Materiais magnetostrictivos, como o TERFENOL-D (Tb0,27-0,30Dy0,73-0,70Fe2) e o GALFENOL (Fe72-82Ga18-28), são aplicados em diversos tipos de atuadores, sensores e coletores de energia. Contudo, existe a necessidade de novos materiais que sejam mais baratos, ambientalmente amigáveis e com melhores propriedades mecânicas. Por essa razão, as ligas de Fe-Al são uma alternativa, já que o alumínio é mais abundante na natureza e é sete vezes mais barato que o gálio. O objetivo desse trabalho foi estudar a influência de dois tratamentos termomecânicos nas propriedades magnéticas das ligas (Fe1-xAlx)98,4B1,6, onde x = 0,18; 0,13 e 0,21. No primeiro processamento, as ligas foram submetidas a um tratamento térmico sob compressão para introduzir uma anisotropia magnetocristalina extrínseca. Para compressões de até 180 MPa, as ligas tratadas sob tensão obtiveram valores de magnetostricção e dos coeficientes piezomagnéticos maiores que o das ligas sem tratamento. Ou seja, este processamento aumentou a sensibilidade das ligas como atuador (d33) e sensor (d33 *). No segundo processamento termomecânico, amostras com formato de chapa foram laminadas e tratadas termicamente para induzir um crescimento anormal de grãos e consequentemente uma textura. Embora não tenha ocorrido crescimento de grão anormal durante o tratamento térmico, os valores de magnetostricção foram maiores que o das amostras como fundidas. Ambos processamentos termomecânicos foram efetivos para melhorar as propriedades magnéticas e a liga (Fe0,87Al0,13)98,4B1,6 foi a que obteve os maiores valores de magnetostricção e dos coeficientes piezomagnéticos. Em outras palavras, dentre as ligas estudadas, esta composição foi mais promissora para ser aplicada em atuadores e sensores. / Magnetostrictive materials, like TERFENOL-D (Tb0.27-0.30Dy0.73-0.70Fe2) and GALFENOL (Fe72-82Ga18-28), are applied in several types of sensors, actuators and energy harvesting. Nevertheless, there is the necessity of new materials that are cheaper, environmentally friendly and with good mechanical properties. For that reason, the Fe-Al alloys are an alternative, since the aluminum is more abundant in nature and is seven times cheaper than gallium. The goal of this work is to study the influence of two thermomechanical proceeding at magnetic properties of the (Fe1- xAlx)98.4B1.6 alloys, which x = 0.18; 0.13 e 0.21. At the first proceeding, the alloys were submitted to a stress annealing to introduce an extrinsic magnetocrystalline anisotropy. Up to 180 MPa of compression stress, stress annealed alloys have magnetostriction and piezomagnetic coefficient values higher than the alloys without annealing. In other words, this proceeding increased the alloys sensibility to be applied like actuators (d33) and sensors (d33 *). At the second thermomechanical proceeding, samples with sheet format were rolled and annealed to induce an abnormal grain growth and, consequently, a texture. Although the annealing not produced an abnormal grain growth, the magnetostriction values are higher than for the as-cast samples. Both proceedings were efficient to improve the magnetic properties and the (Fe0.87Al0.13)98.4B1.6 alloy achieved the higher values of magnetostriction and piezomagnetic coefficient. In another words, between the studied alloys, this composition was the most promising to be applied like actuators and sensors.

