L’acier Ferrium® M54® présente une composition chimique optimisée, basée sur 40 ans d’évolution et de développement des aciers à durcissement secondaire à précipitation de carbures M2C. Le compromis de propriétés Rm/KIC/KISCC obtenu par la nuance M54® permet d’envisager son utilisation dans les trains d’atterrissage d’avions gros porteurs. Cependant, les premiers essais mécaniques, réalisés par l’utilisateur pour la montée en maturité de la nuance, ont montré une variabilité des propriétés mécaniques suivant le traitement thermique appliqué. Ce travail de thèse s’applique donc à décrire les évolutions microstructurales au cours du traitement thermique de la nuance M54® et les impacts sur les propriétés mécaniques en se concentrant notamment sur le traitement par le froid. Les différentes conditions de mise en solution et de revenu testées ont montré une certaine stabilité de la précipitation au revenu et des propriétés mécaniques qui en découlent. La précipitation a été caractérisée à différentes échelles afin de la comparer avec celle issue des nuances de la même famille. En revanche, selon les conditions de traitement par le froid réalisées, la limite d’élasticité varie de manière significative sans qu’aucun des paramètres liés à la précipitation ne soient modifiés. Le taux d’austénite est en revanche un paramètre déterminant pour la limite d’élasticité et est très sensible aux conditions de traitement par le froid : temps et température entre la trempe à l’huile et le traitement cryogénique et température de traitement cryogénique. Un traitement thermique amélioré a ainsi été proposé pour obtenir un taux d’austénite réduit et constant et limiter ainsi les variations de limite d’élasticité. / Ferrium® M54® steel presents an optimized composition, based on 40 years of research and development on secondary hardening steels. This alloy exhibits an excellent Rm/KIC/KISCC balance that allows considering its use in landing gears applications of wide-body aircrafts in the future. However, initial mechanical tests performed by the end-user have shown variability in mechanical properties depending on the applied heat treatment. The main goal of this work is to describe the microstructural evolutions of the alloy M54® during heat treatment and their impact on the resulting mechanical properties with a specific focus on the effect of the cryogenic treatment.The different austenitizing and tempering conditions investigated have shown a stability of the tempering precipitation and mechanical properties. This precipitation has been characterized at different scales and compared with other grades of the same family. On the other hand, depending on cryogenic treatment conditions, a significant variation of the mechanical properties and in particular of the yield strength is observed without any modification in the precipitation distribution and volume fraction or size. Austenite content is critical for the yield strength and is very sensitive to the cryogenic treatment conditions: time and temperature before cryogenic treatment and temperature of cryogenic treatment. An improved heat treatment to obtain reduced and constant austenite content is proposed.

Foram estudados os efeitos da introdução de etapas de tratamento criogênico e do alívio de tensões no ciclo térmico do aço ferramenta para trabalho a frio AISI D2. Variaram-se as temperaturas de tratamento criogênico, sendo elas principalmente: criogênica (-196°C) e subzero (-80°C). Foram variados os tempos de permanência às temperaturas criogênicas: 2, 3, 10, 24 e 30 e 36 horas. Verificou-se o efeito da adição da etapa (130°C/90 minutos) de alívio de tensões previamente ao tratamento criogênico. As amostras com diferentes ciclos térmicos foram submetidas à caracterização metalográfica, difração de raios-X e ensaios de potencial termo-elétrico. Na caracterização metalográfica as amostras foram analisadas por MEV (microscopia eletrônica de varredura) e MEV-FEG (MEV com canhão com emissão por efeito de campo). Os carbonetos secundários (micrométricos) não apresentaram variação. Os carbonetos secundários de revenido (nanométricos) apresentaram-se mais finamente dispersos na matriz nas amostras com tratamento criogênico e sem alívio de tensões. A difração de Raios-X foi realizada no Laboratório Nacional de Luz Síncroton, a luz síncroton foi essencial para detectar as variações pequenas e em escala nanométrica que ocorreram devido às inserções dos tratamentos criogênicos e de alívio de tensões. Foram verificados: i) menor fração volumétrica de austenita retida nas amostras tratadas em temperatura subzero quando comparadas às amostras