L’arille de Momordica cochinchinensis (gac), un fruit de la famille des Cucurbitacées, est la source végétale la plus riche en lycopène et β-carotène. Ces deux composés ont, respectivement, un rôle de puissant antioxydant et de provitamine A, intéressant les compléments santé. Tout d'abord, un procédé d’extraction fractionnée douce a été développé pour extraire ces caroténoïdes naturels en gardant leur qualité originale. Puis, le lycopène et le β-carotène extraits ont été caractérisés et analysés. Au moins 95 % des extraits sont composés de l’isomère all-trans. Ils ne sont pas dégradés pendant le traitement thermique représentant les procédés de formulation. Leur stéréo-mutation thermique a été évaluée. Le lycopène est plus antioxydant et donc plus rapidement isomérisé que le β-carotène à haute température. L’isomérisation augmente leur activité antioxydante, qui a été évalué par test chimique TEAC et sur l’hémolyse des cellules sanguines (KRL) in vitro. Les deux caroténoïdes de l’arille de gac sont beaucoup plus antioxydants que le Trolox contre l’hémolyse. En comparant avec d’autres sources de β-carotène, les caroténoïdes extraits de gac dans ces conditions douces restent antioxydants même à des concentrations plus élevées contrairement à ceux extraits dans des conditions classiques qui deviennent prooxydants. Ces résultats permettent de discuter la bioactivité des caroténoïdes d'après leur qualité et de leur origine, c’est à dire leur source et leur procédé d’extraction. D’un point de vue applicatif, outre le procédé de fractionnement qui est industrialisable, le traitement thermique appliqué permet de contrôler la fonctionnalité des produits riches en caroténoïdes. / The aril of Momordica cochinchinensis (gac), plant from the Cucurbitaceae family, is the richest source of lycopene and β-carotene, which are a strong antioxidant and a pro-vitamin A, respectively, interesting for health-complements. First, a process of soft extraction-fractionation was developed for extracting effectively the natural carotenoids from gac without loss of their original quality. Then, the lycopene and β-carotene extracted from gac were analyzed and characterized. At least 95% of the extracts were composed of the all-trans isomer. They were not degraded during the heat-treatment mimicking formulation processing. Their thermal stereo-mutation was evaluated. Lycopene is more antioxidant, it is thus isomerized more rapidly than β-carotene at high temperature. The isomerization of carotenoids increases their antioxidant activity that was evaluated by the chemical test TEAC and through the hemolysis of red blood cells (KRL) in vitro. The lycopene and β-carotene from gac are notably more antioxidant than Trolox. By comparing with other sources of β-carotene, carotenoids extracted from gac in these soft conditions keep their antioxidant properties, even at high concentration, contrasting with extracts obtained in classical conditions that become prooxidant. From these results, the bioactivity of carotenoids is discussed from their quality and their origin that is their source and extraction process. For application, in addition to the fractionation process which is easily transferable to the industry scale, the heat-treatment used in this study is interesting for controlling products rich in functional carotenoids