Orientador: Antonio Jose Ramirez Londono / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-21T15:16:14Z (GMT). No. of bitstreams: 1 Santos_TiagoFelipedeAbreu_D.pdf: 110699747 bytes, checksum: 6759b8c1d313c0a5ec2220e3fd107447 (MD5) Previous issue date: 2012 / Resumo: Juntas consolidadas a topo com penetração completa, livres de defeitos, foram obtidas usando a técnica de soldagem por atrito com pino não consumível em chapas de 6 mm de espessura para os aços inoxidáveis duplex UNS S32101 e S32205 e os superduplex UNS S32750 e S32760. Testes de dobramento de raiz indicaram a penetração completa e a ausência de trincas bem como inspeção por líquido penetrante. A penetração completa foi atingida quando o aporte energético aumentou de 0,89 kJ/mm para 1,43 kJ/mm. Os testes de tração na junta soldada evidenciaram a falha no MB e o aumento da resistência mecânica da junta associada à uma boa ductilidade, exceto para o UNS S32760. Mapas de dureza mostraram o aumento da dureza em toda junta soldada em relação ao metal de base. Avaliação microestrutural mostrou um pronunciado refinamento do tamanho de grão médio de ambas as fases (ferrita e austenita) na junta soldada para os materiais estudados. A avaliação por microscopia de transmissão indicou a evolução de arranjos celulares formando contornos de grão na ferrita corroborando o mecanismo de recuperação e rescristalização dinâmica contínua. Análise por meio da técnica de EBSD mostrou elevada fração de contornos de grão do tipo 'sigma' na 'gama' indicando a recristalização dinâmica descontínua desta fase. Os AID S32205, S32750, S32760 mostraram sutis alterações na resistência à corrosão para meios com diferentes concentrações de cloretos (3,5% NaCl e 1 M NaCl). Porém, para concentrações mais altas o AISD S32760 exibiu importante decréscimo de resistência a corrosão. Este comportamento foi associado à maior fração de ferrita e a precipitação do nitreto de cromo na junta soldada. O AID S32101 mostrou diminuição da resistência à corrosão na condição como soldado / Abstract: Fully consolidated and full penetration butt joints were produced using friction stir welding (FSW) on 6 mm thick plates of UNS S32101 lean duplex stainless steel (LDSS), S32205 duplex stainless steel (DSS) and S32750 and S32760 superduplex stainless steels (SDSS) with heat input of 1.43 kJ/mm. Liquid penetrant inspection showed the full penetration obtained in the welded joints which was corroborated with the bending tests. Transverse tensile tests of the welded joints failed at the base metal revealing an overmatching weld metal. Moreover, longitudinal tensile tests of the welded joints presented an increase of the yield and tensile strength for all joints together with the elongation, but for UNS S32760, which showed a ductility reduction. Microhardness revealed a hardness increase for all the joints, while the SDSSs presented a more homogeneous hardeness areas of joint. Microstructural evaluation indicated a pronounced grain refinement in the welded joints for all the studied materials achieving down to 1 ?m grain size. Transmission electron microscopy and EBSD indicated dislocation cells evolving towards grain boundaries that corroborates the occurrence of dynamic recovery followed by continuous dynamic recrystallization for ferrite. Austenite exhibited high fraction of high angle grain bondaries associated with 'sigma' boundaries indicating the discontinuous dynamic recrystallization. DSS UNS S32205, SDSS UNS S32750, and S32760 showed good corrosion behavior for 3.5% NaCl and 1 M NaCl environments. However, with the increase of chlorides concentrations, the SDSS UNS S32760 exhibited strong decrease of corrosion performance. This behavior was associated with a combination of high ferrite fraction and chromium nitride precipitation. DSS S32101 exhibited a decrease of corrosion performance when welded / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

Abstract Austenitic high-Mn (15–30 wt.%) based twinning-induced plasticity (TWIP) steels provide great potential in applications for structural components in the automotive industry, owing to their excellent tensile strength-ductility property combination. In certain cases, these steels might also substitute austenitic Cr-Ni stainless steels. The aim of this present work is to investigate the high-temperature flow resistance, recrystallisation and the evolution of microstructure of high-Mn steels by compression testing on a Gleeble simulator. The influence of Al alloying (0–8 wt.%) in the hot rolling temperature range (800°C–1100°C) is studied in particular, but also some observations are made regarding the influence of Cr alloying. Microstructures are examined in optical and electron microscopes. The results are compared with corresponding properties of carbon and austenitic stainless steels. In addition, the mechanical properties are studied briefly, using tension tests over the temperature range from -80°C to 200°C. Finally, a preliminary study is conducted on the corrosion behaviour of TWIP steels in two media, using the potentiodynamic polarization technique. The results show that the flow stress level of high-Mn TWIP steels is considerably higher than that of low-carbon steels and depends on the Al concentration up to 6 wt.