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There is great interest in understanding the contamination of stainless steel by radionuclides across the nuclear fuel cycle. Through study of uptake mechanisms, contaminant localisation and process conditions that affect uptake, decontamination strategies can be tailored to remove built-up radioactive species. This study focusses on understanding stainless steel contamination by inactive lanthanides and radioactive actinide species (U, Np, Pu and Am) in acidic media. Through depth profiling, contamination has been seen to localise on the interface of the oxide layer and the bulk metal (at depths of up to 100 nm) indicating a potentially tenacious contamination mechanism. Furthermore, contaminant was observed at greater depths within the material (up to ~300 nm), suggesting penetration beyond the passive layer in to the bulk of the material. Long term immersion studies (up to 9 months) in 12 M HNO3 have also been undertaken to investigate the effect of surface corrosion on contaminant uptake. After 3 months the surface had undergone intergranular corrosion and grain droppage was observed. Further surface analysis revealed localisation of contaminants within the steel grain boundaries and vacancies. Once again, this may necessitate a more aggressive decontamination strategy. Conditions have been identified that enhance uptake of transuranic contaminants. Highest levels of uptake were seen in polished steel samples immersed in 4 M HNO3. The Np-237, Pu-239 and Am-241 contaminated samples showed surface concentrations of up to 1.2x107, 9.4x105 and 1x109 Bq/m2, respectively. In the case of Np contamination of stainless steel, microfocus X-ray absorption spectroscopy has shown the surface-mediated reduction of Np(V) leading to Np(IV) adsorption.

This thesis deals with properties of austenitic stainless steel 304L processed by SLM technology and tested at room and cryogenics temperatures. Result is description of mechanical properties and microstructure. First step was to develop processing parameters to achieve porosity of prints fell below 0,01 %. Following tensile test showed higher yield and ultimate tensile strength than conventionally fabricated parts, even at temperature -80 °C, but at cost of reduced ductility. Due to deformation and low temperature austenite transformed into martensite. This transformation also occurred in Charpy toughness test, that resulted in ductile to brittle behaviour.

In this study, the effects of stress and strain rate on cyclic deformation, secondary hardening, martensitic phase transformation, crack initiation, and fatigue behavior of type 304L stainless steel are examined. A series of load and strain controlled uniaxial zero and non-zero mean strain fatigue tests were conducted with varying frequencies in order to investigate the effect of loading rate on fatigue behavior. The volume fraction of martensite was quantified for several tests using x-ray diffraction and electron backscatter diffraction. The loading rates were found to have a direct effect on the microstructure and fatigue behavior of the alloy investigated. Adiabatic heating from an increased rate of loading was found to effect martensite formation which is a major contributor to the secondary hardening phenomena associated with many austenitic stainless steels under cyclic loading. Also affected by the microstructural changes were cyclic deformation, crack initiation, microstructurally small crack growth, and fatigue behavior.

The performance of a coupled viscoplastic model of FSW has been evaluated over a variety of tool RPMs and feed rates. Initial results suggested that further optimization of the material parameters and an additional ability to model the thermal recovery of the material would improve the overall performance of the model. Therefore, an experimental/numeric approach was taken to improve and quantitatively compare the performance of the model based upon the thermal profile of the workpiece. First, an experimental method for obtaining real-time temperature measurements during Friction Stir Processing (FSP) of 304L Stainless Steel was developed. The focus of the method was to ensure that the obtained temperatures were both accurate and repeatable. The method was then used to obtain thermal cycle data from nine welds, each at different operating conditions ranging in tool rotational speed from 300 to 500 RPMs and in feed rate from 0.85 to 2.54 mm/s (2 - 6 in/min). Then a family of nine numerical models was created, each model corresponding to one welding condition. The performance due to improved convergence stability and the added thermal recovery term are also discussed. A gradient following technique was used to optimization and iteratively adjust nine material parameters to minimize the difference between the numerical and experimental temperature for the whole family of models. The optimization decreased the squared error between the numerical and measured temperatures by 76%. Recommendations are also made that may allow the optimization method to return greater dividends.