tratadas em temperaturas criogênicas, indicando um comportamento cinético em C da curva de transformação; ii) diminuição da relação c/a dos parâmetros do reticulado cristalino da martensita e aumento do parâmetro a da austenita (devido à partição de carbono da martensita supersaturada em carbono para a austenita) causando estabilização da austenita com a inserção da etapa de alívio de tensões; iii) aumento no parâmetro a da austenita retida residual após revenimentos, com consequente aumento no teor de carbono da mesma, devido à partição de carbono; iv) maior fração volumétrica de carbonetos de revenido (M7C3 e M2C) nas amostras com tratamento criogênico logo após a têmpera, seguido da amostra com tratamento criogênico + alívio de tensões, seguidos da amostra somente temperada e revenida e por fim da amostra com alívio de tensões e sem tratamento criogênico. Os ensaios de potencial termo-elétrico (realizados no INSA-Lyon) foram utilizados para verificar o comportamento das amostras nas temperaturas de revenimento. Foram realizados tratamentos isotérmicos (130°C, 210°C, 350°C, 450°C e 520°C) cumulativos com tempos de 1 minuto até 130 horas. Verificou-se que: i) nos primeiros estágios do revenimento a cinética é favorecida pelo tratamento criogênico (precipitação de carbonetos \'eta\' ou \'epsilon\'); ii) o alívio de tensões atrasa os dois primeiros estágios do revenimento; iii) há maior crescimento dos carbonetos de liga nas amostras sem tratamento criogênico. O refinamento dos carbonetos secundários de revenimento foi atribuído a uma sequência de precipitações de carbonetos de revenido in situ: \'eta\' -> \'teta\' -> M7C3 e M2C. / The effects of cryogenic treatments and of stress relief treatment introduced in the thermal cycle of the cold work tool steel AISI D2 were studied. The cryogenic temperatures were varied: cryogenic (-196°C) and subzero (-80°C). It was also varied the holding times at cryogenic temperatures: 2, 3, 10, 24, 30 and 36 hours. The effect of including a stress relief heat treatment previously to the cryogenic treatment was also verified. Samples submitted to different thermal cycles were studied using metallographic characterization, X-ray diffraction and electric power measurements. The metallographic characterization used SEM (scanning electron microscopy) and SEM-FEG (SEM with field emission gun), besides OM (optical microscopy). It was not found any variation in the secondary carbides (micrometrics) precipitation. The temper secondary carbides (nanometrics) showed to be more finely dispersed in the matrix of the samples with cryogenic treatment and without stress relief. The X-ray diffractions were carried out at the Brazilian Synchrotron Light Laboratory; synchrotron light was essential to detect small and nano sized variations occurring due to the addition of the cryogenics and stress relief treatments. It was verified: i) lower austenite volumetric fraction in the samples with subzero treatment if compared to the cryogenic treated samples, an indication of a C curve kinetic behavior of the transformation; ii) the stress relief treatment produced an decrease in the c/a relationship of the martensite lattice parameters and an increase in the austenite a parameter (explained by carbon atoms partition from the supersatured martensite to the retained austenite); iii) after double tempering occurred an increase in the a parameter of the remaining austenite lattice, indicating an increase in the carbon content of the residual retained austenite, due to carbon partition; iv) higher volumetric fraction of temper carbides (M7C3 and M2C) if the samples were cryogenic treated just after quench (to room temperature), followed by the sample with cryogenic treatment + stress relief, after the sample just quenched and tempered and finally by the samples with stress relief without cryogenic treatment. Thermo-electric power measurements (carried out at INSA-Lyon) characterized the samples behavior after tempering at different temperatures. Cumulative isothermal treatments (130°C, 210°C, 350°C, 450°C e 520°C) with increasing times (from 1 minute to 130 hours) were used. It was verified that: i) the kinetic is favoured by the cryogenic treatment in the first temper stage (\'eta\' or \'epsilon\' carbide precipitation); ii) the stress relief delayed the first and second temper stage; iii) the samples without cryogenic treatment showed to have a bigger growing for the alloys carbides in the last stage of temper. The refinement of the temper secondary carbides was attributed to an in situ carbide precipitation during tempering: \'eta\' -> \'teta\' -> M7C3 e M2C.

