Made available in DSpace on 2014-10-09T12:55:34Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:54Z (GMT). No. of bitstreams: 0 / As propriedades mecânicas de ferramentas confeccionadas com aços rápidos estão intimamente ligadas às características dos carbonetos dispersos na microestrutura desses materiais. Neste trabalho foi estudado o efeito do ciclo comercial de tratamento térmico de austenitização e revenimento em amostras do aço AISI/SAE M2 produzidas por metalurgia convencional, metalurgia do pó e conformação por spray. Para a realização deste estudo foram desenvolvidos métodos para a extração seletiva dos carbonetos dos tipos MC e M6C, onde M representa: vanádio, cromo, ferro, molibdênio e tungstênio, utilizando técnicas de dissolução química e eletrolítica. Estes métodos permitiram a quantificação por diferença de massa dos carbonetos do tipo M6C e MC. A extração seletiva revelou a existência de um carboneto do tipo MC com estequiometria ainda não reportada na literatura. Os parâmetros cristalográficos deste carboneto foram determinados utilizando-se o método de Rietveld. A estrutura cristalina foi refinada a partir de dados obtidos por difração de raios X, utilizando energias próximas da borda de absorção dos elementos metálicos do carboneto, através do uso de radiação de luz síncrotron. Os resultados obtidos pelo método de Rietveld permitiram determinar o grupo espacial F m -3 m para este carboneto, e que o parâmetro de rede e a estequiometria estão relacionados com a microestrutura e o teor de carbono do material antes do ciclo de tratamento térmico, porém indicando uma forte convergência para uma estequiometria comum. O conjunto dos resultados obtidos mostrou que o ciclo de tratamento térmico comercial, utilizado neste trabalho, induz ao aumento significativo da fração de carbonetos, quando comparado com o ciclo de tratamento térmico convencional descrito na literatura. A fração de carbonetos do tipo MC tem aumento mais significativo, que a do carboneto do tipo M6C, como conseqüência das alterações na estequiometria do carboneto do tipo MC. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Orientadores: Theo Guenter Kieckbusch, Valdecir Luccas / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica / Made available in DSpace on 2018-08-10T18:45:44Z (GMT). No. of bitstreams: 1 Quast_LedaBattestin_D.pdf: 1972832 bytes, checksum: a34ffd60e85d88858ba49961e507cd34 (MD5) Previous issue date: 2008 / Resumo: A influência da incorporação de gorduras alternativas low e zero trans na cristalização da manteiga de cacau foi avaliada através da caracterização física de misturas binárias de manteiga de cacau com gordura de cupuaçu, gordura CBR low trans e gordura CBS, nas proporções de 5, 10, 15, 20, 25 e 30 %. O processo de pré-cristalização (temperagem) foi realizado em um reator encamisado de escala piloto dotado de um agitador e com capacidade para 700 mL. As amostras foram caracterizadas através da curva de sólidos, tensão de ruptura (snap test), calorimetria diferencial de varredura e difração de raios-X. A melhor condição de pré-cristalização da manteiga de cacau pura (taxa de resfriamento de 1,8 ºC/min, cristalização à 24 ºC por um tempo de 8 minutos) também foi utilizada nos ensaios com as misturas, com exceção das amostras com 20, 25 e 30 % de CBR e CBS que foram pré-cristalizadas a 23 ºC por 10 minutos. A manteiga de cacau apresentou um perfil de fusão de gordura na boca, DS(25ºC-35ºC), de 59,2 %, que sofreu apenas pequenas alterações com a adição de até 20 % de cupuaçu e até 30 % de CBR. A curva do conteúdo de sólidos sugere a formação de um eutético entre a manteiga de cacau e a gordura CBS. A tensão de ruptura para a manteiga de cacau foi de 2,48 kgf/cm2 e a adição das gorduras tende a diminuí-la, sendo que com 30 % de cupuaçu e 30 % de CBR esse valor foi 1,90 kgf/cm2 e 1,81 kgf/cm2, respectivamente. Para a amostra com 30 % de CBS a tensão de ruptura baixou para 0,39 kgf/cm2. Observou-se uma diminuição do ponto de fusão das misturas quando comparadas à da manteiga de cacau pura. A difração de raios-X identificou a forma cristalina b como predominante para a manteiga de cacau e para a gordura de cupuaçu enquanto que para as gorduras CBR e CBS a principal forma cristalina é a b'. A incorporação de apenas 10 % das gorduras CBR e CBS à manteiga de cacau promoveu interferências na estruturação cristalina das amostras. O estudo indicou ser possível adicionar até 30 % de gordura de cupuaçu ou CBR e até 10 % de gordura CBS sem alterar de forma sensível os atributos físicos da manteiga de cacau / Abstract: Physical properties of pre-crystallized cocoa butter with the addition of alternative low and zero trans fats were studied. Binary mixtures of cocoa butter were conducted using cupuassu fat, CBR low trans and CBS at 5, 10, 15, 20, 25 and 30 % (w/w) levels. Pre-crystallization was carried out using a lab scale jacket vessel (700 mL) whit stirring system. Samples were evaluated by means