Cette thèse porte sur l’influence des transformations de phases solide-solide sur la propagation de fissure. On souhaite ainsi mieux comprendre les variations de ténacité en cours de soudage par exemple, ou bien pendant la réparation d’une fissure. Dans ce travail, la ténacité est obtenue à partir de l’intégrale J. Il existe de nombreuses méthodes expérimentales permettant d’obtenir la ténacité critique JIC mais qui sont difficilement applicables pour des essais se déroulant pendant une transformation de phase. C’est pourquoi nous avons proposé une méthode couplant essai mécanique et mesure par corrélation d’images avec de la simulation par éléments finis. Les essais sont réalisés sur de simples éprouvettes plates pré fissurées, faciles à usiner et simple à chauffer par induction. Les essais sont conduits pour différentes températures et jusqu’à rupture. En sus des mesures d’efforts et déplacements de traverse, la corrélation d’images nous fourni également les champs de déplacement sur chaque face de l’éprouvette. Chaque essai est ensuite simulé par éléments finis où la ténacité critique est calculée par la méthode G-Theta au maximum de la charge supportée par l’éprouvette. Les simulations précédentes intègrent les conditions aux limites obtenues par corrélation et le comportement mécanique considéré est celui que nous avons identifié sur des essais de caractérisation. Deux nuances de matériau ont été étudiées avec cette méthode ; l’acier inoxydale 15-5PH ainsi que l’acier ferritique 16MND5. Pour ces deux matériaux, différentes températures d’essai ont été choisies avant, pendant et après la transformation pour effectuer les essais de rupture ainsi que de caractérisation du comportement mécanique. Les résultats de cette étude montrent que la transformation de phase peut avoir un impact non négligeable sur la ténacité. Ainsi, pour le 15-5PH, le taux d’austénite résiduel est un facteur important et les essais pendant la transformation martensitiques montrent que la ténacité critique peut être inférieure pendant celle ci à celle du matériau purement austénitique. Dans le cas du 16MND5, la ténacité est beaucoup plus faible à 600°C (et bainitique) qu’à température ambiante ce qui est assez logique. Par contre, lors du refroidissement, depuis 600° (austénitique) jusqu’à la température ambiante (bainitique), nous avons obtenu une ténacité critique relativement constante. En conclusion, cette étude apporte une solution quant à la mesure de la ténacité critique de matériau pendant des transformations de phases, ce que ne permettent pas forcément les essais normalisés. Pour le 15-5PH, la ténacité critique semble évoluer pendant la transformation martensitique et est assez dépendante du taux d’austénite résiduelle. Il semble par contre que pour le 16MND5, la ténacité critique soit assez peu dépendante de la fraction volumique d’austénite et la valeur obtenue varie peu au cours du refroidissement du matériau depuis 600°C. / Ou study focuses on the effects of phase transformations on crack propagation. We want to understand the changes of fracture toughness during welding. In this work, fracture toughness is expressed by J-integral. There are many experimental methods to obtain the critical toughness JIC but they are impractical for our investigation during phase transformation. That is the reason why we have proposed a method coupling mechanical tests, digital image correlation and finite element simulation. The fracture tests are implemented on pre-cracked single edge notched plate sample which is easy for machining and heat conduct during phase transformation. The tests are conducted at different temperatures until rupture. Digital image correlation gives us the displacement information on every sample. Each test is then simulated by finite element where the fracture toughness is evaluated by the method G-Theta at the crack propagation starting moment found by potential drop method and digital image correlation technical. Two materials have been studied, 15Cr-5Ni martensitic precipitation hardening stainless steel and 16MND5 ferritic low carbon steel. For these two materials, different test temperatures were chosen before, during and after phase transformation for testing and failure characterization of the mechanical behavior. Investigation result shows that metallurgical phase transformation has an influence on fracture toughness and further crack propagation. For 15-5PH, the result of J1C shows that the as received 15-5PH has higher fracture toughness than the one at 200°C. The toughness is also higher than the original material after one cycle heat treatment probably due to some residual austenite. Meanwhile, pure austenite 15-5PH at 200°C has higher fracture toughness than pure martensitic 15-5PH at 200°C. For 16MND5, the result also proves that the phase transformation affects fracture toughness. The as received material has bigger J1C than the situation where it was heated to 600°C. On the other hand, the material at 600°C just before isothermal bainite transformation after the austenitization during cooling process also has higher fracture toughness than the one at 600°C before austenitization. These two conclusions are consistent well with the result of 15-5PH. But the final situation of 16MND5 after one cycle heat treatment has a slightly smaller J1C than the receiving situation. It means that one cycle heat treatment hasn't an significant influence on 16MND5fracture toughness. Conclusions show that one should pay attention to the heating period before austenitization of the substrate material when people do the welding as the higher temperature will bring the lower fracture toughness during this process. While during cooling period, the fracture toughness doesn't change a lot during, before or after the cooling induced phase transformation. Even for 15-5PH, it has a better fracture toughness after the martensite transformation than before.