Les ventes des fromages AOP subissent un affaiblissement. L’utilisation de ces fromages sous forme d’ingrédient représente une alternative intéressante à la dégustation et permettrait de maintenir une activité durable aux producteurs de ces fromages. L’objectif de ce travail est d’explorer les potentialités de 4 catégories de fromages à pâte persillée AOP du Massif-Central à être utilisés comme ingrédient à chaud pour répondre à des propriétés telles que « fondant, nappant, filant, gratinant». Les fonctionnalités recherchées pour ce type d’usage ont été prospectées à l’aide de méthodes physico-chimiques et instrumentales classiques mais également à l’aide de méthodes spectrales et sensorielles afin d’enrichir les observations de la macro et microstructure fromagère et de la perception du consommateur. Dans un premier temps, les caractéristiques physicochimiques, rhéologiques et sensorielles à froid et certaines propriétés à chaud ont été décrites pour les 4 catégories de fromages. Ces premiers résultats ont permis de cataloguer les fromages selon des caractéristiques essentiellement liées à l’organisation matricielle des composants tels que les protéines, les matières grasses, les minéraux. L’analyse sensorielle a permis de décrire précisément certaines propriétés à froid qui ne sont pas mises en évidence par d’autres analyses. Les pâtes persillées ont une grande hétérogénéité de pâte due à la présence de« veines » de moisissures. La seconde partie est une étude sur la capacité de la SFS en tant que méthode d’étude de la micro structure, à prédire la diversité de composition de ces fromages. Malgré la forte hétérogénéité des fromages, la SFS permet une « empreinte » identifiable des fromages et prédit certains mais pas la totalité des paramètres physicochimiques. L’évolution de la macro et microstructure de ces fromages au cours du chauffage et du refroidissement a ensuite été étudiée par SFS et par test de compression dynamique. Ces méthodes décrivent bien la fonte de la matière grasse et de la matrice fromagère. Elles sont corrélées entre elles et démontrent une relation entre la structure moléculaire et les propriétés rhéologiques de ces fromages. Une étude comparative des propriétés sensorielles des fromages a été menée à froid et après chauffage. Les attributs décrivent des caractéristiques de texture différentes entre les 2 conditions. Cette démarche a permis de bien différencier les 4 catégories de fromages et de mettre en évidence certains attributs de qualité ou de défaut pour une utilisation à chaud. En conclusion, ces 4 catégories de fromages à pâte persillée ont des potentialités à être utilisées comme ingrédient pour usage à chaud. L’analyse sensorielle a caractérisé les perceptions des consommateurs vis à vis de ces fromages chauffés et ainsi aider à préciser leurs fonctionnalités. Les analyses rhéologiques et spectrales ont apporté des explications liées à ce traitement au niveau de la macro et microstructure de la matrice fromagère. / Sales of PDO cheeses undergo a decline. The use of these cheeses in the form of ingredient represents an interesting alternative to the tasting and would allow to maintain a sustainable business activity to the producers of these cheeses. The objective of this work is to investigate the potentialities of four categories of Blue cheese PDO of the Massif Central as an ingredient to meet their properties during heating such as "melting, stretchability, browning". The functional properties desired for this type of cheese have been investigated by physico-chemical methods and instrumental classics and also by spectral method and sensory evaluations to enrich the observations of the macro and microstructure of the cheese and the consumer perception. First, the physicochemical, rheological, sensory characteristics and certain properties during heating have been reported for four categories of Blue cheese. These initial results allowed us to characterize the cheese studied according to their characteristics essentially which were related to the organization matrix constitutes such as proteins, fats, minerals. The sensory analysis allowed to describe exactly certain properties which are not revealed by theother analyses. Blue-veined cheeses have a great heterogeneity due to the presence of "veins" of mold. The second part is a study on the ability of the SFS method to study the micro structure and to predict the diversity of composition of these cheeses. Despite the high heterogeneity of cheeses, SFS allows an identifiable 'fingerprint' of cheese and predicts some but not the totality of the physicochemical parameters. The evolution of the macro-and microstructure of these cheeses during heating and cooling was then studied by SFS and dynamic shear test. These methods describe well the melting temperature of the fat and the cheese matrix. They are correlated between them and demonstrate a relationship between the molecular structure and the rheological properties of these cheeses. A comparative study of the sensory textural properties of cheeses was carried out in the non- and heated forms. The attributes describe different characteristics of texture between the two conditions. This approach allowed to differentiate well the four categories of cheeses and to highlight on certain attributes of quality or defects to be used in cooking application. In conclusion, these four categories of Blue-veined cheeses have the potential to be used as an ingredient in cooking application. The sensory analysis characterized the perceptions of the consumers in both non- and heated forms and thus helps to specify their features. The rheological and spectral analyses have provided explanations related to this treatment at the level of the macro and microstructure of the cheese matrix.