A indústria aeronáutica tem buscado melhorias no conceito de integridade estrutural, a partir do desenvolvimento de projetos mais otimizados com a produção de aeronaves mais leves e seguras. Tais projetos garantem aeronaves operacionalmente mais viáveis e redução no consumo de combustível, beneficiando o fabricante, os operadores e a população em geral, pois aplica o conceito de aeronave verde. Estruturas aeronáuticas em operação recebem solicitações de cargas típicas de vôo, como pressurização, sustentação, que por sua vez, geram esforços dos mais variados tipos e suas combinações, como tração, compressão, fadiga, torção, flexão, flambagem, cargas aeroelásticas, vibrações e flutter, associados a ambientes críticos. O conhecimento sobre o comportamento do material estrutural perante ambientes corrosivo ou de baixa temperatura, é importante para avaliação da vida útil das aeronaves. Neste contexto, o objetivo deste trabalho foi avaliar o comportamento da liga AA2050-T84 sob ponto de vista de corrosão-fadiga e tenacidade a fratura em criogenia e, correlacionar com a microestrutura e fractografia através de ensaios mecânicos e de tenacidade a fratura em temperatura ambiente e criogênica. As condições de ensaios foram determinadas próximas a de serviço a que o material será inserido sendo, para criogenia -54 ºC e para os ensaios de propagação de trinca por fadiga em atmosfera ambiente e névoa salina com concentração de solução de 3,5% e 5% NaCl, frequência de 15Hz e razões de carga R = 0,1 e 0,5. Os resultados em criogenia mostraram que há melhora nas propriedades trativas e estabilidade na tenacidade, pois o material retém dutilidade com o decréscimo da temperatura. Os ensaios de propagação de trinca por fadiga foram executados com ΔK decrescente e os parâmetros para geração de névoa salina foram determinados experimentalmente. As curvas de crescimento de trinca e determinação do fator limite foram comparadas quanto a razão de carga e atmosfera de ensaio. Observou-se que para os ensaios de propagação de trinca por fadiga a presença da névoa salina acelera a taxa de propagação e resultam em um fator limite menor. / The aviation industry has sought improvements with the concept of structural integrity, from the development of more optimized designs with production aircraft with low weight and secure. These projects ensure an aircraft more operationally doable and reduced fuel consumption, benefiting the manufacturer, operators and the people, applying the concept of green aircraft. Aerospace structures in operation receive requests loads typical of flight, how pressurization support and lift that produce several types and combinations of requests, such as tensile, compression, fatigue, torsion, bending, buckling , aeroelastic loads, vibration and flutter associated with critical environments. Knowledge about the behavior of the structural material into corrosive environments or cryogenic temperature, it is important for evaluation to the lifetime of the aircraft. Accordingly , the aim of this study was to estimate the behavior of AA2050 - T84 alloy, about corrosion-fatigue and fracture toughness at cryogenic situations and correlate with microstructure and fractography, by mechanical tests and fracture toughness at room temperature and cryogenic. The test conditions has been determined near of the service that the material will be inserted, for cryogenic temperature -54 ºC and testing of fatigue crack propagation in air and salt spray with concentration of 3.5% and 5% NaCl, frequency 15Hz and load ratios R = 0.1 and 0.5. The cryogenic results showed that there improvement in tensile properties and stability in toughness due the restraint of ductility with decreasing temperature. Tests of fatigue crack propagation were carried out with ΔK decreasing and the parameters to obtain salt spray were determined experimentally. The crack growth curves and determination of the threshold were compared the according to load ratio and test atmosphere. In the fatigue crack propagation it was observed that presence of salt spray accelerates the rate of propagation and result in a lower threshold.