Lors d’un recuit inter-critique d’un acier dit « Medium Manganèse », dont la teneur en Mn est située entre 4 et 12 %, avec une microstructure initiale complètement martensitique, la formation de l’austénite obéit à un mécanisme spécifique qui porte le nom d'ART - « Austenite Reverted Transformation » (transformation inverse de l’austénite). L’objectif de ce travail de thèse était d’étudier et de modéliser les évolutions microstructurales en lien avec les propriétés mécaniques lors d’un recuit ART. Il a été déterminé que la microstructure finale se compose de phases de nature (ferrite, austénite résiduelle et martensite de trempe) et morphologie (en forme d’aiguille et polygonale) différentes. Une attention particulière a été accordée aux cinétiques de dissolution des carbures et de formation de l’austénite. Une vision complète de ces processus a été construite. En outre, le mécanisme de stabilisation de l’austénite résiduelle à la température ambiante a été étudié et discuté. Enfin, des essais de traction ont été réalisés afin d’évaluer le comportement mécanique de l’acier après différents recuits ART et établir le lien avec la microstructure. Une analyse plus détaillée du comportement de chaque constituant de la microstructure a été effectuée. A l'issue de cette thèse, un modèle complet est disponible pour calculer les courbes de contrainte vraie - déformation vraie d’un acier Medium Mn / During the intercritical annealing of fully martensitic Medium Mn steel, containing from 4 to 12 wt.% Mn, the formation of austenite happens through the so-called “Austenite Reverted Transformation” (ART) mechanism. In this PhD work, the evolution of both microstructure and tensile properties was studied as a function of holding time in the intercritical domain. The microstructure evolution was studied using a double experimental and modeling approach. The final microstructure contained phases of different natures (ferrite (annealed martensite), retained austenite and fresh martensite) and of different morphologies (lath-like and polygonal). A particular attention was paid to the kinetics of austenite formation in connection with cementite dissolution and to the morphology of the phases. A mechanism was proposed to describe the formation of such microstructure. The critical factors controlling thermal austenite stability, including both chemical and size effects, were determined and discussed, based on the analysis of the retained austenite time-evolution. At last, tensile properties of the steel were measured as a function of holding time and the relation between microstructure and mechanical behavior was analyzed. Advanced analysis of the individual behavior of the three major constituents was performed. As a final output of this work, a complete model for predicting the true-stress versus true-strain curves of medium Mn steels was proposed

The effect of Laves phase (Fe2Nb) formation on the Charpy impact toughness of the ferritic stainless steel type AISI 441 was investigated. The steel exhibits good toughness after solution treatment at 850°C, but above and below this treatment temperature the impact toughness decreases sharply. With heat treatment below 850°C the presence of the Laves phase on grain boundaries and dislocations plays a significant role in embrittlement of the steel whereas above that temperature, an increase in the grain size from grain growth plays a major role in the impact embrittlement of this alloy. The toughness results agree with the phase equilibrium calculations made using Thermo–Calc® whereby it was observed that a decrease in the Laves phase volume fraction with increasing temperature corresponds to an increase in the impact toughness of the steel. Annealing above 900°C where no Laves phase exists, grain growth is found which similarly has a very negative influence on the steel’s impact properties. Where both a large grain size as well as Laves phase is present, it appears that the grain size may be the dominant embrittlement mechanism. Both the Laves phase and grain growth, therefore, have a significant influence on the impact properties of the steel, while the Laves phase’s precipitation behaviour has also been investigated with reference to the plant’s manufacturing process, particularly the cooling rate after a solution treatment. The microstructural analysis of the grain size shows that there is a steady increase in grain size up to about 950°C, but between 950°C and 1000°C there is a sudden and rapid 60 % increase in the grain size. The TEM analysis of the sample that was annealed at 900°C shows that the Laves phase had