Die verformungsinduzierten Phasenumwandlungen und die Zwillingsbildung wurden in drei metastabilen austenitischen Cr-Mn-Ni-Stählen mit unterschiedlichem Nickelgehalt im breiten Temperaturbereich untersucht. Die entwickelten STU- und DTU-Diagramme fassen die gewonnenen Erkenntnisse zusammen und charakterisieren die verformungsinduzierten Gefügeänderungsprozesse in Abhängigkeit von der Spannung und der Temperatur. Die thermodynamischen Berechnungen bestätigen die Unterschiede in der chemischen Triebkraft für die Martensitumwandlung zwischen den Stählen und erklären unterschiedliches Werkstoffverhalten. Ein thermodynamisch-mechanisches Modell der verformungsinduzierten α‘-Martensitbildung wurde entwickelt. Der maximale α‘-Martensitanteil wird als Funktion der Gesamttriebkraft und der Temperatur mit einer guten Genauigkeit beschrieben. Des Weiteren wurde ein Modell der Umwandlungsplastizität mit Berücksichtigung der Plastizitätsverringerung infolge der isothermen oder spannungsinduzierten Martensitbildung entwickelt. Außerdem wurde der Einfluss von Mikroseigerungen auf die verformungsinduzierte Martensitbildung anhand drei Modellstähle untersucht und bestätigt.

A crescente demanda de aplicações de aços inoxidáveis austeníticos e a constante pressão para redução de custo nas empresas siderúrgicas, devido à alta volatilidade no custo do níquel, resultaram em novos desenvolvimentos de aços da série 200. Esta nova classe de aços inoxidáveis austeníticos contém elevados teores de manganês e nitrogênio em substituição ao elemento níquel. A justificativa para a realização deste trabalho é a escassez de estudos comparativos entre aços inoxidáveis austeníticos da série 200 e série 300 disponíveis na literatura em relação ao comportamento da transformação de fase induzida pela deformação e da resistência à corrosão. Os principais fatores que afetam a microestrutura no endurecimento por deformação são: a energia de defeito de empilhamento, composição química, temperatura, grau, taxa e modo de deformação. Realizou-se uma análise crítica e adequação dos conceitos de níquel e cromo equivalente para os aços AISI 201 e AISI 304. Amostras desses aços foram solubilizadas, laminadas e racionadas em diferentes condições para caracterização microestrutural com o auxílio de técnicas de microscopia óptica, microscopia eletrônica de varredura, difração de raios X, ferritoscópio e microdureza. Curvas de endurecimento em função do grau de deformação, fração volumétrica de martensita em função do grau de deformação, assim como a evolução microestrutural e sua respectiva identificação de fase com o grau de deformação foram resultados obtidos deste trabalho. Em geral, aumentando a deformação plástica a frio, maior é a dureza para ambos os aços e maior é a fração volumétrica de martensita induzida por deformação. O aço AISI 201 é mais susceptível a transformação de fase do que o aço AISI 304 devido a sua menor EDE. Ensaios eletroquímicos de espectroscopia de impedância eletroquímica e polarização potenciodinâmica anódica foram realizados para avaliação da resistência a corrosão e para avaliar o comportamento da repassivação. Ambos os aços apresentaram comportamento similares quanto à resistência à corrosão, além de apresentarem potenciais de corrosão da ordem de 10-8 A/cm², típico de materiais passivos. / The continuous increase in the application demand of austenitic stainless steels and the constant pressure for cost reduction in the steelmaking industry, due to the high instability of nickel price, has conduced to new developments of the AISI 200 series steels. This new austenitic stainless steel series employes high manganese and nitrogen contents in substitution to nickel. The reason of this work is the lack of comparative studies in the literature between austenitic stainless steels of 200 and 300 series relative to the martensite strain induced phase transformation and its corrosion resistance. The main factors that affect microstructure on strain-hardening are: stacking fault energy, chemical composition, temperature, strain and strain rate. A critical analysis of the concept related to the nickel and chrome equivalents for the AISI 201 and AISI 304 steels has been carried out. Samples of these steels were heat treated and cold rolled to different strains for subsequent microstructural evaluation using equipments such as optical microscope, scanning electron microscope, X-ray diffraction, microhardness and ferritoscope. Strain hardening versus strain, martensite volume fraction versus strain, as well as microstructure evolution and its respective phase identification with strain are some of the main results obtained in this study. In general, increasing the strain hardening, the higher will be the hardness of both stainless steels and higher is the induced martensite volume fraction. The AISI 201 steel presented higher susceptibility to induced phase transformation in comparison to the AISI 304 steel due to its lower stacking fault energy. Electrochemical impedance spectroscopy and anodic potenciodynamic polarization were the techniques used in this work to evaluate the corrosion resistance and passivation behavior respectively. Both steels presented similar corrosion resistance, apart from presenting a corrosion potential of about 10-8 A/cm² , which is typical for passivated materials.