Na produção do etanol a etapa mais importante e crítica é a fermentação, por isso, há necessidade de focar a atenção ao processo e contaminações. Os contaminantes bacterianos de maior presença nessa etapa são os Lactobacillus. Com essa preocupação os objetivos deste trabalho são mostrar alternativas a redução desses contaminantes sendo eles no caldo ou no fermento (leveduras). Para isso amostras de caldo de cana-de-açúcar contaminados in vitro, individualmente, com sete diferentes espécies de Lactobacillus foram submetidas ao tratamento térmico visando confirmar a sensibilidade das mesmas à temperatura da água em ebulição. Amostras do caldo de cana-de-açúcar foram colocadas em uma cuba de clarificação com a água em ebulição. Foram retiradas amostras em diferentes tempos (0, 2, 3, 4 e 5 minutos) para que realizasse contagens (UFC/mL). Como já era esperado, as bactérias em questão se mostraram sensíveis à altas temperaturas não sobrevivendo por mais de 4 minutos. E com isso levantou-se a hipótese destas estarem presentes em dornas de fermentação devido à falhas de processamento (como uma clarificação ineficiente) e recontaminações posteriores. O projeto teve como objetivo também buscar uma alternativa ao tratamento ácido (ácido sulfúrico), utilizado como forma de descontaminação das leveduras (fermento). Foram utilizadas diferentes soluções alcoólicas (15, 20, 25, 30 e 35 % v/v) e em diferentes pH (2,5 e 6,0). Estas foram contaminadas, individualmente, com as mesmas sete diferentes espécies de Lactobacillus para verificação de sua sensibilidade ao etanol. Nos tempos (0, 30, 60, 90 e 120 minutos) foram retiradas amostras para contagens (UFC/mL). Os Lactobacillus se mostraram sensíveis ao etanol sendo mais evidente a concentrações maiores que 20% v/v. / In the ethanol production the most important and critical stage is the fermentation, therefore the necessity of focusing the attention to the process and contaminations. The contaminants of bigger presence in this stage are the Lactobacillus. With this concern the purpose of this work are shown alternatives to these contaminants. For that, samples of sugar cane broth contaminated in vitro, with seven different Lactobacillus species were subjected to the thermal treatment aiming to confirm the sensitivity of them at temperature of boiling water. Samples of sugar cane broth were placed in clarification vat with boiling water and were withdrawn in different times (0, 2, 3, 4 and 5 minutes) so that it carried out counting (UFC/mL), checking the sensitivity of microorganisms to temperature. As was expected, the bacteria in question were sensitive not survive for more than 4 minutes. And with that raised the possibility of they were present in fermentation tanks due to the failure of processing (like an inefficient clarification) and subsequent recontamination. The purpose of the project is also find an alternative to acid treatment (sulphuric acid), used as decontamination form of the yeast (leaven). Were used different alcoholic solutions (15, 20, 25, 30 and 35 % v/v) and in different pH (2,5 and 6,0). These were contaminated (separately) in laboratory with the same seven different lactobacillus genus for checking their sensitivity to ethanol. At times (0, 30, 60, 90 and 120 minutes) samples were withdrawn for counts (UFC / mL). The Lactobacillus were sensitive to ethanol, being more evident at 20% v / v.

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

This thesis focused on austenitic-ferritic (duplex) stainless steels and their mechanical and technological properties. The theoretical part includes introduction to chemical composition, structure, heat treatment and properties of these steels. The practical part focuses on influence of casting temperature on technological properties of ASTM A890 Gr4A stainless duplex steel. Furthermore, there is evaluated influence of chemical composition and heat treatment on structure and mechanical properties of different duplex stainless steels.