Made available in DSpace on 2017-07-21T20:42:40Z (GMT). No. of bitstreams: 1 DANIELLE C CAMILO.pdf: 6225328 bytes, checksum: 7aa2969809ed8acd7663b74ba2aa6efd (MD5) Previous issue date: 2013-07-10 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The emphasis of this work was to characterize the mechanical properties of aluminum alloy AA7050 subjected to cryogenic rolling and natural aging. Samples of aluminum alloy AA7050 were cryogenically rolled in four degrees of effective strain: = 0,5, = 0,9,= 1,1 and = 1,4. For each degree of deformation, the samples were naturally aged for 0 hours, 10 hours, 100 hours and 1000 hours. The analysis of the kinetics of natural aging indicated with 10 hours was achieved transform a fraction of 50%, which shows that the rate of transformation in this alloy was relatively high, requiring low energy of activation to occur. The calculated Avrami exponent was equal to 0,828 indicating that precipitation occurs in dislocations. By means of metallographic analysis evidenced a microstructural refinement, which was more intense for higher degrees of deformation. Mechanical properties were evaluated by Vickers microhardness measurements and tensile testing. The sample without deformation the hardness increase 30% in 10 hours of natural aging, reaching a stabilization from 1000 hours. For the deformed samples had an average increase in hardness from 80% after 1000 hours regardless of the degree of deformation. There was a competition between the static recovery and precipitation in the early hours of natural aging for samples more deformed (= 1,1 and = 1,4). The results also indicate that for higher degrees of deformation (= 1,1 and = 1,4) the natural aging did not affect the mechanical properties under tension significantly. On the other hand, for lower degrees of reduction, increased mechanical strength was more significant. For the initial sample, the yield strength increased 153% with 1000 hours of natural aging. A sample of ε = 0,5 and 1000 hours presented a 323% yield strength greater than as-quench sample. Furthermore, regarding all samples deformed, this condition had the highest total elongation (15%), representing an optimal combination of deformation and thermal treatment. The images of electron microscopy of the fracture surfaces revealed the occurrence of ductile fracture primarily, with plenty of dimples, for all conditions. Thermal analysis (DSC) results confirmed the high volume fraction of GP zones and η’ phase, formed in natural aging. Moreover, the deformation changed the form of DSC curves, especially at a temperature of precipitation of η' due to the increase of sites for nucleation. The EDS microanalysis, both particles in the fracture surface when the dissolved material for extraction of precipitates indicated the elements forming the phases MgZn2, Al2CuMg, Al2Cu, Al2Zn3Mg3, Mg2Si, and Al7Cu2Fe AlZnMgCu. The x-ray diffraction indicate a crystallographic texture for lower degree of reduction in the direction [110], which was associated with bimodal distribution of grain size. / A ênfase do presente trabalho foi caracterizar as propriedades mecânicas da liga de alumínio AA7050 submetida à laminação criogênica e envelhecimento natural. Amostras da liga de alumínio AA7050 foram laminadas criogenicamente em quatro graus de deformação equivalente: = 0,5; = 0,9; = 1,1 e = 1,4. Para cada grau de deformação, as amostras foram envelhecidas naturalmente por 0 hora, 10 horas, 100 horas e 1000 horas. A análise da cinética de envelhecimento natural indicou que com 10 horas de envelhecimento foi atingida uma fração transformada de 50%, o que mostra que a velocidade de transformação nessa liga é relativamente alta, exigindo baixa energia de ativação para ocorrer. O expoente de Avrami calculado foi igual a 0,828, indicando que a precipitação ocorre em discordâncias. Por meio da análise metalográfica constatou-se um refino microestrutural, o qual foi mais intenso para maiores graus de deformação. As propriedades mecânicas foram avaliadas por meio de medidas de dureza Vickers por micro-impressão e ensaio de tração uniaxial. A amostra sem deformação aumentou sua dureza em 30% nas primeiras 10 horas de envelhecimento natural, atingindo uma estabilização a partir de 100 horas. Já as amostras deformadas tiveram um aumento médio de 80% na dureza após 1000 horas, independentemente do grau de deformação. Foi observada uma competição entre a recuperação estática e a precipitação nas primeiras horas de envelhecimento natural para as amostras mais deformadas ( = 1,1 e = 1,4). Os resultados também indicam que para maiores graus de deformação ( = 1,1 e = 1,4) o envelhecimento natural não afetou as propriedades mecânicas sob tração significativamente. Por outro lado, para menores graus de redução, o aumento da resistência mecânica foi mais significativo. Para a amostra inicial, o limite de escoamento aumentou em 153% com 1000 horas de envelhecimento natural. A amostra com ε = 0,5 e 1000 horas de envelhecimento apresentou um limite de escoamento 323% maior do que a amostra inicial, solubilizada. Além disso, em relação à todas as amostras deformadas, esta condição apresentou o maior alongamento total (15%), representando uma combinação ótima de deformação e tratamento térmico. As imagens de microscopia eletrônica das superfícies de fratura revelaram a ocorrência de fratura essencialmente dúctil, com abundância de “dimples”, para todas as condições. Os resultados de análise térmica (DSC) confirmaram a elevada fração volumétrica de zonas GP e da fase η’, formadas no envelhecimento natural. Além disso, a deformação alterou a forma das curvas de DSC, principalmente na temperatura de precipitação de η’, devido ao aumento de sítios para nucleação. As microanálises por EDS, tanto das partículas na superfície de fratura quando no material dissolvido para extração de precipitados, indicaram os elementos formadores das fases MgZn2, Al2CuMg, Al2Cu, Al2Zn3Mg3, Mg2Si, Al7Cu2Fe e AlZnMgCu. As difrações de raios x indicaram textura cristalográfica para o menor grau de redução, na direção [110], o que foi associado com a distribuição bimodal de tamanho de grão.