%, while the structure is fully austenitic at hot rolling temperatures. At higher Al contents, the flow stress level is reduced, due to the presence of ferrite. The static recrystallisation kinetics is slower compared to that of carbon steels, but it is faster than is typical of Nb-microalloyed or austenitic stainless steels. The high Mn content is one reason for high flow stress as well as for slow softening. Al plays a minor role only; but in the case of austenitic-ferritic structure, the softening of the ferrite phase occurs very rapidly, contributing to overall faster softening. The high Mn content also retards considerably the onset of dynamic recrystallisation, but the influence of Al is minor. Similarly, the contribution of Cr to the hot deformation resistance and static and dynamic recrystallisation, is insignificant. The grain size effectively becomes refined by the dynamic and static recrystallisation processes. The tensile testing of TWIP steels revealed that the Al alloying and temperature have drastic effects on the yield strength, tensile strength and elongation. The higher Al raises the yield strength because of the solid solution strengthening. However, Al tends to increase the stacking fault energy that affects strongly the deformation mechanism. In small concentrations, Al suppresses martensite formation and enhances deformation twinning, leading to high tensile strength and good ductility. However, with an increasing temperature, SFE increases, and consequently, the density of deformation twins decreases and mechanical properties are impaired. Corrosion testing indicated that Al alloying improves the corrosion resistance of high-Mn TWIP steels. The addition of Cr is a further benefit for the passivation of these steels. The passive film that formed on 8wt.% Al-6wt.%Cr steel was found to be even more stable than that on Type 304 steel in 5–50% HNO3 solutions. A prolonged pre-treatment of the steel in the anodic passive regime created a thick, protective and stable passive film that enhanced the corrosion resistance also in 3.5% NaCl solution.

Abstract In this thesis, methods to process ultrafine ferritic (UFF) structures in steels, i.e. grain sizes below about 3 μm have been investigated. It is shown here, in accordance with the results in the literature, that a steel with a UFF grain size can be obtained by two methods, more or less convenient to mass production: deformation-induced ferrite transformation from fine-grained austenite (the DIF route) and the static recrystallization of various heavily cold-worked initial microstructures (the SRF/SRM route). In the present work, the influencing factors in the processing of UFF structure in the DIF route have been systematically studied in four low-carbon steels: one C-Mn steel and Nb, Nb-Ti and Nb-high Ti microalloyed steels. A high strain, a low deformation temperature close to Ar3 and a fine prior austenite grain size are beneficial to promote the formation of UFF grains. Especially by using complex pretreatments to refine the prior austenite grain size, cold rolling, repeating the low-temperature reheating cycle or using martensitic initial microstructure, a UFF grain size can be obtained in these steels at the strain of 1.2 (70% reduction) at 780 °C. By controlling the cooling rate, the type of the second phase can be adjusted. When using the static recrystallization route, it was found that UFF is difficult to obtain from a single-phase ferrite, but it is relatively readily obtained from deformed pearlite, bainite or martensite, especially in high-carbon steels with 0.3–0.8%C. In deformed pearlite, the cementite lamellae fragmented and spheroidised in the course of heavy deformation can provide numerous nucleation sites by the particle stimulated nucleation mechanism and retard the subgrain and recrystallized grain growth. Nucleation and retardation of grain growth are effective also in deformed bainite, martensite or high-carbon tempered martensite, as discussed in detail in the work. The thermal stability of UFF grained steels was tested and found to be generally excellent, but it varies depending on the processing method. The UFF structure obtained by the SRM route has a thermal stability somewhat weaker than that of the DIF route. For a given steel, UFF grains may show different grain growth modes, related to the dispersion of second phase particles. In the DIF structure, abnormal grain growth occurs at 700 °C after about 2.5 h, while in the SRM structure, normal grain growth takes place slowly at 600 °C. Carbides on the grain boundaries seem to play an important role in inhibiting grain coarsening. No coarse-grained zone was formed at the HAZ of electron beam or laser welded seams, as performed at low heat inputs (up to 1.5 kJ/cm) on thin strips. The hardness even increased from the base metal towards the HAZ and the weld metal in all seams as an indication that they were hardened during the rapid cooling.