Cíle této práce jsou: (i) vyhodnocení vlivu Y2O3 kelímku na kontaminaci indukčně tavené NiTi slitiny obohacené niklem, (ii) optimalizace podmínek, při kterých jsou tavby uskutečněny a (iii) získání nových DSC a 3D AP dat o vlivu vodíkové atmosféry na martenzitickou transformaci a na strukturu NiTi slitin obohacené niklem s tvarovou pamětí. Byly provedeny následující experimenty: – Pět taveb bylo navrženo a provedeno tak, aby byla snížena maximální tavící teplota. – Pět přetaveb bylo uskutečněno při teplotě 1500 C s dobou výdrže 2, 10 a 20 minut a při teplotách 1450 C a 1550 C s 20 minutovou dobou výdrže. Experiment byl navržen tak, aby byl vyšetřen vliv tavící teploty a doby výdrže na obsah kyslíku pocházejícího z kelímku Y2O3 v tavenině. – Tepelné zpracování NiTi slitiny obohacené niklem v režimu I (žíhání) a v režimu II (kombinace žíhání se stárnutím) pod atmosférou vodíku, směsi vodíku s héliem a pod referenční atmosférou čistého hélia. Získané výsledky jsou: – Navržené tavící postupy vedou ke snížení maximální tavící teploty a to z 1800 C na 1400 C. Přesto toto velké snížení maximální tavící teploty nevedlo k významnému poklesu obsahu kyslíku. – Během přetavby uskutečněné při teplotě 1500 C s dobou výdrže 2 minuty se obsah kyslíku navýšil o trojnásobek jeho počáteční hodnoty a příliš se nelišil od obsahu kyslíku naměřeného ve slitině, která byla přetavena při stejné teplotě s dobou výdrže 10 minut. K nárustu o čtyřnásobek počáteční hodnoty obsahu kyslíku došlo u přetavby vedené na teplotě 1450 C po dobu 20 minut a hodnota obsahu kyslíku se příliš nelišila od hodnoty naměřené ve slitině přetavené při teplotě 1550 C se stejnou dobou výdrže. – S rostoucím parciálním tlakem vodíku dochází k potlačení jednokrokové martenzitické transformace. Významný pokles výšky DSC píku nastává při parciálním tlaku 100 mbar. 3D AP analýza odhalila, že nedochází k žádné lokální změně koncentrace a nebo pozic niklových a titanových atomů ve vzorku, který byl žíhán v režimu I ve vodíku. Bylo objeveno, že vodík tvoří stabilní intersticiální tuhý roztok v NiTi B2 mřížce, kde vytváří systém nanodomén s obsahem vodíku vyšší než 10 at%.

Die vorliegende Arbeit beschäftigt sich mit der Entwicklung von Sol-Gel-Beschichtungen durch Optimierung der Ausgangszusammensetzung und der Applikations-Parameter für den Korrosionsschutz der Aluminium-Legierung AA7075. Verschiedene Arten von Silanen, z. B. Tetraethoxysilan (TEOS), Phenyltriethoxysilan (PTES) und Phenyltrim­ethoxysilan (PTMS) sind verglichen worden: Der Sol-Gel-Film aus PTMS präpariert, weist dabei die höchste Hydrophobizität auf, was sich insbesondere in den Barriere-Eigenschaften dieser Verbindung zeigte. Die Wirkung von Essigsäure als Katalysator in Sol-Gel-Prozessen wurden untersucht, um die optimale Katalysatorkonzentration für den Korrosionsschutz der beschichteten Proben zu ermitteln. Die Korrosionsbeständigkeit der beschichteten Proben sinkt bei höheren Konzentrationen des sauren Katalysators durch die Auflösung des Aluminiumoxids an der Substratoberfläche. Allerdings führten zu niedrige Konzentrationen des Katalysators zur Verlangsamung der Hydrolysereaktionen der Silane und es bildete sich poröse Sol-Gel-Schichten. Die Wärmebehandlung der beschichteten Aluminium-Proben ist für die Vernetzung des Films erforderlich. Eine Wärmebehandlung bei 300 ˚C für 2,5 Stunden ergab dabei den besten Korrosionsschutz. Höhere Temperaturen führten zu einer Verschlechterung der Eigenschaften der Filme, was mit der Zerstörung des organischen Teil des Films erklärt werden kann. Darüber hinaus verursachen zu niedrige Temperaturen einen geringeren Korrosionsschutz der beschichteten Aluminium-Proben. Vermutlich ist die geringe Vernetzung des Sol-Gel-Films bei Temperaturen was für als 300 ˚C verantwortlich. Die beschichteten Aluminium-Proben wuden mittels Raster-Elektronenmikroskopie (SEM), Energiedispersive Röntgenspektroskopie (EDX), Röntgen-Photoelektronenspektroskopie (XPS) und elektrochemischen Techniken charakterisiert. / The present work pertains to the development of sol-gel coatings by optimizing the composition and the application parameters for corrosion protection of aluminum alloy AA7075. Different kinds of silanes e.g. tetraethoxysilane (TEOS), phenyltriethoxysilane (PTES) and phenyltrimethoxysilane (PTMS) have been compared: the sol-gel film prepared from PTMS shows highest hydrophobicity manifested by the best barrier property of this compound. The effect of acetic acid as a catalyst on the chemistry of the sol is investigated in order to estimate the best catalyst concentration for better corrosion protection of the coated samples. The corrosion resistance of the coated samples is found to be decreasing at higher concentrations of the catalyst due to the dissolution of the aluminum oxide at the substrate surface in the acid sol. However, lower concentrations of the catalyst lead to low hydrolysis reactions of the silanes and non-dense sol-gel films have been formed. The heat treatment of the coated aluminum samples is required for cross-linking of the film. The heat treatment at 300 ˚C for 2.5 hours exhibits the best corrosion protection. Higher treatment-temperatures lead to degradation of the properties of the film which can be described in terms of destroying the organic part of the film. Moreover, low treatment-temperatures cause low corrosion protection of the coated aluminum samples which is presumably attributed to the low cross-linking of the sol-gel film at temperatures less than 300 ˚C. The coated aluminum samples are characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS) and electrochemical techniques.