of solid fat content, snap test, differential scanning calorimetry and X-Ray diffraction. The better condition for plain cocoa butter pre-crystallization was determined as follows: cooling rate (1,8 ºC/min), crystallization time (8 minutes), crystallization temperature (24 ºC). These conditions were also used for mixtures precrystallization (tempering). Mixtures with 20, 25 and 30 % of CBR and CBS were pre-crystallized at 23 ºC for 10 minutes. Regarding to solid fat content, cocoa butter fusion profile DS(25ºC-35ºC) was 59,2 %. Similar values were obtained for mixtures with up to 30 % of cupuassu and up to 30 % of CBR fats. Mixtures with CBS fat indicated eutectic effect. Snap value for crystallized cocoa butter was 2,48 kgf/cm2. The snap values decreased with the increase of the alternative fats proportion. Mixtures containing cupuassu fat or CBR have similar trend regarding to snap values profile. For mixtures with 30 % of cupuassu and CBR the snap values were 1,90 kgf/cm2 and 1,81 kgf/cm2, respectively. CBS 30% have the lowest snap value (0,39 kgf/cm2). Similar trend was observed regarding to melting point. Alternative fats incorporation decreased the melting point of the mixtures. Regarding to X-Ray diffraction, cocoa butter and cupuassu fat patterns results showed the formation of ß phase. For CBS and CBR patterns, there are evidence of ß¿ phase formation. The addition of 10 % CBR and CBS fat to cocoa butter was detected by X-ray diffraction patterns. The addition of up to 30 % cupuassu or CBR fat, and up to 10 % CBS butter showed no significant differences of physical properties when compared to cocoa butter / Doutorado / Engenharia de Processos / Doutor em Engenharia Química

L’objectif de ce travail est d’optimiser la résistance au revenu d’un acier martensitique à 0,6% de carbone, faiblement allié en Cr, V, et Si/Al. Une série d’alliage modèle ternaire de haute pureté (Fe-C-X, X=Cr, V, Si, Al) a été élaborée à l’EMSE par fusion en creuset froid.. L’étude du comportement des alliages a été réalisée au moyen d’une caractérisation fine de la précipitation (Diffraction RX, MEB-FEG, MET) complétée par des mesures dilatométriques. Le comportement des alliages modèles a été comparé à celui de l’alliage industriel. Le vanadium est responsable de deux effets : (i) les carbures de vanadium bloquent la croissance des grains au cours de l’austénitisation ; (ii) le vanadium dissous permet la précipitation d’une cémentite (V,Cr,Fe)3C à l’origine d’un pic de durcissement secondaire pour un revenu vers 550°C. Le silicium a un effet particulier : il stabilise la matrice martensitique et retarde la précipitation de la cémentite vers des températures de revenu plus élevées, augmentant ainsi la résistance au revenu. Cependant, le silicium se révèle nocif pour le procédé industriel de mise en forme utilisé. Deux nouveaux alliages ont alors été élaborés pour chercher un élément de substitution à l’aluminium : un alliage ou le silicium est remplacé par l’aluminium, et un alliage ou le silicium est absent. L’aluminium reste neutre dans l’alliage mais l’étude de ces deux nuances a permis de mettre en évidence la possibilité d’utiliser une nuance ne contenant pas de silicium mais présentant une résistance au revenu comparable a celle de la nuance industrielle, du fait de la présence conjointe du chrome et du vanadium. / The purpose of this work is to optimise the strength of a tempered martensitic medium C steel, containing low-level of Cr, V and Si/Al. A series of high purity "model" ternary alloys (Fe-C–X, X=Cr, V, Si, Al) was prepared (EMSE) by the cold crucible method. The initial structures of quenched alloys were optimised through appropriate austenitizing conditions. Analysis of alloys behaviour on tempering was performed through carbide precipitation characterisation (X-ray diffraction, SEM and TEM), completed by hardness and dilatometric measurements. The behaviour of "model" alloys was compared to that of the industrial material.Vanadium addition is responsible for two effects: (i) vanadium carbides lock the grain growth during the austenitizing; (ii) dissolved vanadium promotes the precipitation of (V,Cr)3C, that is at the origin of a secondary hardening peak near 550°C. Silicon addition has an interesting effect, as it stabilises the martensitic matrix and increases the temperature of cementite precipitation. Therefore, a high value of hardness is conserved up to high tempering temperatures.Unfortunately, because of some noxious properties, the industrial process in concern excludes the presence of Si. That’s why two new model alloys have been prepared and tested, in which the silicon addition (i) was absent, or (ii) replaced by Al.Aluminium has been shown to be "neuter" vs tempering behaviour. Moreover, the interesting effect of secondary hardening (550°C) has been observed in both Si-free steels, showing that alloying with only Cr and V can be enough to get the expected behaviour of the studied steel.