Eutectoid steel strips are designed for the production of parts for intensive use such as clutches, seat slides, and springs as they exhibit<p>excellent strength levels and wear resistance. These properties arise from the unique morphology of lamellar pearlite which can be considered<p>as a self-laminated nanoscale composite. However, a spheroidization annealing step is nowadays necessary to improve the cold forming properties before further cold rolling steps.<p>This thesis is aimed at improving the tensile ductility of the hot rolled products of eutectoid composition in order to eliminate the intermediate<p>annealing step. Two strategies are proposed.<p>The first is to transpose the concept of controlled rolling developed for HSLA to<p>eutectoid steels. Through a strict adjustment of the austenite processing and of the cooling strategy, it is possible to improve the ductility<p>of the final lamellar microstructure. The way the processing parameters influence the hot deformation of austenite, the eutectoid transformation and of the subsequent spheroidization annealing is deeply<p>investigated. It is found that refinement and pancaking of austenite<p>is beneficial as it reduces the pearlite block size improving the total<p>tensile elongation. Accelerated cooling is of paramount importance to<p>achieve fine Interlamellar spacing (ILS), which lead to high strength<p>levels and accelerate spheroidization during subsequent annealing.<p>The second approach involves intercritical or warm deformation. Warm processing of eutectoid steels is first explored by torsion testing<p>and then up-scaled to a pilot rolling-line. The interactions between thermomechanical parameters, rolling forces generated and microstructural<p>evolution are carefully scrutinized. During concurrent hot deformation, spheroidization of cementite takes place almost instantaneously<p>in both torsion and rolling. The restoration processes occurring in the ferrite matrix depends on the strain path and the strain rates. Low strain rates (0,1 s−1) and simple shear promotes the formation of a recrystallized-like HABs network of about 3μm in size.<p>Plane strain compression and high strain rates (10 s−1) leads to the formation of a typical recovered dislocation substructure (LABs) of 1μm in size. During annealing, no recrystallization occurs and the LABs substructure remains stable. This substructure influences drammatically the mechanical properties: the strength is very high and the work-hardening behavior is poor due to high recovery rate in the region close to the LABs. However, due to the presence of spheroidized<p>cementite particles the ductility of warm rolled eutectoid steels is higher than that of ultra fine grained low carbon steels. / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished

Abstract In this thesis, the influence of reversion and recrystallization annealing on microstructure and mechanical properties was studied in metastable austenitic low-Ni high-Mn stainless steels, some alloyed with up to 0.45 wt.