A compositionally graded Ti-xCr (10≤x≤30 wt%) alloy has been fabricated using Laser Engineered Net Shaping (LENSTM) to study the microstructural phase evolution along a compositional gradient in both as-deposited and heat treated conditions (1000°C followed by furnace cooling or air cooling). The alloys were characterized by SEM BSE imaging, XRD, EBSD, TEM and micro-hardness measurements to determine processing-structure-property relations. For the as-deposited alloy, α-Ti, β-Ti, and TiCr2 (C15 Laves) phases exist in varying phase fractions, which were influential in determining hardness values. With the furnace cooled alloy, there was more homogeneous nucleation of α phase throughout the sample with a larger phase fraction of TiCr2 resulting in increased hardness values. When compared to the air cooled alloy, there was absence of wide scale nucleation of α phase and formation of ω phase within the β phase due to the quicker cooling from elevated temperature. At lower concentrations of Cr, the kinetics resulted in a diffusionless phase transformation of ω phase with increased hardness and a lower phase fraction of TiCr2. In contrast at higher Cr concentrations, α phase separation reaction occurs where the β phase is spinodally decomposed to Cr solute-lean β1 and solute-rich β2 resulting in reduced hardness.

The presented diploma thesis deals with various types of quenching and their respective effects on mechanical and structural properties of AlSi7Mg0.6 alloy castings. Cast with precision casting technology into a self-supporting ceramic shell made by plaster investment technology, flat test bars cast by Alucast were used as experimental samples. Sample castings were used in both cast state and after T6 heat treatment. Air-flow and air-water combination with varying water passage (spraying) were used as the quenching media in the quenching process of the castings. In order to evaluate the effect of five different quenching processes on the structure and mechanical properties of the castings, the method of light microscopy, Brinell hardness test and static traction test were used. Evaluation and porosity and SDAS quantifications were carried out by means of image analysis. Experiments did not prove right the hypothesis holding that low SDAS values inevitably mean higher mechanical properties of the castings. On the other hand, distinct is the negative influence of heterogeneous structure and porosity. Despite the fact that the heat treatment was successful in reducing the influence of structural inhomogeneities, it cannot be concluded that spray quenching has an utterly positive bearing on the mechanical and structural properties of the castings.

The subject of this master thesis is focused to the refining of the cast structure of gamma-TiAl–2Nb alloy using cyclic heat treatment and to the analysis of the grain refining mechanism. Structure evolution after applied cycles of heat treatment was characterized using light, laser and electron microscopy and using microhardness tests. Application of five heat treatment cycles during which two phase transformations (eutectoid and alpha-recrystallization reactions) repeatedly took place resulted in refining of the cast columnar structure having the mean grain size 512 microns to fully lamellar structure containing gamma and alpha2 phases having the mean grain size 229 microns. Lamellae thickness of gamma was not changed while the thickness of alpha2 phase decreased, up to 78 nm. Refining of alpha2 phase resulted in the increase of the microhardness by 20 %. The recrystallized cast structure obtained by cyclic heat treatment and the knowledge on the mechanisms of the refining the structure were compared with the literature data and were discussed in order to propose more efficient procedure for refining thermal treatment of cast TiAl alloys.