already completely dissolved and cannot, therefore, be responsible for “unpinning of grain boundaries” at temperatures of 900°C and higher where this “sudden” increase in grain size was found. The most plausible explanation appears to be one of Nb solute drag that loses its effectiveness within this temperature range, but this probably requires some further study to fully prove this effect. During isothermal annealing within the temperature range of 600 to 850°C, the time – temperature – precipitation (TTP) diagram for the Laves phase as determined from the transformation kinetic curves, shows two classical C noses on the transformation curves. The first one occurring at the higher temperatures of about 750 to 825°C and the second one at much lower temperatures, estimated to possibly be in the range of about 650 to 675°C. The transmission electron microscopy (TEM) analyses show that there are two independent nucleation mechanisms that are occurring within these two temperature ranges. At lower temperatures of about 600°C, the pertaining nucleation mechanism is on dislocations and as the temperature is increased to above 750°C, grain boundary nucleation becomes more dominant. Also, the morphology of the particles and the mis-orientation with the matrix changes with temperature. At lower temperatures the particles are more needle-like in shape, but as the temperature is increased the shape becomes more spheroidal. The effect of the steel’s composition on the Laves phase transformation kinetics shows that by lowering the Nb content in these type 441 stainless steels, had no significance effect on the kinetics on precipitation of the Laves phase. However, a Mo addition and a larger grain size of the steel, retard the formation of the Laves phase, although the optimum values of both parameters still need further quantification. The calculation made for the transformation kinetics of the Laves phase, using the number density of nucleation sites No and the interfacial energy, as the fitting parameters in this work, demonstrated a reasonable agreement with experimental results. / Thesis (PhD)--University of Pretoria, 2010. / Materials Science and Metallurgical Engineering / unrestricted

Die vorliegende Arbeit behandelt die Wechselwirkung von Verarbeitung und Gefüge Mn-Al basierter hartmagnetischer Werkstoffe sowie die Auswirkung des Gefüges auf deren Eigenschaften. Dabei wurde das Gefüge der metastabilen tau-Phase im Anschluss an die Phasenbildung aus der Hochtemperaturphase epsilon-MnAl und die Auswirkung einer anschließenden Umformung untersucht. Der Schwerpunkt der Arbeit lag in der Analyse der Evolution verschiedener Gefügebestandteile, wie Grenzflächenverteilung, Versetzungen und Korngröße unter Verwendung von Rasterelektronenmikroskopie und Elektronenrückstreubeugung. Die epsilon-tau Umwandlung kann auf 2 verschiedene Routen erfolgen. In beiden Fällen wird die Bildung von 3 kristallographisch unterschiedlichen zwillingsähnlichen Defekten beobachtet, die als wahre Zwillinge, Ordnungszwillinge und Pseudozwillinge bezeichnet werden. Sie lassen sich als Rotationen um einen kristallographischen {111}-Pol beschreiben. Der Anteil der Zwillingsdefekte nach der Umwandlung, aber auch die Korngröße und Versetzungsdichte sind von der gewählten Umwandlungsroute abhängig. Während die Sättigungspolarisation annähernd gleich ist, reagiert die Koerzitivfeldstärke sensitiv auf den Gefügezustand. Eine niedrige Korngröße und hohe Versetzungsdichte tragen zu ihrer Erhöhung bei. Eine anschließende Kaltumformung erzeugt ein vielfach verzwillingtes Verformungsgefüge mit hoher Koerzitivfeldstärke. Wärmebehandlungen und die Analyse der Schärfe von Kikuchi-Beugungsbildern haben gezeigt, dass nicht die hohe Zwillingsdichte, sondern primär Versetzungen im Verformungsgefüge die Koerzitivfeldstärke steigern. Warmumformung von tau-MnAl führt zur dynamischen Rekristallisation. Die Kinetik der Gefügeneubildung und die resultierende Korngröße sind stark von der Umformtemperatur abhängig. Durch Umformung lässt sich eine kristallographische Texturierung von tau-MnAl erreichen. Die Orientierung der magnetisch leichten [001]-Richtung ist dabei vom gewählten Umformverfahren und gegebenenfalls von der Nachbehandlung abhängig. Statische und dynamische Rekristallisation reduzieren den Anteil der Zwillingsdefekte signifikant und besonders Pseudozwillinge und Ordnungszwillinge werden im Gefüge beseitigt. Das Rekristallisationsgefüge weist gegenüber dem Umwandlungsgefüge einen geringeren Widerstand gegen die mit der Zersetzungsreaktion verbundene Bildung von beta-Mn auf. Die Ursache liegt in einer selektiven beta-Mn-Bildung an allgemeinen Korngrenzen, während die Zwillingsdefekte einen erhöhten Widerstand gegen sie Zersetzung aufweisen.