Submitted by Angela Maria de Oliveira (amolivei@uepg.br) on 2018-04-26T13:22:22Z No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Marcel Tadshi Izumi.pdf: 4222698 bytes, checksum: e7c749993223b983b4e37d54985610de (MD5) / Made available in DSpace on 2018-04-26T13:22:22Z (GMT). No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Marcel Tadshi Izumi.pdf: 4222698 bytes, checksum: e7c749993223b983b4e37d54985610de (MD5) Previous issue date: 2018-02-22 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Três metais CFC comercialmente puros (alumínio, cobre e prata) foram deformados por ensaios de tração uniaxial e caracterizados por difração de raios X in situ, utilizando uma fonte síncrotron, em temperatura ambiente (293K) e criogênica (77K). A supressão parcial da recuperação dinâmica decorrente do processamento criogênico permite melhorias nas propriedades mecânicas, tais como ductilidade e resistência. Esta supressão resulta em um aumento na densidade de defeitos internos dos metais durante a deformação, promovendo um refino microestrutural e aumento da microdeformação. O refino microestrutural é manifestado pela evolução de dimples na superfície de fratura e pela redução do tamanho médio de cristalitos. Todos os metais apresentaram maior resistência mecânica em temperaturas criogênicas, entretanto somente o cobre e a prata apresentaram aumento de ductilidade. Esse comportamento é atribuído à menor energia de defeito de empilhamento destes metais em comparação com o alumínio. / Three FCC commercially pure metals (aluminum, copper and silver) were deformed by uniaxial tensile tests and were characterized by in situ X-ray diffraction, using a synchrotron source, at room (293K) and cryogenic (77K) temperatures. The partial suppression of dynamic recovery due to cryogenic processing allows an improvement in mechanical properties, such as ductility and strength. This suppression results in an increase in the internal defects density of metals during the strain, promoting microstructural refining and increase of microstrain. The microstructural refinement is manifested by dimples evolution on the fracture surface and reduction of average crystallite size. All metals present higher mechanical strength at cryogenic temperature, nevertheless the ductility only was increased in copper and silver. This behavior is attributed to lower stacking fault energy of these metals in comparison with aluminum.

Foram estudados os efeitos da introdução de etapas de tratamento criogênico e do alívio de tensões no ciclo térmico do aço ferramenta para trabalho a frio AISI D2. Variaram-se as temperaturas de tratamento criogênico, sendo elas principalmente: criogênica (-196°C) e subzero (-80°C). Foram variados os tempos de permanência às temperaturas criogênicas: 2, 3, 10, 24 e 30 e 36 horas. Verificou-se o efeito da adição da etapa (130°C/90 minutos) de alívio de tensões previamente ao tratamento criogênico. As amostras com diferentes ciclos térmicos foram submetidas à caracterização metalográfica, difração de raios-X e ensaios de potencial termo-elétrico. Na caracterização metalográfica as amostras foram analisadas por MEV (microscopia eletrônica de varredura) e MEV-FEG (MEV com canhão com emissão por efeito de campo). Os carbonetos secundários (micrométricos) não apresentaram variação. Os carbonetos secundários de revenido (nanométricos) apresentaram-se mais finamente dispersos na matriz nas amostras com tratamento criogênico e sem alívio de tensões. A difração de Raios-X foi realizada no Laboratório Nacional de Luz Síncroton, a luz síncroton foi essencial para detectar as variações pequenas e em escala nanométrica que ocorreram devido às inserções dos tratamentos criogênicos e de alívio de tensões. Foram verificados: i) menor fração volumétrica de austenita retida nas amostras tratadas em temperatura subzero quando comparadas às amostras tratadas em temperaturas criogênicas, indicando um comportamento cinético em C da curva de transformação; ii) diminuição da relação c/a dos parâmetros do reticulado cristalino da martensita e aumento do parâmetro a da austenita (devido à partição de carbono da martensita supersaturada em carbono para a austenita) causando estabilização da austenita com a inserção da etapa de