A crescente demanda de aplicações de aços inoxidáveis austeníticos e a constante pressão para redução de custo nas empresas siderúrgicas, devido à alta volatilidade no custo do níquel, resultaram em novos desenvolvimentos de aços da série 200. Esta nova classe de aços inoxidáveis austeníticos contém elevados teores de manganês e nitrogênio em substituição ao elemento níquel. A justificativa para a realização deste trabalho é a escassez de estudos comparativos entre aços inoxidáveis austeníticos da série 200 e série 300 disponíveis na literatura em relação ao comportamento da transformação de fase induzida pela deformação e da resistência à corrosão. Os principais fatores que afetam a microestrutura no endurecimento por deformação são: a energia de defeito de empilhamento, composição química, temperatura, grau, taxa e modo de deformação. Realizou-se uma análise crítica e adequação dos conceitos de níquel e cromo equivalente para os aços AISI 201 e AISI 304. Amostras desses aços foram solubilizadas, laminadas e racionadas em diferentes condições para caracterização microestrutural com o auxílio de técnicas de microscopia óptica, microscopia eletrônica de varredura, difração de raios X, ferritoscópio e microdureza. Curvas de endurecimento em função do grau de deformação, fração volumétrica de martensita em função do grau de deformação, assim como a evolução microestrutural e sua respectiva identificação de fase com o grau de deformação foram resultados obtidos deste trabalho. Em geral, aumentando a deformação plástica a frio, maior é a dureza para ambos os aços e maior é a fração volumétrica de martensita induzida por deformação. O aço AISI 201 é mais susceptível a transformação de fase do que o aço AISI 304 devido a sua menor EDE. Ensaios eletroquímicos de espectroscopia de impedância eletroquímica e polarização potenciodinâmica anódica foram realizados para avaliação da resistência a corrosão e para avaliar o comportamento da repassivação. Ambos os aços apresentaram comportamento similares quanto à resistência à corrosão, além de apresentarem potenciais de corrosão da ordem de 10-8 A/cm², típico de materiais passivos. / The continuous increase in the application demand of austenitic stainless steels and the constant pressure for cost reduction in the steelmaking industry, due to the high instability of nickel price, has conduced to new developments of the AISI 200 series steels. This new austenitic stainless steel series employes high manganese and nitrogen contents in substitution to nickel. The reason of this work is the lack of comparative studies in the literature between austenitic stainless steels of 200 and 300 series relative to the martensite strain induced phase transformation and its corrosion resistance. The main factors that affect microstructure on strain-hardening are: stacking fault energy, chemical composition, temperature, strain and strain rate. A critical analysis of the concept related to the nickel and chrome equivalents for the AISI 201 and AISI 304 steels has been carried out. Samples of these steels were heat treated and cold rolled to different strains for subsequent microstructural evaluation using equipments such as optical microscope, scanning electron microscope, X-ray diffraction, microhardness and ferritoscope. Strain hardening versus strain, martensite volume fraction versus strain, as well as microstructure evolution and its respective phase identification with strain are some of the main results obtained in this study. In general, increasing the strain hardening, the higher will be the hardness of both stainless steels and higher is the induced martensite volume fraction. The AISI 201 steel presented higher susceptibility to induced phase transformation in comparison to the AISI 304 steel due to its lower stacking fault energy. Electrochemical impedance spectroscopy and anodic potenciodynamic polarization were the techniques used in this work to evaluate the corrosion resistance and passivation behavior respectively. Both steels presented similar corrosion resistance, apart from presenting a corrosion potential of about 10-8 A/cm² , which is typical for passivated materials.