The master thesis deals with the influence of heat treatment and storage time on microstructure and mechanical properties of 26MnB5 steel, which is used in the production of tubular components in the quenched and tempered state. The objective was to increase the plasticity of the steel by the definition of new process parameters of the induction heat treatment line. New tempering diagrams of 26MnB5 steel for two various speeds of the heat treatment line were established and used to determine new tempering temperature and speed of the heat treatment line. Observation of the influence of storage time on mechanical properties of the steel did not reveal that it is liable to ageing.

This thesis deals with the properties of ledeburitic chrome-vanadium tool steel after heat treatment. Theoretical part contains charakterization of ledeburitic steels, the posibility of manufacturing and heat treatment. There are also briefly describes the principles of the test methods, which were used. The practical part is focused on describing the results of 12 sample groups, with different heat treatment. The results are compared in the final discussion.

La majorité des produits verriers du marché sont issus d’une opération de mise en forme à hautes températures, suivie d’une phase de refroidissement contrôlé afin d’éliminer (verre recuit) ou générer (verre trempé) des contraintes résiduelles. Le comportement mécanique du verre étant fortement thermo-dépendant, le contrôle des températures est un élément déterminant pour le succès du procédé de fabrication. Lors de la simulation numérique, pour ce milieu semi-transparent, les échanges thermiques par conduction et par rayonnement sont à considérer. La résolution de l’ETR (Equation de Transfert Radiatif) est menée dans cette thèse par le biais de la « Méthode P1 » et le « Back Ray Tracing » (BRT). Les deux codes développés ont été validés par l’étude comparative avec les données en températures et en contraintes résiduelles issues de la littérature sur le refroidissement dans l’épaisseur du verre soumis à des conditions variées en convection naturelle et forcée. Une expérimentation qui consiste à refroidir un disque de verre sur un support métallique a été développée dans le but de comparer les températures et contraintes générées par l’expérimentation et par la modélisation issue du couplage thermomécanique avec les deux codes P1 et BRT. De manière plus originale, la méthode BRT a été étendue à des géométries de révolution. Une première approche a consisté à étudier le fluage d’une goutte de verre et à analyser l’influence du choix du modèle de résolution de l’ETR sur les températures et les géométries au cours de la mise en forme. / Most of glass products on the market come from a high-temperature forming operation, followed by a controlled cooling phase to remove (annealed glass) or generate (tempered glass) residual stresses. Since the mechanical behaviour of the glass is highly thermo-dependent, temperature control is a determining factor for the success of the manufacturing process. During numerical simulations, for this semi-transparent medium, heat exchanges by conduction and radiation have to be considered. In this work, the resolution of the ETR (radiative transfer Equation) is carried out using the "P1 method" and the "Back Ray tracing" (BRT). The two developed codes were validated by the comparative study with the temperature and residual stresses data from the literature on cooling in the thickness of the glass subject to various conditions in natural and forced convection. An experimentation which consists in cooling a glass disk on a metal support was developed in order to compare the temperatures and stresses generated by the testing and by the modelling resulting from the thermomechanical coupling with the two codes P1 and BRT. In a more original way, the BRT method was extended to revolving geometries. A first approach was to study the creep of a glass gob and to analyze the influence of the choice of the ETR's resolution model on the temperatures and geometries during the forming.

No description available.