alívio de tensões; iii) aumento no parâmetro a da austenita retida residual após revenimentos, com consequente aumento no teor de carbono da mesma, devido à partição de carbono; iv) maior fração volumétrica de carbonetos de revenido (M7C3 e M2C) nas amostras com tratamento criogênico logo após a têmpera, seguido da amostra com tratamento criogênico + alívio de tensões, seguidos da amostra somente temperada e revenida e por fim da amostra com alívio de tensões e sem tratamento criogênico. Os ensaios de potencial termo-elétrico (realizados no INSA-Lyon) foram utilizados para verificar o comportamento das amostras nas temperaturas de revenimento. Foram realizados tratamentos isotérmicos (130°C, 210°C, 350°C, 450°C e 520°C) cumulativos com tempos de 1 minuto até 130 horas. Verificou-se que: i) nos primeiros estágios do revenimento a cinética é favorecida pelo tratamento criogênico (precipitação de carbonetos \'eta\' ou \'epsilon\'); ii) o alívio de tensões atrasa os dois primeiros estágios do revenimento; iii) há maior crescimento dos carbonetos de liga nas amostras sem tratamento criogênico. O refinamento dos carbonetos secundários de revenimento foi atribuído a uma sequência de precipitações de carbonetos de revenido in situ: \'eta\' -> \'teta\' -> M7C3 e M2C. / The effects of cryogenic treatments and of stress relief treatment introduced in the thermal cycle of the cold work tool steel AISI D2 were studied. The cryogenic temperatures were varied: cryogenic (-196°C) and subzero (-80°C). It was also varied the holding times at cryogenic temperatures: 2, 3, 10, 24, 30 and 36 hours. The effect of including a stress relief heat treatment previously to the cryogenic treatment was also verified. Samples submitted to different thermal cycles were studied using metallographic characterization, X-ray diffraction and electric power measurements. The metallographic characterization used SEM (scanning electron microscopy) and SEM-FEG (SEM with field emission gun), besides OM (optical microscopy). It was not found any variation in the secondary carbides (micrometrics) precipitation. The temper secondary carbides (nanometrics) showed to be more finely dispersed in the matrix of the samples with cryogenic treatment and without stress relief. The X-ray diffractions were carried out at the Brazilian Synchrotron Light Laboratory; synchrotron light was essential to detect small and nano sized variations occurring due to the addition of the cryogenics and stress relief treatments. It was verified: i) lower austenite volumetric fraction in the samples with subzero treatment if compared to the cryogenic treated samples, an indication of a C curve kinetic behavior of the transformation; ii) the stress relief treatment produced an decrease in the c/a relationship of the martensite lattice parameters and an increase in the austenite a parameter (explained by carbon atoms partition from the supersatured martensite to the retained austenite); iii) after double tempering occurred an increase in the a parameter of the remaining austenite lattice, indicating an increase in the carbon content of the residual retained austenite, due to carbon partition; iv) higher volumetric fraction of temper carbides (M7C3 and M2C) if the samples were cryogenic treated just after quench (to room temperature), followed by the sample with cryogenic treatment + stress relief, after the sample just quenched and tempered and finally by the samples with stress relief without cryogenic treatment. Thermo-electric power measurements (carried out at INSA-Lyon) characterized the samples behavior after tempering at different temperatures. Cumulative isothermal treatments (130°C, 210°C, 350°C, 450°C e 520°C) with increasing times (from 1 minute to 130 hours) were used. It was verified that: i) the kinetic is favoured by the cryogenic treatment in the first temper stage (\'eta\' or \'epsilon\' carbide precipitation); ii) the stress relief delayed the first and second temper stage; iii) the samples without cryogenic treatment showed to have a bigger growing for the alloys carbides in the last stage of temper. The refinement of the temper secondary carbides was attributed to an in situ carbide precipitation during tempering: \'eta\' -> \'teta\' -> M7C3 e M2C.