L’objectif de cette étude e est de comprendre le processus de déalliage de l’acier inoxydable austénitique 304L avec l’intention de transcrire ce raisonnement aux aciers duplex. Des essais ont été réalisés au sein d’une solution aqueuse désaérée d’hydroxyde de sodium à 50%, portés à une température de 80°C sous pression atmosphérique et à potentiel libre. - L’alliage 304L se dissout en formant une couche nanoporeuse riche en nickel métallique sur sa surface. - L’alliage 2202 se dissout et présente deux comportements différents : o la ferrite s’appauvrit en nickel o l’austénite se recouvre d’une couche nanoporeuse constituée de nickel métallique. o les deux phases ont des vitesses de dissolution distinctes, l’austénite se dissolvant plus rapidement que la ferrite. Les cinétiques de dissolution des deux alliages sont différentes : l’alliage 2202 présente une meilleure résistance à la corrosion que l’alliage 304L. Cependant l’austénite de l’alliage 2202 se comporte de manière identique à l’alliage 304L et présente les mêmes caractéristiques. La ferrite semble conférer à l’alliage duplex une protection contre la corrosion caustique au détriment de l’austénite.La mise en évidence de la couche du nickel métallique presque pur est confrontée avec des modèles existants de déalliage. Des expériences complémentaires ont prouvées la simultanéité des étapes de dissolution de l'alliage, de la redéposition des atomes de Ni et de leur réarrangement sur la surface. / The aim of this study is to understand the process of dealloying of austenitic stainless steel 304L with the intention to put this reasoning to the duplex steels. Tests were conducted in a deaerated aqueous solution of sodium hydroxide at 50%, heated to a temperature of 80°C at atmospheric pressure and free potential. • The alloy 304L is dissolved to form a nanoporous layer rich in nickel metal on its surface. • The alloy 2202 is dissolved and has two different behaviors: o Ferritic phase is depleted in nickel o Austenite is covered by a nanoporous layer consists of metallic nickelo The two phases have different dissolution rates: austenite dissolves faster than ferrite. Kinetic dissolution of two alloys is different: alloy 2202 has better corrosion resistance than alloy 304L. However, the behavior of the austenite of the alloy 2202 is identical to the alloy 304L and has the same characteristics. The ferrite appears to give the duplex alloy corrosion protection against caustic at the expense of austenite. The identification of the layer of almost pure metallic nickel is confronted with existing models of dealloying. Additional experiments proved the simultaneous steps of dissolution of the alloy, redeposition of Ni atoms and their rearrangement on the surface.

O aço inoxidável é amplamente utilizado em sistemas para processamento e obtenção de derivados de folhelhos pirobetuminosos. Em função dos problemas de corrosão, originários da composição química dos folhelhos e do processamento em si, são gastos anualmente valores expressivos em manutenção e paradas programadas para reparos nestes sistemas. O presente trabalho busca estudar o processo de corrosão do aço inoxidável AISI 304L em meio simulado de retortagem de folhelhos, em condições de alta temperatura e em presença de elevados teores de enxofre, orgânico e inorgânico, empregando técnicas microscópicas e eletroquímicas. Os resultados mostraram que a temperatura influencia diretamente no processo de corrosão do aço, causando modificação na camada externa de óxidos. Este processo é agravado com a presença de sulfetos no meio, havendo formação, principalmente, de sulfetos de ferro sobre a superfície do aço inoxidável AISI 304L e consequente aumento do processo de corrosão. Foi observado que o enxofre de origem orgânica promove maior destruição da camada de óxido protetor do aço e aumento na formação do filme de sulfeto aderido à superfície deste material. Verificou-se ainda que o processo corrosivo é predominantemente químico, sendo o filme formado considerado protetor, do ponto de vista eletroquímico, no meio eletrolítico estudado / Stainless steel is widely used in systems for processing and obtaining of derivatives of oil shale. Due to the corrosion problems, are spending significant amounts in maintenance and shutdowns for repairs annually in processing these materials. The present work aims to study the corrosion process of stainless steel AISI 304 in simulated media of shale retorting under conditions of high temperature and elevated levels of sulfur, organic and inorganic, using electrochemical and microscopic techniques. The results showed that temperature directly influences the corrosion process of steel, causing modification in the outer layer of oxides with formation of iron sulfides on the surface of steel AISI 304L and consequent increase the corrosion process. This process is enhanced with the presence of sulfur in the simulated media. It was observed that the organic sulfur was a precursor and a catalyst for the studied corrosion process, promoting greater destruction of the protective oxide layer of steel and increase in the formation of iron sulfide deposits on the surface of this material. It was found that the corrosion process is predominantly chemical, with small contribution of electrochemical processes