The increasing demands for lightweight designs with high strength call for improved manufacturing processes regarding heat treatment of steel. The manufacturing process has considerable potential to improve the mechanical performance and to obtain more reliable results with less variation. The goal of this thesis is to establish new knowledge regarding improved manufacturing processes in industrial heat treatment applications. Three research questions with associated hypotheses are formulated. Process experiments, evaluation of the mechanical performance, and modelling of the fatigue behaviour assist in answering the questions. The gas quenching procedure following low-pressure carburising differs from the conventional procedure of gas carburising and oil quenching. It is shown that the introduction of a holding time during the low-temperature part of the quench has a positive effect on mechanical properties, with some 20 percent increase in fatigue strength. This is attributed to increased compressive surface residual stress and stabilisation of austenite. Tempering is a common manufacturing process step following hardening in order to increase the toughness of the steel. However, the research shows that the higher hardness from eliminating tempering from the manufacturing process is beneficial for contact fatigue resistance. The untempered steel showed not only less contact fatigue damage but also a different contact fatigue mechanism. Straightening of elongated components is made after heat treatment in order to compensate for distortions. The research shows that straightening of induction hardened shafts may lead to lowering of the fatigue strength of up to 20 percent. A fracture mechanics based model is developed to estimate the effects of straightening on fatigue strength. / Ökande krav på höghållfasta lättviktskonstruktioner kräver förbättrade tillverkningsprocesser för värmebehandling av stål. Det finns stor potential att förbättra mekanisk prestanda och att erhålla mer tillförlitliga resultat med mindre variation genom att förbättra tillverkningsprocessen. Målet med denna avhandling är att etablera ny kunskap kring tillverkningsprocesser inom industriella värmebehandlingsapplikationer. Tre forskningsfrågor med tillhörande hypoteser formuleras. Processexperiment, utvärdering av mekanisk hållfasthet och modellering av utmattningsbeteende bygger upp besvarandet av frågorna. Gaskylning som följer lågtrycksuppkolning skiljer sig från det konventionella förfarandet med gasuppkolning och släckning i olja. Resultaten visar att en hålltid i den nedre delen av kylningsförloppet har positiv inverkan på utmattningshållfastheten. Orsaken till förbättringen hänförs till ökade tryckrestspänningar samt stabilisering av austenit. Anlöpning är en vanlig tillverkningsprocess som efterföljer härdning för att öka stålets seghet. Forskningen visar däremot att den högre hårdheten för oanlöpt stål är fördelaktig för motstånd mot kontaktutmattning. Oanlöpt stål visade mindre mängd kontaktutmattningsskador och även en annan skademekanism. Riktning av långa komponenter görs efter värmebehandling för att kompensera för de formförändringar som uppstår. Forskningen visar att riktning av induktionshärdade axlar kan leda till sänkning av utmattningshållfastheten med upp till 20 procent. En brottmekanisk modell som uppskattar effekten av riktning på utmattningshållfasthet presenteras. / <p>QC 20150410</p>

The capacity of soft annealing of low alloyed tubes at Ovako’s continuous annealing furnaces have been evaluated by comparing how it is done today with information from published and internal articles on the subject. It was found that it is possible to reduce the cycle time by 30 % for one furnace, 55 % for one furnace and 72 % for two furnaces. Two separate fullscale tests were made to assess whether the faster soft annealing procedure was feasible. The tests were performed without any reconstruction of the furnace and were made by continuously vary the speed of the batch inside thefurnace. The temperature in the batch was measured and compared with results from computer simulations of the heating/cooling sequences. The computer simulations were performed in COMSOL. The soft annealing was evaluated according to the SEP-520 standard ,which means evaluating the microstructure and hardness. The results show that the faster heat treatment could yield lower grades than today but still meet it’s requirements. In order to achieve this increase  a reconstruction of the furnaces is needed and the reconstruction is  briefly treated in the report. Ideas to further increase the speed of the soft annealing procedure are also presented.