Les onduleurs sont des systèmes magnétiques créant un champ périodique permanent. Les sources de rayonnement synchrotron dites de « troisième génération » produisent du rayonnement accordable de haute intensité lorsque les particules relativistes sont accélérées dans ce champ magnétique. A une énergie donnée des électrons, l’émission est rayonnée à d’autant plus courte longueur d’onde que le champ magnétique créé est important et que la période est petite. Une première solution consiste à mettre les aimants sous vide. Le sujet de thèse consiste à améliorer les performances magnétiques de ce type d’onduleur de 30% en refroidissant le système magnétique. L’utilisation de la nuance d’aimant Pr2Fe14B permet de refroidir les aimants à la température de l’azote liquide ce qui simplifie beaucoup le système de refroidissement.Dans le chapitre I les caractéristiques magnétiques des onduleurs sont décrites, les différents types d’onduleurs sont présentés et l’état de l’art des onduleurs cryogénique est effectué. Dans le chapitre II plusieurs échantillons d’aimants permanents NdFeB et PrFeB de différents fournisseurs sont caractérisés. Deux prototypes d’onduleurs cryogéniques de 4 périodes, un avec la nuance NdFeB et l’autre avec la nuance PrFeB sont étudiés et réalisés afin de comparer et d’ajuster s’il y a besoin le modèle de simulation du système magnétique. La conception d’un onduleur cryogénique de 2 m utilisant la nuance d’aimant PrFeB en partant d’un onduleur sous vide de 2 m utilisant la nuance d’aimant SmCo est effectuée. La période de l’onduleur est optimisée et les forces magnétiques associées sont calculées. Dans le chapitre III la conception du châssis et des différentes pièces mécaniques est présentée. L’étude thermique qui inclut les apports de chaleur des différentes pièces et les calculs d’apport de chaleur du faisceau d’électrons pour tous les modes de remplissage du faisceau d’électrons et à différentes position dans l’anneau de stockage sont effectués. Le système de refroidissement est optimisé et la conception du circuit de refroidissement sur les poutres d’aimants est présentée. Dans le chapitre IV les différentes méthodes utilisées pour les mesures magnétiques sont décrites, les bancs de mesures magnétiques utilisés à SOLEIL sont présentés. La conception du banc de mesure magnétique intégré dans la chambre à vide afin de mesurer l’onduleur cryogénique à des températures cryogéniques est effectuée. Dans le chapitre V les différentes étapes de la construction de onduleur sous vide U20 (assemblage magnétique, corrections magnétique et « shimming », « magic finger », assemblage mécanique de la chambre à vide, l’installation et la caractérisation avec le faisceau) sont effectuées. Dans le chapitre VI les différentes étapes de la construction de l’onduleur cryogénique, le montage, l’ajustement et la calibration du banc de mesures à froid dans la chambre à vide de l’onduleur sont présentées. Les résultats de mesures magnétiques à froid sont comparés avec les mesures magnétiques de l’onduleur à température ambiante. La caractérisation de l’onduleur avec le faisceau d’électrons est effectuée et les perspectives d’amélioration de cet onduleur cryogénique sont proposées. / Undulators are magnetic systems which produce periodic magnetic field. Synchrotron radiation sources called third generation produce high intensity radiation when relativistic particles are accelerated in this magnetic field. The radiation is emitted at shorter wave length for high magnetic field and small period undulators. A first solution consists to integrate the magnetic system in a big vacuum chamber. The subject of the thesis is to improve the magnetic performance of an in vacuum undulator of 30 % by cooling down the magnetic system at cryogenic temperature. Using Pr2Fe14B permanent magnet allows cooling down directly to the liquid nitrogen temperature which simplified the cooling system.IN chapter I the magnetic characteristics of undulators are described, different types of undulators are presented and the state of the art of cryogenic undulator is given. In chapter II permanent magnet samples Pr2Fe14B Nd2Fe14B from different companies are characterised. Two four period prototypes, one with Pr2Fe14B and one with Nd2Fe14B have been assembled and measured to compare with the magnetic system simulation. The magnetic design of a full scale 2 m Pr2Fe14B undulator has been performed. The period of the undulator is optimised and the magnetic forces calculated. In chapter III the mechanical design of the carriage and different mechanical parts is presented. Thermal studies which include the dissipated power from different mechanical parts and from the electrons beam for all filling modes and different positions in SOLEIL storage ring. The cooling system is optimised and the design of the cooled girders is presented. In chapter IV the different magnetic measurements methods are described and the magnetic measurement bench used at SOLEIL presented. The design of magnetic bench installed in the vacuum chamber and dedicated to the magnetic measurement at cryogenic temperature is presented. In chapter V the different steps for the construction of an in-vacuum undulator (magnetic assembly, shimming, magic finger, mechanical assembly of the vacuum chamber, installation and commissioning with the electrons beam) are presented. In chapter VI the different steps of the constructing of a cryogenic undulator, the assembly and the ajustement of cryogenic temperature magnetic bench are described. The magnetic measurements of the undulator at cryogenic and room temperature are compared. The commissioning of the undulator with the electrons beam is presented and the perspectives to improve this cryogenic undulator are proposed.