% Nb. Further, the effect of the various microstructures created by reversion and recrystallization on strain-induced martensite transformation in tensile testing was investigated. The aim was to achieve excellent combinations of strength and ductility in the steels and to improve understanding of the behaviour of ultrafine-grained austenitic stainless steels during deformation. All the steels were cold-rolled up to 60% thickness reduction producing up to 60% strain-induced &#945;’-martensite in the austenitic structure. Annealing was carried out using a Gleeble thermomechanical simulator between 450–1100 &#176;C for durations of 0.1–1000 s. The resultant microstructures were examined using different research equipment and methods. Regardless of the amount of Nb alloying, shear- and diffusion-controlled reversion could be completed by annealing at 700 &#176;C, although at this temperature no recrystallization of the untransformed cold-rolled austenite occurred. At 800 &#176;C, however, the cold-rolled austenite recrystallized, producing a non-uniform grain structure comprising ultrafine-grained areas formed via reversion and coarser ones formed by recrystallization of the retained austenite. At 900 &#176;C, a uniform fine austenite grain size of about 2 &#956;m was obtained. At higher annealing temperatures of 1000–1100 &#176;C, normal grain growth of fine grains took place during prolonged annealing in steel with no Nb. However, grain growth was effectively retarded by alloying with 0.28 wt.% Nb. The non-uniform structures consisting of reverted and retained austenite exhibited excellent combinations of yield strength and uniform elongation. The results also showed that tensile strain-induced martensite nucleation sites and &#945;’-martensite formation vary in a complex way depending on grain size. / Tiivistelmä Väitöstyössä tutkittiin reversiohehkutuksen vaikutusta metastabiilin 1% nikkeliä ja 9% mangaania sisältävien austeniittisten ruostumattomien terästen mikrorakenteeseen ja mekaanisiin ominaisuuksiin sekä austeniitin raekoon ja mikrorakenteen vaikutusta muokkausmartensiitin syntyyn vetokokeessa. Koeteräksistä osa oli lisäksi niobiseostettuja. Tavoitteena oli nostaa teräksien lujuutta ja ymmärtää ultrahienorakeisen austeniittisten ruostumattomien terästen käyttäytymistä muokkauksessa. Teräkset kylmämuokattiin 60% valssausreduktiolla, jolloin austeniittiseen rakenteeseen muodostui muokkausmartensiittia enimmillään 60%. Reversiohehkutukset tehtiin Gleeble termomekaanisella simulaattorilla lämpötiloissa 450–1100 &#176;C ja 0.1–1000 s pitoajoilla. Saatuja mikrorakenteita tutkittiin eri tutkimuslaitteistoilla ja -menetelmillä. 700 &#176;C hehkutuksessa leikkautumalla ja diffuusion välityksellä tapahtuva reversio oli nopea myös niobi-seostetuilla teräksillä, mutta rekristallisaatiota ei tapahtunut. 800 &#176;C hehkutuksessa muokkauksessa teräksiin jäänyt austeniitti rekristallisoitui, mutta raerakenne muodostui epätasaiseksi koostuen reversion tuottamasta ultrahienoista rakeista ja jäännösausteniitin rekristallisaation tuottamista karkeammista rakeista. Sitä vastoin hehkutus 900 &#176;C:ssa tuotti tasainen 2 &#956;m austeniitin raekoon. Pitkissä hehkutuksissa korkeammissa lämpötiloissa 1000–1100 &#176;C niobi-seostamattomissa teräksissä tapahtui hienojen rakeiden normaalia rakeenkasvua. Kuitenkin 0.28p-% niobi-seostuksen havaittiin oleva riittävä estämään rakeenkasvu. Reversion ja osittaisen rekristallisaation tuottamilla raerakenteilla saatiin erinomaiset myötölujuus-tasavenymäyhdistelmät. Vetokokeissa martensiitin ydintymispaikat ja -nopeus vaihtelivat monimutkaisella tavalla raekoosta riippuen.