Cette thèse se décompose en deux parties. Dans un premier temps nous nous intéressons à la sélection bayésienne de variables dans un modèle probit mixte.L'objectif est de développer une méthode pour sélectionner quelques variables pertinentes parmi plusieurs dizaines de milliers tout en prenant en compte le design d'une étude, et en particulier le fait que plusieurs jeux de données soient fusionnés. Le modèle de régression probit mixte utilisé fait partie d'un modèle bayésien hiérarchique plus large et le jeu de données est considéré comme un effet aléatoire. Cette méthode est une extension de la méthode de Lee et al. (2003). La première étape consiste à spécifier le modèle ainsi que les distributions a priori, avec notamment l'utilisation de l'a priori conventionnel de Zellner (g-prior) pour le vecteur des coefficients associé aux effets fixes (Zellner, 1986). Dans une seconde étape, nous utilisons un algorithme Metropolis-within-Gibbs couplé à la grouping (ou blocking) technique de Liu (1994) afin de surmonter certaines difficultés d'échantillonnage. Ce choix a des avantages théoriques et computationnels. La méthode développée est appliquée à des jeux de données microarray sur le cancer du sein. Cependant elle a une limite : la matrice de covariance utilisée dans le g-prior doit nécessairement être inversible. Or il y a deux cas pour lesquels cette matrice est singulière : lorsque le nombre de variables sélectionnées dépasse le nombre d'observations, ou lorsque des variables sont combinaisons linéaires d'autres variables. Nous proposons donc une modification de l'a priori de Zellner en y introduisant un paramètre de type ridge, ainsi qu'une manière de choisir les hyper-paramètres associés. L'a priori obtenu est un compromis entre le g-prior classique et l'a priori supposant l'indépendance des coefficients de régression, et se rapproche d'un a priori précédemment proposé par Gupta et Ibrahim (2007).Dans une seconde partie nous développons deux nouvelles méthodes MCMC basées sur des populations de chaînes. Dans le cas de modèles complexes ayant de nombreux paramètres, mais où la vraisemblance des données peut se calculer, l'algorithme Equi-Energy Sampler (EES) introduit par Kou et al. (2006) est apparemment plus efficace que l'algorithme classique du Parallel Tempering (PT) introduit par Geyer (1991). Cependant, il est difficile d'utilisation lorsqu'il est couplé avec un échantillonneur de Gibbs, et nécessite un stockage important de valeurs. Nous proposons un algorithme combinant le PT avec le principe d'échanges entre chaînes ayant des niveaux d'énergie similaires dans le même esprit que l'EES. Cette adaptation appelée Parallel Tempering with Equi-Energy Moves (PTEEM) conserve l'idée originale qui fait la force de l'algorithme EES tout en assurant de bonnes propriétés théoriques et une utilisation facile avec un échantillonneur de Gibbs.Enfin, dans certains cas complexes l'inférence peut être difficile car le calcul de la vraisemblance des données s'avère trop coûteux, voire impossible. De nombreuses méthodes sans vraisemblance ont été développées. Par analogie avec le Parallel Tempering, nous proposons une méthode appelée ABC-Parallel Tempering, basée sur la théorie des MCMC, utilisant une population de chaînes et permettant des échanges entre elles. / This thesis is divided into two main parts. In the first part, we propose a Bayesian variable selection method for probit mixed models. The objective is to select few relevant variables among tens of thousands while taking into account the design of a study, and in particular the fact that several datasets are merged together. The probit mixed model used is considered as part of a larger hierarchical Bayesian model, and the dataset is introduced as a random effect. The proposed method extends a work of Lee et al. (2003). The first step is to specify the model and prior distributions. In particular, we use the g-prior of Zellner (1986) for the fixed regression coefficients. In a second step, we use a Metropolis-within-Gibbs algorithm combined with the grouping (or blocking) technique of Liu (1994). This choice has both theoritical and practical advantages. The method developed is applied to merged microarray datasets of patients with breast cancer. However, this method has a limit: the covariance matrix involved in the g-prior should not be singular. But there are two standard cases in which it is singular: if the number of observations is lower than the number of variables, or if some variables are linear combinations of others. In such situations we propose to modify the g-prior by introducing a ridge parameter, and a simple way to choose the associated hyper-parameters. The prior obtained is a compromise between the conditional independent case of the coefficient regressors and the automatic scaling advantage offered by the g-prior, and can be linked to the work of Gupta and Ibrahim (2007).In the second part, we develop two new population-based MCMC methods. In cases of complex models with several parameters, but whose likelihood can be computed, the Equi-Energy Sampler (EES) of Kou et al. (2006) seems to be more efficient than the Parallel Tempering (PT) algorithm introduced by Geyer (1991). However it is difficult to use in combination with a Gibbs sampler, and it necessitates increased storage. We propose an algorithm combining the PT with the principle of exchange moves between chains with same levels of energy, in the spirit of the EES. This adaptation which we are calling Parallel Tempering with Equi-Energy Move (PTEEM) keeps the original idea of the EES method while ensuring good theoretical properties and a practical use in combination with a Gibbs sampler.Then, in some complex models whose likelihood is analytically or computationally intractable, the inference can be difficult. Several likelihood-free methods (or Approximate Bayesian Computational Methods) have been developed. We propose a new algorithm, the Likelihood Free-Parallel Tempering, based on the MCMC theory and on a population of chains, by using an analogy with the Parallel Tempering algorithm.