Cette thèse est une étude expérimentale du comportement thermo-mécanique superélastique d'un fil nanocristallin Ti-50.9Ni at.% Ni en alliage à mémoire de forme (SMA) (diamètre 0.5 mm), après subir un cold work (CW). Les AMF sont capables d'induire des changements de température importants lorsqu'ils sont chargés mécaniquement. Ce phénomène est dû à un important couplage thermomécanique présent dans cette transformation de phase solide entre les phases Austénite (A) et Martensite (M).La chaleur latente par unité de masse (ΔH) tout au long de la transformation de phase est l'énergie responsable de cette variation de température. La détermination de ΔH est généralement effectuée par calorimétrie à balayage différentiel (DSC). Cependant, pour les SMA nanocristallins, les résultats DSC obtenus ne sont pas concluants sur la détermination de cette propriété.Dans ce travail, une méthode utilisant la corrélation d'image numérique (DIC) et les mesures de champ thermique (TFM) a été utilisée pour analyser les couplages thermomécaniques lors d'une transformation de phase induite par contrainte. Des champs cinématiques et thermiques ont été acquis lors d'essais de traction superélastiques réalisés sur des fils CW NiTi soumis à différentes températures de traitements thermiques (TTT) allant de 523 à 598 K pendant 30 min. Un tel traitement thermique à basse température favorise une boucle totalement superélastique sans plateau de contrainte et sans déformation de type Lüders. En supposant un modèle thermique uniforme, les sources de chaleur impliquées lors du chargement cyclique ont été estimées. Cette puissance thermique par unité de masse a été comparée à la puissance mécanique et intégrée au fil du temps pour obtenir l'équilibre énergétique. De plus, grâce à une analyse thermodynamique basée sur l'énergie libre de Gibbs, les valeurs de ΔH, ainsi que la fraction de martensite, ont été estimées au cours des transformations de phase A-M directe et inverse M-A. L'analyse des résultats a conduit aux conclusions suivantes: (1) Les puissances et énergies thermiques et mécaniques présentaient une dépendance significative vis-à-vis du TTT. (2) Malgré l'effet important des valeurs du TTT sur les réponses mécaniques et thermiques, les ΔH obtenues étaient très proches pour tous les TTT et dans la même gamme de valeurs fondée dans la littérature pour un alliage Ti-50.9Ni at.% Ni entièrement recuit testé par technique DSC. (3) Pour une deformation donnée, la fraction de martensite augmente avec l'augmentation de TTT. (4) Pour une contrainte imposée de 4,5%, la fraction de martensite augmente de 30% à 40% en augmentant le TTT de 523K à 598K. / This PhD thesis is an experimental study of the thermomechanical superelastic behaviour of a Ti-50.9Ni at.% Ni Shape Memory Alloy (SMA) nanocrystalline thin wire (diameter 0.5 mm), in a Cold Worked (CW) state. SMAs are capable of inducing important temperature change when they are mechanically loaded. This phenomenon is due to an important thermomechanical coupling present in this solid phase transformation between Austenite (A) and Martensite (M) phases. The latent heat per unit of mass (∆H) throughout the phase transformation is the energy responsible of this temperature variation. The determination of ∆H is generally performed by differential scanning calorimetry (DSC). However, for nanocrystalline SMAs, the obtained DSC results are non conclusive on the determination of this property.In this work, a method using digital image correlation (DIC) and thermal field measurements (TFM) was used to analyse the thermomechanical couplings during a stress induced phase transformation (SIPT). Kinematics and thermal full fields were acquired during superelastic tensile tests performed on the CW NiTi wire submitted to different heat treatments temperatures (HTT) ranging from 523 to 598 K during 30 min. Such a heat treatment at low temperature promoted a fully superelastic loop without stress plateau and no Lüders-like deformation. Assuming a uniform thermal model, the heat sources involved during the cyclic loading were estimated. This thermal power per unit of mass was compared to the mechanical one and integrated over the time to get energy balance. Further, through a thermodynamic analysis based on the Gibbs free energy, the values of ∆H, as well as the martensite fraction, were estimated during the forward A-M and reverse M-A phase transformations. The analysis of the results led to the following conclusions: (1) Thermal and mechanical powers and energies presented a significant dependence on the HTT. (2) Despite the strong effect of the values of the HTT on mechanical and thermal responses, the obtained ∆H were very close for all HTT and in the same range of values founded in the literature for a fully annealed Ti-50.9Ni at.% Ni alloy tested via DSC technique. (3) For a given strain, martensite fraction increases with increasing HTT. (4) For an imposed strain of 4.5%, the martensite fraction increases from 30% to 40% when increasing HTT from 523K to 598K.