Due to their diversity, soft matter systems provide a convenient platform to study a variety of physical phenomena like phase transitions and collective motion. Encompassing a wide range of equilibrium and non-equilibrium systems, they often provide significant insight into the statistical mechanics of different kinds of many-body systems. Though large scale properties of such systems are of fundamental interest in their own accord, since most experimental realizations of soft matter systems are finite sized, there is a growing need to understand the effects of confinement or boundary conditions on the collective behaviour of such systems. The primary purpose of this thesis is to study the effects of boundary conditions or confinement on both equilibrium and non-equilibrium soft matter systems via theoretical modelling. For equilibrium systems we have studied a system of colloidal particles in harmonic confinement, and for non-equilibrium systems we consider a system of self-propelled rods in both harmonic and hard wall confinement. In Chapter 1 we first lay down some basic concepts of stochastic dynamics and Brownian motion, before discussing some of the recent results on confinement effects on colloidal systems, showing how the properties of a finite sized colloidal system can be very different from those of large, un confined systems. Thereafter turning to non-equilibrium active systems, we discuss various fundamental problems posed by these systems due to their unique ability to generate and dissipate energy on their own. We also point out some instances of observed confinement effects in such systems, such as boundary aggregation and transient hedgehog-like clusters near the boundary. Chapter 2 deals with the effect of harmonic confinement on a finite sized colloidal assembly, where we show that such finite size effects coupled with a confining potential can give rise to special features like initial position dependent expulsion of dopant particles. First we model experimentally studied small two-dimensional colloidal assemblies trapped by a defocussed laser beam by Langevin dynamics simulations in the presence of harmonic confinement and demonstrate how the system shows a crossover from liquid state to crystalline state as a function of the stiffness of the confinement. We also show that in the crystalline state the system can be effectively modelled as a rigid body under small force perturbations. Notably, while studying the dynamics of a defect particle inside these crystallites, we found evidence for the occurrence of self purification by the crystallites. In this process, a dopant is spontaneously expelled out of the crystallite. Surprisingly, this phenomena has a strong dependence on the initial position of the dopant, which turns out to be the consequence of the non monotonic spatial variation of the free energy of the system as a function of the dopant position. This is caused by a difference in the rate of change of internal energy and entropy with the dopant position, with the entropy decreasing faster when the dopant is closer to the centre. This can be attributed to the amount of disruption of crystalline order in the assembly due to the incommensurate dimensions of the defect particle. In order to put these results in a general perspective, we verify in the last part of this chapter that the presence of this free energy barrier is independent of the exact functional forms of the confining potential and the interaction of a defect particle with the host particles, as well as the shape and size of the defect particle. Moving to non-equilibrium systems, we consider, in Chapter 3, the effect of harmonic and hard wall confinement on a two-dimensional system of self-propelled rods (SPRs). Though there have been very limited studies of confinement effects on such systems, existing studies are adequate to show that their behaviour near a boundary wall can be very different, e.g. formation of hedgehog like clusters near a boundary wall. First we show that for harmonic confinement small systems show polar order, which decays with system size, eventually going away for large systems. But the effect of hard wall confinement turns out to be rather different, where the system shows isotropic and clustered states depending on the values of activity and density. We construct a complete activity-density phase diagram showing four distinct phases. For high density and high activity, the rods