L'Inconel 718 est un superalliage base-nickel très utilisé pour la fabrication de pièces aéronautiques soumises à de fortes contraintes et de hautes températures. La maîtrise de la microstructure finale issue de la mise en forme à chaud est un des éléments clés pour le contrôle des propriétés mécaniques et pour répondre aux exigences strictes du secteur. Dans cette étude, l'évolution de la microstructure de l'Inconel 718 est étudiée au moyen d'essais de torsion suivis d'une trempe à l'eau (pour examiner les évolutions dynamiques) ou d'un maintien à la température de déformation puis d'une trempe à l'eau (pour examiner les évolutions post-dynamiques). Ces essais sont réalisés dans les domaines de température δ-supersolvus et δ-subsolvus et pour des vitesses de déformation de 10-2 à 0.1 s-1. Des analyses microstructurales par microscopie électronique à balayage et cartographie des orientations cristallographiques par EBSD sont réalisées pour suivre l'évolution de la fraction recristallisée, de la taille de grains recristallisés ainsi que de l'état de précipitation lors de la déformation et des maintiens pré- et post-déformation. Sur base de ces observations expérimentales, les principaux mécanismes métallurgiques actifs sont identifiés, puis modélisés : écrouissage, germination de nouveaux grains, migration de joints de grains, et interaction avec les particules de seconde-phases. Un modèle d'évolution microstructurale en champ moyen a été enrichi pour prendre en compte l'ensemble de ces mécanismes élémentaires et leur dépendance aux conditions thermomécaniques. Ce modèle permet de décrire, pour les domaines δ-subsolvus et δ-supersolvus, les cinétiques de recristallisation dynamique et post-dynamique de l'Inconel 718, les cinétiques de précipitation et dissolution de la phase δ, ainsi que l'évolution de la taille de grains. Il prédit également les courbes contrainte-déformation dans le domaine de température δ-supersolvus. / Inconel 718 is nickel-based Superalloy widely used in the aeronautic industry to manufacture aircraft parts subjected to extreme in-service conditions of high stresses at elevated temperatures. Controlling the microstructure after hot forming is a key element to control the mechanical properties of the final products and meet the tight specifications imposed by the aeronautic industry.In this work, the microstructure evolution of Inconel 718 was investigated via isothermal and iso-strain rate torsion tests followed by water quenching (to investigate dynamic evolution) or by annealing at deformation temperature then water quenching (to investigate post-dynamic evolution). These tests were conducted in both δ-Supersolvus and δ-Subsolvus temperature domains and for strain rates of 0.01 to 0.1 s-1.Scanning electron microscopy (SEM) and Electron Back Scattered Diffraction (EBSD) were used to characterize the microstructure and follow the evolution of the recrystallized fraction, the recrystallized grain size and the δ-phase precipitation after deformation and during pre-deformation and post-deformation annealing. Based on these experimental observations, the main metallurgical mechanisms have been identified and modelled: hardening, nucleation of new grains, grain boundaries migration and the δ-phase- recrystallization interaction.A two-site mean field approach having a low computational cost was chosen to model the microstructural evolution at different thermomechanical conditions. This model describes the main mechanisms taking place during hot forming of Inconel 718 in both δ-Supersolvus and δ-Subsolvus domains and predicts the recrystallization kinetics in both dynamic and post-dynamic regimes , the δ-phase precipitation and dissolution kinetics and the grain size evolution. The model predicts also the strain-stress curves at high temperatures in the absence of δ-phase particles.