Made available in DSpace on 2016-03-15T19:36:57Z (GMT). No. of bitstreams: 1 Dante da Costa Ribeiro.pdf: 1584757 bytes, checksum: 5a421e40bb3ea48cad64df542faaceb6 (MD5) Previous issue date: 2009-04-24 / Martensitic Stainless Steel hás always been used in the injection moulds because of their properties as high polishability and high corrosion resistence that alows it to inject some kind of polymers, such as PVC, because of its resistance to chlorinate gas that the process normally has, and in the injection of acrylic because of its high finishing surface state that the mould needs and, consequently, of the injected product, that are characteristics intrinsics to those materials. Beside the martensitic stainless steel, the stainless aged steel are very used, but, in such applications this steel are not able to suffer the nitriding process, what make its application not so good because there are no ways to increase its surface. In this paper will be studied about aged stainless steel that will pass through the shot peening process and without this process to see how will be the surface result. As there are no literatures about this subject, because besides it is about some old tecnologies, the study shall result in a new application of those techniques making a revolution in the utilization of those materials in some industrial applications as plastic moulds and mechanichal devices. / Os aços inoxidáveis martensíticos sempre foram muito utilizados no ramo de moldes plásticos devido as suas propriedades como alta polibilidade e resistência à oxidação elevada, que permitem a injeção de certos polímeros, como o policrilato de vinila, por conta de sua resistência aos gases clorídricos desprendidos no processo e também na injeção de acrílico por causa do alto grau de acabamento que pode ser conferida à superfície do molde e, conseqüentemente, ao produto injetado, são características intrínsecas a tais materiais. Fora os materiais inoxidáveis martensíticos, os endurecíveis por precipitação também são muitíssimo utilizados, porém, em algumas aplicações tais aços não são passíveis do processo termoquímico de nitretação, o que prejudica a sua utilização por conta de não ter nenhum processo onde um endurecimento superficial seja aplicado. Neste trabalho será realizado o estudo sobre os aços endurecíveis por precipitação passando pelo processo de shot peening e sem passar por tal processo afim de se verificar como ficará a superfície após tal processo. Como faltam literaturas sobre comparativos a respeito desta aplicação por apesar de se tratar de tecnologias antigas, o estudo poderá resultar em uma nova utilização de tais técnicas revolucionando a utilização destes materiais em certas aplicações industriais como em moldes plásticos e em dispositivos mecânicos.

Due to its hardness, martensite, perhaps, is the most desirable structure, but at the same time, martensite is very brittle. Balancing between hardness and brittleness is a challenge that steel manufacturers must deal with it. To decrease brittleness and to solve this problem, designers purposely temper the steel. Heat treatment, e.g., slowing down the quenching quota/rate, will form a procedure of martensite formation incomplete phase and consequently a mixture of austenite-martensite. Tempering is another alternative to operate on martensite and make it malleable without losing hardness and preventing brittleness. As its seen, the heat treatment for controlling the mechanical chemical property is crucial. Managing the critical temperature, A1, A3, and Ms) during martensite formation, which influences the transformation process, must be considered. The Prior Austenite Grain Size also has been measured.  This project has examined the critical temperature for three wire steel specimens to determine the martensite start temperature (Ms), microstructure, and hardness. The project has mainly used dilatometry. Besides that, light optical microscopy (LOM), hardness measurement of specimens, and empirical equations for determining the critical temperatures have been used. This work has been made up of two main parts: literature review and experimental work/ project procedure.

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.

Die verformungsinduzierten Phasenumwandlungen und die Zwillingsbildung wurden in drei metastabilen austenitischen Cr-Mn-Ni-Stählen mit unterschiedlichem Nickelgehalt im breiten Temperaturbereich untersucht. Die entwickelten STU- und DTU-Diagramme fassen die gewonnenen Erkenntnisse zusammen und charakterisieren die verformungsinduzierten Gefügeänderungsprozesse in Abhängigkeit von der Spannung und der Temperatur. Die thermodynamischen Berechnungen bestätigen die Unterschiede in der chemischen Triebkraft für die Martensitumwandlung zwischen den Stählen und erklären unterschiedliches Werkstoffverhalten. Ein thermodynamisch-mechanisches Modell der verformungsinduzierten α‘-Martensitbildung wurde entwickelt. Der maximale α‘-Martensitanteil wird als Funktion der Gesamttriebkraft und der Temperatur mit einer guten Genauigkeit beschrieben. Des Weiteren wurde ein Modell der Umwandlungsplastizität mit Berücksichtigung der Plastizitätsverringerung infolge der isothermen oder spannungsinduzierten Martensitbildung entwickelt. Außerdem wurde der Einfluss von Mikroseigerungen auf die verformungsinduzierte Martensitbildung anhand drei Modellstähle untersucht und bestätigt.