spontaneously arrange themselves into a stable vortex structure in which the rods exhibit global radial polar order. Surprisingly this order does not decay with system size: the radial orientation of the rods exhibit strong spatial correlation even in large systems, ruling out the possibility that the radial order is a finite-size effect. Using other geometrical shapes of the hard wall boundary, we confirm this phase to be independent of the shape of the boundary. We also demonstrate how small modifications of the boundary conditions at the hard wall can collapse the clustered and vortex phases to a global flocking phase similar to that found in earlier studies of hydrodynamic active particles under confinement. Based on these observations, we conclude that the bulk of the system is strongly affected by the subjected boundary condition, which is rather unusual for large systems. In Chapter 4 this thesis concludes with a summary of the main results and suggestions for future work along similar lines

Matériaux incontournables des matériaux fonctionnels, les alliages à mémoire de forme(AMF) peuvent présenter de très larges déformations réversibles. La Transformation de Phase Martensitique (TPM), ayant lieu lorsqu’il est soumis à une action mécanique ou thermique, lui confère des caractéristiques particulières. Le comportement thermomécanique des AMF est à présent bien maîtrisé. Cependant la connaissance de leur comportement `a la rupture reste un enjeu majeur pour leur dimensionnement dans le cadre de leur industrialisation pérenne. Ces travaux de recherche se sont attachés `a la connaissance, la description et la quantification du phénomène de localisation en pointe de fissure liée à la TPM induite sous contrainte, au travers du développement d’un modèle prédictif et de sa corrélation expérimentale par mesures de champs simultanées lors d’essais de rupture sur des éprouvettes fissurées de NiTi. Deux modèles analytiques basés sur la mécanique linéaire de la rupture, intégrant le caractère dissymétrique du comportement des AMF en traction/compression, ont été développés pour la prédiction des zones de transformation au voisinage de la pointe de fissure en tenant compte des différents modes de rupture ( élémentaires et mixtes I+II) et du rayon de courbure en pointe de fissure. Un banc de caractérisation par mesures simultanées de champs cinématiques par corrélation d’images (DIC) et thermique par thermographie infrarouge a été développé pour cartographier les champs expérimentaux d’essais de rupture en mode I sur des éprouvettes pré-fissurées. Cette bonne corrélation des modèles analytiques ouvre de nombreuses perspectives concernant l’analyse du couplage thermo mécanique associé à la TPM en pointe de fissure, l’enrichissement des modèles analytiques initiaux, et la confrontation avec les résultats expérimentaux pour des modes de rupture plus complexes (II et mixte I+II). / Major player among functional materials, Shape Memory Alloys (SMA) may undergo verylarge reversible strain. SMA exhibit a Martensitic Phase Transformation (MPT) when they aresubmitted to mechanical or thermal actions, and that gives them some specific characteristics.The thermomechanical behavior of SMA is now well controlled. However, the knowledge of theSMA fracture behavior is a major challenge for their design and sizing for their sustainableindustrialization. This research project has focused on the understanding, describing and quantifyingof the phenomenon of localization at the crack tip due to stress-induced MPT. The study includestwo main aspects: the development of an analytical model and its experimental correlation bysimultaneous field’s measurements during tests on cracked NiTi specimens. Two analytical modelsbased on the linear fracture mechanics and those introduce the asymmetrical nature of the SMAbehavior in tension/compression, were developed for the prediction of transformation zones in thevicinity of the crack tip, taking into account the fracture mode (elementary and mixed ones)and the radii of curvature of the crack tip. A testbench with the measurement of simultaneouskinematic field with Digital Image Correlation (DIC) and thermal field with infrared thermographywas designed for mapping the experimental fields during fracture tests in mode I on pre-crackedspecimen. This good correlation of analytical models opens up many perspectives on the analysisof thermomechanical coupling associated with the MPT at the crack tip, the enrichment of the initialanalytical models, and comparison with experimental results for more complex failure modes (II andmixed I+II).