As Si-manufacturing compatible SiGe HBTs are making rapid in-roads into RF through mm-wave circuit applications, with performance levels steadily marching upward, the use of these devices under extreme environment conditions are being studied extensively. In this work, test structures of SiGe HBTs were designed and put into extremely low temperatures, and a new negative differential resistance effect and a novel collector current kink effect are investigated in the cryogenically-operated SiGe HBTs. Theory based on an enhanced positive feedback mechanism associated with heterojunction barrier effect at deep cryogenic temperatures is proposed. The accumulated charge induced by the barrier effect acts at low temperatures to enhance the total collector current, indirectly producing both phenomena. This theory is confirmed using calibrated 2-D DESSIS simulations over temperature. These unique cryogenic effects also have significant impact on the ac performance of SiGe HBTs operating at high-injection. Technology evolution plays an important role in determining the magnitude of the observed phenomena, and the scaling implications are addressed. Circuit implication is discussed.

A cryogenic (325-80 K) ion mobility-mass spectrometer was designed and constructed in order to improve the analytical figures-of-merit for the chemical analysis of small mass analytes using ion mobility-mass spectrometry. The instrument incorporates an electron ionization source, a quadrupole mass spectrometer, a uniform field drift cell spectrometer encased in a cryogenic envelope, and an orthogonal geometry time-of-flight mass spectrometer. The analytical benefits of low temperature ion mobility are discussed in terms of enhanced separation ability, ion selectivity and sensitivity. The distinction between resolving power and resolution for ion mobility is also discussed. Detailed experimental designs and rationales are provided for each instrument component. Tuning and calibration data and methods are also provided for the technique. Proof-of-concept experiments for an array of analytes including rare gases (argon, krypton, xenon), hydrocarbons (acetone, ethylene glycol, methanol), and halides (carbon tetrachloride) are provided in order to demonstrate the advantages and limitations of the instrument for obtaining analytically useful information. Trendline partitioning of small analyte ions based on chemical composition is demonstrated as a novel chemical analysis method. The utility of mobility-mass analysis for mass selected ions is also demonstrated, particularly for probing the ion chemistry which occurs in the drift tube for small mass ions. As a final demonstration of the separation abilities of the instrument, the electronic states of chromium and titanium (ground and excited) are separated with low temperature. The transition metal electronic state separations demonstrated here are at the highest resolution ever obtained for ion mobility methods. The electronic conformational mass isomers of methanol (conventional and distonic) are also partially separated at low temperature. Various drift gases (helium, neon, and argon) are explored for the methanol system in order to probe stronger ion-neutral interaction potentials and effectuate higher resolution separations of the two isomeric ions. Finally, two versatile ion source designs and a method for axially focusing ions at low pressure (1-10 torr) using electrostatic fields is presented along with some preliminary work on the ion sources.

This work represents several years' research into the field of radiation hardening by design. The unique characteristics of a SiGe HBT, described in Chapter 1, make it ideally suitable for use in extreme environment applications. Chapter 2 describes the total ionizing dose effects experienced by a SiGe HBT, particularly those experienced on an Earth-orbital or lunar-surface mission. In addition, the effects of total dose are evaluated on passive devices. As opposed to the TID-hardness of SiGe transistors, a clear vulnerability to single-event effects does exist. This field is divided into three chapters. First, the very nature of single-event transients present in SiGe HBTs is explored in Chapter 3 using a heavy-ion microbeam with both bulk and SOI platforms [31]. Then, in Chapter 4, a new device-level SEU-hardening technique is presented along with circuit-design techniques necessarily for its implementation. In Chapter 5, the circuit-level radiation-hardening techniques necessarily to mitigate the effects shown in Chapter 3 are developed and tested [32]. Finally, in Chapter 6, the performance of the SiGe HBT in a cryogenic testing environment is characterized to understand how the widely-varying temperatures of outer space may affect device performance. Ultimately, the built-in performance, TID-tolerance, and now-developing SEU-hardness of the SiGe HBT make a compelling case for extreme environment electronics. The low-cost, high-yield, and maturity of Si manufacturing combine with modern bandgap engineering and modern CMOS to produce a high-quality, high-performance BiCMOS platform suitable for space-borne systems.