La présente thèse s’inscrit dans un contexte d’optimisation des procédés de forgeage et de traitements thermiques des alliages de titane pour les pièces de moteurs Snecma.Les sociétés TIMET, élaborateur, et SNECMA, motoriste, ont identifié des enjeux très analogues concernant le forgeage des billettes en alliage de titane destinées à la fabrication de disques moteurs. Il est nécessaire d'acquérir une maîtrise complète de la gamme de transformation, de la coulée au produit final. Ce traitement thermomécanique comporte une alternance d’étapes de forgeage dans les domaines bêta, à haute température, et alpha + bêta, à basse température.L’objectif est de déterminer expérimentalement et de modéliser le comportement mécanique ainsi que les évolutions de microstructure de l’alliage Ti17 au cours d'une déformation dans le domaine alpha + bêta suivie d’un maintien en bêta.En amont, ces travaux mènent à une meilleure compréhension des facteurs qui influencent la taille de grain dans le domaine bêta : la taille de grain bêta initiale, les orientations des aiguilles alpha dans le grain, la déformation et la désorientation subies lors du forgeage en alpha + bêta, etc.En ce qui concerne les applications, ils s’intègrent à un post-processeur métallurgique dédié au forgeage des alliages de titane, qui utilise les histoires thermomécaniques issues d’un calcul par éléments finis. / The thesis is part of a broader optimization program related to the forging and the heat treatments of SNECMA-engine components in titanium alloys.TIMET (producer) and SNECMA (engine manufacturer) companies have identified very similar issues concerning the forging of billets in titanium alloy for manufacturing engine discs. They need thus to gain complete control over the transformation range, from the casting to the final product. This thermomechanical treatment involves alternating forging steps in the beta domain, at high temperature, and in the alpha + beta field, at lower temperatures.The aim is to simulate the forging step in the two-phase, alpha + beta, range followed by recrystallization in the beta field during which microstructure evolves. This simulation involves the following phenomena: grain deformation, recrystallization and grain growth of the beta matrix and disorientation/fragmentation of the alpha-Widmanstätten platelets. More specifically, the effects of deformation in the alpha + beta field on the subsequent beta-grain growth during the heat treatment at higher temperatures have been analyzed in the case of Ti17 titanium alloy.Upstream, the work leads to a better understanding of the factors that influence grain size in the beta domain: the initial beta-grain size, the orientation of alpha needles in the grains, the distortion and disorientation experienced during the alpha + beta forging, etc. With regard to the applications, the above results will be implemented into a metallurgical post-processor dedicated to the forging process of titanium alloys, using the thermomechanical history resulting from a finite-element calculation.

L'élaboration des aciers ODS fait appel à une étape de consolidation par filage à chaud. Les propriétés très anisotropes de ces matériaux à l'état filé, notamment les nuances purement ferritiques (>12% Cr), nécessitent une meilleure compréhension des effets du procédé de filage sur la microstructure. Ainsi, ce travail de thèse a pour objectif principal d'étudier les évolutions de la microstructure lors de la transformation à chaud des aciers inoxydables ODS ferritiques, et plus globalement de comprendre le comportement de ces matériaux sous sollicitation mécanique à haute température. Pour cela, des essais de filage interrompus et des essais thermomécaniques de torsion et de compression à chaud (1000-1200°C) ont été réalisés sur plusieurs aciers ferritiques à 14% de Cr présentant différents taux de renfort en titane et en yttrium. Les microstructures obtenues après déformation ont été caractérisées par EBSD.L'ensemble des analyses microstructurales effectuées montre que la mise en forme à chaud des aciers ferritiques par filage s'accompagne d'une recristallisation dynamique de type continue. Après formation des sous-joints par restauration, leurs désorientations continuent à croître, et ceux-ci se transforment graduellement en joints de grains au cours de la déformation. La cinétique de ce mécanisme semble néanmoins fortement influencée par les caractéristiques de la précipitation présente dans le matériau ; la recristallisation devenant moins complète lorsque les précipités sont plus fins et plus nombreux. En plus du taux de renfort, l'étude de la déformation de ces nuances en torsion et en compression dans des conditions proches de celles observées en filage révèle également une forte influence de la température sur leur comportement. Les microstructures de déformation présentent une évolution d'autant plus importante que la température et/ou le taux de renfort sont limités. À 1000°C, les évolutions observées indiquent la présence de la recristallisation dynamique continue. En revanche, lorsque l'on augmente la température et/ou le taux de renfort, la déformation s'accompagne d'une évolution limitée de la microstructure, notamment en torsion où un endommagement sévère aux niveaux des joints de grains est observé. Dans ce cas, les résultats sont interprétés par un mécanisme d'accommodation de la déformation au voisinage des joints de grains. Les paramètres rhéologiques calculés à partir de ces essais mécaniques confirment la tendance à une faible activité plastique au sein des grains dans les nuances renforcées. / The production of ODS steels involves a powder consolidation step usually using the hot extrusion (HE) process. The anisotropic properties of extruded materials, especially in the ODS ferritic grades (>wt%12Cr), need a better understanding of the metallurgical phenomena which may occur during HE and lead to the observed microstructure. The hot working behavior of these materials is of particular interest. The methodology of this work includes the microstructure analysis after interrupted hot extrusion, hot torsion and hot compression (1000-1200°C) tests of ferritic steels with 14%Cr and different amounts in Ti and Y2O3.The microstructure evolution during hot extrusion process is associated with continuous dynamic recrystallization (CDRX). It leads to the creation of new grains by the formation of low angle boundaries, and then the increase of their misorientation under plastic deformation. The investigations highlight also the role of precipitation on the kinetics of this mechanism; it remains incomplete in the presence of fine and dense nanoprecipitates. After hot deformation in torsion and compression, it is noticed that both precipitates and temperature deformation have a significant impact on the deformation mechanisms and microstructure evolution. Indeed, the CDRX is dominant when temperature and amount of reinforcement are limited. However, when they are increased, limited microstructure evolution is observed. In this case, the results are interpreted through a mechanism of strain accommodation at grain boundaries, with low dislocation activity in the bulk of the grains.

