation of cementite. In particular, it aims to justify the mechanical properties based on crack nucleation and growth mechanisms. The reported mechanical properties enable a comparison with those of the well-known high Mn and Hadfield steels.

No description available.

Duplex stainless steels can be very attractive alternatives to austenitic grades due to their almost double strength at equal pitting corrosion resistance. When welding, the duplex alloys normally require addition of filler metal, while the commodity austenitic grades can often be welded autogenously. Over-alloyed consumables are used to counteract segregation of important alloying elements and to balance the two phases, ferrite and austenite, in the duplex weld metal. This work focuses on the weldability of the recently-developed lean duplex stainless steel LDX 2101® (EN 1.4162, UNS S32101). The pitting corrosion resistance of this grade is better than that of austenitic AISI 304 (EN 1.4307) and can reach the level of AISI 316L (EN 1.4404). The austenite formation is rapid in LDX 2101 compared to older duplex grades. Pitting resistance tests performed show that 1-2.5 mm thick laser and gas tungsten arc (GTA) welded LDX 2101 can have good corrosion properties even when welding autogenously. Additions of filler metal, nitrogen in the shielding gas, nitrogen-based backing gas and use of laser hybrid welding methods, however, increase the austenite formation. The pitting resistance may also be increased by suppressing formation of chromium nitrides in the weld metal and heat affected zone (HAZ). After thorough post-weld cleaning (pickling), pitting primarily occurred 1-3 mm from the fusion line, in the parent metal rather than in the HAZ. Neither the chromium nitride precipitates found in the HAZ, nor the element depletion along the fusion line that was revealed by electron probe microanalysis (EPMA) were found to locally decrease the pitting resistance. The preferential pitting location is suggested to be controlled by the residual weld oxide composition that varies over the surface. The composition and thickness of weld oxide formed on LDX 2101 and 2304 (EN 1.4362, UNS S32304) were determined using X-ray photoelectron spectroscopy (XPS). The heat tint on these lean duplex grades proved to contain significantly more manganese than what has been reported for standard austenitic stainless steels in the AISI 300 series. A new approach to heat tint formation is presented; whereby evaporation of material from the weld metal and subsequent deposition on the already-formed weld oxide are suggested to contribute to weld oxide formation. This is consistent with manganese loss from the weld metal, and nitrogen additions to the GTA shielding gas enhance the evaporation. The segregation of all elements apart from nitrogen is low in autogenously welded LDX 2101. This means that filler wire additions may not be required as for other duplex grades assuming that there is no large nitrogen loss that could cause excessive ferrite contents. As the nitrogen appears to be controlling the austenite formation, it becomes essential to avoid losing nitrogen during welding by choosing nitrogen-containing shielding and backing gas. / QC 20101213