O aço inoxidável é amplamente utilizado em sistemas para processamento e obtenção de derivados de folhelhos pirobetuminosos. Em função dos problemas de corrosão, originários da composição química dos folhelhos e do processamento em si, são gastos anualmente valores expressivos em manutenção e paradas programadas para reparos nestes sistemas. O presente trabalho busca estudar o processo de corrosão do aço inoxidável AISI 304L em meio simulado de retortagem de folhelhos, em condições de alta temperatura e em presença de elevados teores de enxofre, orgânico e inorgânico, empregando técnicas microscópicas e eletroquímicas. Os resultados mostraram que a temperatura influencia diretamente no processo de corrosão do aço, causando modificação na camada externa de óxidos. Este processo é agravado com a presença de sulfetos no meio, havendo formação, principalmente, de sulfetos de ferro sobre a superfície do aço inoxidável AISI 304L e consequente aumento do processo de corrosão. Foi observado que o enxofre de origem orgânica promove maior destruição da camada de óxido protetor do aço e aumento na formação do filme de sulfeto aderido à superfície deste material. Verificou-se ainda que o processo corrosivo é predominantemente químico, sendo o filme formado considerado protetor, do ponto de vista eletroquímico, no meio eletrolítico estudado / Stainless steel is widely used in systems for processing and obtaining of derivatives of oil shale. Due to the corrosion problems, are spending significant amounts in maintenance and shutdowns for repairs annually in processing these materials. The present work aims to study the corrosion process of stainless steel AISI 304 in simulated media of shale retorting under conditions of high temperature and elevated levels of sulfur, organic and inorganic, using electrochemical and microscopic techniques. The results showed that temperature directly influences the corrosion process of steel, causing modification in the outer layer of oxides with formation of iron sulfides on the surface of steel AISI 304L and consequent increase the corrosion process. This process is enhanced with the presence of sulfur in the simulated media. It was observed that the organic sulfur was a precursor and a catalyst for the studied corrosion process, promoting greater destruction of the protective oxide layer of steel and increase in the formation of iron sulfide deposits on the surface of this material. It was found that the corrosion process is predominantly chemical, with small contribution of electrochemical processes