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.

Цель работы – установление влияния нейтронного облучения на стабильность структуры и фазового состояния ферритно-мартенситной стали ЭП823. Данная работа посвящена анализу влияния нейтронного облучения на фазовые и структурные составляющие стали. Исследования проводились на образцах оболочек твэлов, облученных в составе материаловедческой сборки в реакторе БН-600 при температурах 570, 600, 660 ˚С до повреждающих доз 51,3, 75,1 и 81,1 сна. Определялись методами металлографии и стереометрического анализа характеристики структурных составляющих, вторичных фаз, образовавшихся в процессе облучения, оценивались характеристики радиационной пористости, плотность дислокаций. Исследования были выполнены на сканирующем электронном микроскопе MIRA3 FEG-SEM, оснащенном детекторами вторичных и отраженных электронов и приставкой энергодисперсионного анализа характеристического рентгеновского излучения x-Act 6 фирмы Oxford Instruments. Так же проводились исследования на просвечивающем электронном микроскопе фирмы JEM-2000EX при ускоряющем напряжении 100 кВ в просвечивающем режиме. Количественная обработка изображений для получения размерных характеристик выделений проводилась с использованием программного обеспечения «Цифровая фотолаборатория SIAMS Photolab», а также при помощи программного обеспечения сканирующего электронного микроскопа MIRE3 FEG-SEM. Проведенное исследование стали Х12НМВБФСР в исходном состоянии показало, что ее структура состоит из мартенсита, остаточного феррита, крупных карбидов на основе Nb и по границам ферритных зерен и мартенситных реек, образуются карбиды типа М23С6. После нейтронного облучения содержание карбидов типа М23С6 увеличивается, в зернах феррита образуется χ-фаза, у которой с повышением температуры облучения понижается концентрация и увеличивается в размерах, по границам обнаружена мелкодисперсная α-фаза, обогащенная хромом, которая при повышенных температурах исчезает, так же по границам зерен мартенсита наблюдается небольшое количество радиационных пор. Прошедшие изменения микроструктуры под воздействием нейтронного облучения не привели к существенным изменениям механических свойств. / The aim of the work is to establish the effect of neutron irradiation on the stability of the structure and phase state of the EP823 ferrite-martensitic steel. This work is devoted to the analysis of the effect of neutron irradiation on the phase and structural components of steel. The studies were carried out on samples of fuel rod shells irradiated as part of a materials science assembly in the BN-600 reactor at temperatures of 570, 600, 660 ℃ to damaging doses of 51.3, 75.1, and 81.1 dpa. The characteristics of structural components and secondary phases formed during irradiation were determined by metallography and stereometric analysis, and the characteristics of radiation porosity and dislocation density were evaluated. The studies were performed using a MIRA3 FEG-SEM scanning electron microscope equipped with secondary and reflected electron detectors and an x-Act 6 energy dispersive analysis of characteristic X-ray radiation from Oxford Instruments. Studies were also carried out on a transmission electron microscope of the JEM-2000EX company at an accelerating voltage of 100 kV in the transmission mode. Quantitative image processing to obtain the dimensional characteristics of the secretions was carried out using the software "Digital Photo Laboratory SIAMS Photolab", as well as using the software of the scanning electron microscope MIRE3 FEG-SEM. The study of steel X12NMVBFSR in the initial state showed that its structure consists of martensite, residual ferrite, large carbides based on Nb and along the boundaries of ferritic grains and martensitic rails, carbides of the M23C6 type are formed. After neutron irradiation, the content of carbides of the M23C6 type increases, a χ-phase is formed in the ferrite grains, in which the concentration decreases and increases in size with an increase in the irradiation temperature, a fine alpha-phase enriched in chromium is found along the boundaries, which disappears at elevated temperatures, as well as a small number of radiation pores are observed along the boundaries of martensite grains. The past changes in the microstructure under the influence of neutron irradiation did not lead to significant changes in the mechanical properties.