Le mottage ou l’agglomération non désirée des cristaux déliquescents est un phénomène récurrent dans l’industrie, notamment au cours du transport et du stockage. Les variations des conditions environnantes sont fréquemment responsables de la dégradation de ce type de poudres. En particulier, les fluctuations de l’humidité ambiante conduisent à la formation d’une solution saturée par déliquescence du solide puis à la formation de ponts solides par évaporation de l’eau. Dans cette étude, on se concentre sur le chlorure de sodium. L’équilibre avec la vapeur d’eau et les cinétiques de prise et perte en eau sont analysés et reliés au comportement mécanique macroscopique des cristaux. Le contact avec des cristaux de différente nature tels que le sucrose met en évidence le phénomène de déliquescence mutuelle. Le modèle des solutions régulières appliqué aux systèmes ternaires comportant du NaCl, du sucrose et de l’eau permet de mieux comprendre la chute de déliquescence. La présence des molécules d’eau à la surface des cristaux et la condensation capillaire à faible humidité relative provoque la déliquescence de NaCl et du sucrose simultanément. L’évaporation de l’eau et la recristallisation des cristaux à partir de la solution ainsi formée sont inhibées, en particulier à la composition solide du point eutonique. Le comportement singulier à cette composition qui s’apparente à celui d’un corps pur montre une recristallisation partielle du mélange "eutonique" associée à la formation d’une phase amorphe dans les conditions de l’expérimentation. Afin d’éviter le renforcement au mottage, l’étude de différents agents anti-mottants révèle l’efficacité du stéarate de magnésium. / Caking or undesired agglomeration of deliquescent crystals is a recurrent phenomenon in industry, especially during transportation and storage. The variation of environmental conditions is often pointed out as a cause of the degradation of this kind of powders. More precisely, the fluctuations of ambient humidity lead to the formation of a saturated solution by deliquescence followed by the formation of solid bridges when water evaporates. Sodium chloride is chosen as a model substance in this study. The equilibrium with water vapor and the kinetics of water uptake and loss are analyzed and related to the mechanical macroscopic behavior of crystals. The contact with crystals of different nature such as sucrose highlights the phenomenon of mutual deliquescence. The model of regular solutions applied to ternary systems containing NaCl, sucrose and water allows a better understanding of deliquescence lowering. The presence of water molecules and capillary condensation at low relative humidity lead to the deliquescence of NaCl and sucrose simultaneously. Water evaporation and recrystallization of solid from such solution is compromised, especially at the solid composition of the “eutonic point”. The singular behavior at this composition which resembles to the one of a pure substance shows a partial recrystallization of the “eutonic” mixture and the formation of an amorphous phase under the experimental conditions applied. In order to avoid caking reinforcement, the study of differentanti-caking agents reveals the efficiency of magnesium stearate.