Une approche expérimentale mettant en œuvre des techniques électrochimiques et mécaniques a été utilisée pour étudier la corrosion sous contrainte (CSC) de l’acier inoxydable 304L dans des électrolytes acides (0,5-5 M H2SO4) avec et sans chlorure. La CSC a été réalisée dans le but d’étudier les aspects cristallographique et cinétique de la rupture. La microscopie électronique à balayage a dévoilé, d’une part, des traces successives au niveau des plans de glissement sur les facettes de la fissure, et d’autre part une vitesse non-linéaire de la fissuration. Une méthode a été proposée pour accéder à la cristallographie de fissuration en utilisant la diffraction d'électrons rétrodiffusés (EBSD). Il a été démontré que les ruptures préférentielles s’effectuent au niveau des plans {111} pour ¾ du temps et des plans {110} le reste du temps. Ces résultats soutiennent les modèles récents de la CSC, tels que la plasticité localisée rehaussée par la corrosion. Les profils d’évolution de la contrainte appliquée/résiduelles ont été déterminés par diffraction des rayons X avant et après CSC. Ces analyses serviront à développer un modèle de rupture micro-mécanique. Lors des essais potentiodynamiques optimisés de corrosion, les taux de dissolution élémentaires et le courant total ont été mesurés en combinant une cellule d'écoulement électrochimique et l'analyse des produits de corrosion par spectroscopie d'émission atomique à plasma à couplage inductif. Ces résultats ont été utilisés, pour séparer la partie de courant consacré à la formation de la couche passive du courant total. Le modèle de conduction ionique sous tension élevée a été mis à jour pour calculer le taux de passivation et l'épaisseur de la couche passive. Les contraintes dans le matériau expliquent une différence mesurable de la cinétique de croissance du film passif et de son épaisseur. / : A multidisciplinary experimental approach of electrochemical and mechanical techniques was employed to study the corrosion of different stress states of 304L stainless steel in acidic electrolytes (0.5-5 M H2SO4) with and without chloride additives. Stress corrosion cracking (SCC) conditions were applied to evidence cracking crystallographical and propagation aspects. Scanning electron microscopy of SCC revealed clear traces of successive slipping planes and consequent dissolutions on the crack facets, and nonlinear crack propagation kinetics. A method was proposed to access cracking crystallography using electron back scattered diffraction. It demonstrated {111} and {110} preferential cracking planes in proportion of about 75% and 25% respectively, which supports recent SCC models such as corrosion enhanced localized plasticity. The profiles of (applied/residual) stress evolution measured by X-ray diffraction before and after SCC were used as an introduction to develop a micro-mechanical cracking model. During optimized potentiodynamic corrosion tests, elemental dissolution rates and total current transients were measured by combining electrochemical flow cell and downstream solution analysis by inductively coupled plasma atomic emission spectroscopy. The results were used to separate the current portion spent on passive film formation from the total current. The high field ion conduction model was upgraded to calculate the constructed passive film thickness and passivation rate. The applied stress caused a measurable difference in passive film growth kinetics and its thickness.

In view of the significant advantages offered by semi-solid processing, such as reduction in number of intermediate processing steps and energy input, and the potential for improving component complexity, it is of paramount interest to develop indigenous technology for semi-solid forming of steels, especially nuclear grade steels. For adopting semisolid processing as an alternative method of manufacturing of steels, it is essential to study the amenability of the steel for the process, understand the fundamental mechanisms of micro structural evolution and evaluate the mechanical properties of the steel after processing. To achieve this goal, the present work attempts to appraise the amenability of a low-carbon variant of 18%Cr-8%Ni austenitic stainless steel (304L SS) for semi-solid processing. Among the many requirements of the feedstock in semi-solid processing, a key feature that makes it amenable for semi-solid processing is the unique microstructure containing solid spheroids in a liquid matrix, thereby enabling thixo-tropic behaviour in the alloy. To understand the micro structural evolution in the steel, during major steps of semi-solid processing (partial melting, soaking and solidification), several experiments are carried out by varying the key parameters such as temperature, soaking time and cooling rate. Experimental results are analyzed in details to specify the effects of these parameters on the microstructure of semi-solid processed steel. The analysis indicates different phase transformation sequences during solidification of the steel from its semi-solid state. On the basis of experimental results, mechanism for micro structural evolution during partial melting and subsequent solidification of 304L SS is proposed. The effect of soaking time on the size and shape of the solid globules is analyzed using the theory of anisotropic Ostwald ripening. The semi-solid processing parameters, such as soaking time and temperature, are found to have significant influence on the globule distribution, globule shape, ferrite distribution and dislocation density, which in turn govern the tensile behaviour and mechanical properties of the steel after processing. Semi-solid processed 304L SS exhibits lower yield strength, ultimate tensile strength and higher strain hardening in temperature range 303–873K compared to as-received (rolled and subsequently annealed) 304L SS. However, semi-solid processed steel shows higher uniform elongation and fracture strain compared to the as-received steel. A pronounced effect of semi-solid processing is also found on the high temperature plasticity and dynamic recrystallization pattern. This work demonstrates the amenability of 300 series austenitic stainless steels for semi-solid processing. The investigation provides the significant insight into the mechanism of micro structural evolution in austenitic stainless steels during semi-solid processing and the important information on the mechanical properties and plastic flow behavior of the semi-solid processed steel. The results give crucial inputs for the optimization of processing parameters for obtaining the desired property in the product, and also for deciding the potential industrial application of the process.