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.

Paramagnetické niklem stabilizované tenké vrstvy plošně centrovaného kubického Fe, epitaxně narostené na monokrystalickém substrátu Cu(100) jsou známy svou schopností strukturní a magnetické fázové přeměny při ozáření iontovým svazkem, a to do prostorově centrované kubické struktury charakteristické feromagnetickými vlastnostmi. Monokrystalický Cu(100) substrát je možné také nahradit Si(100) s mezivrstvou Cu(100). Pomocí fokusovaného iontového svazku lze dále snadno lokálně modifikovat magnetické vlastnosti ozařované vrstvy. Tato metoda přímého zápisu magnetických struktur je alternativou k běžným litografickým technikám, nabízející nové jimi nedosažitelné možnosti. Připravené magnetické struktury následně využíváme k propagaci spinových vln. V práci je představen celý proces od růstu vrstev, přes přípravu mikrostruktur, až po studium jejich struktury a statických i dynamických magnetických vlastností. S využitím vektorového síťového analyzátoru studujeme ve vrstvách a v mikrostrukturách připravených fokusovaným iontovým svazkem feromagnetickou rezonanci a propagující se spinové vlny. Zdrojem spinových vln o definovaných vlnových vektorech jsou litograficky připravené koplanární vlnovody, sloužící také k induktivní detekci vln. Pomocí feromagnetické rezonance kvantitativně určujeme materiálové charakteristiky jako jsou saturační magnetizace a parametr útlumu a ze spekter propagujících módů následně určujeme charakteristiky spinových vln, které porovnáváme s dalšími feromagnetickými materiály.

Shape memory alloys (SMAs) operating as solid-state actuators pose economic and environmental benefits to the aerospace industry due to their lightweight, compact design, which provides potential for reducing fuel emissions and overall operating cost in aeronautical equipment. Despite wide applicability, the implementation of SMA technology into aerospace-related actuator applications is hindered by harsh environmental conditions, which necessitate extremely high or low transformation temperatures. The versatility of the NiTi-based SMA system shows potential for meeting these demanding material constraints, since transformation temperatures in NiTi can be significantly raised or lowered with ternary alloying elements and/or Ni:Ti ratio adjustments. In this thesis, the expansive transformation capabilities of the NiTi-based SMA system are demonstrated with a low and high-temperature NiTi-based SMA; each encompassing different stages of the SMA development process. First, exploratory work on the NiTiSn SMA system is presented. The viability of NiTiSn alloys as low-temperature SMAs (LTSMAs) was investigated over the course of five alloy heats. The site preference of Sn in near-equiatomic NiTi was examined along with the effects of solution annealing, Ni:Ti ratio adjustments, and precipitation strengthening on the thermomechanical properties of NiTiSn LTSMAs. Second, the thermomechanical processability of NiTiHf high-temperature SMA (HTSMA) wires is presented. The evolution of various microstructural features (grain size reduction, oxide growth, and nano-precipitation) were observed at incremental stages of the hot rolling process and linked to the thermal and mechanical responses of respective HTSMA rods/wires. This work was carried out in an effort to optimize the rolling/drawing process for NiTiHf HTSMAs.

The thesis is focused on high-temperature superconducting (HTS) ceramics series of bismuth. Specifically, there is studied Bi2Sr2CaCu2O8+x phase, known as the 2212 phase. The theoretical part describes the basic properties of superconductivity and superconductors, the properties of cuprate ceramics and description of LBCO, YBCO and BSCCO structures. The experimental part deals with the preparation of the precursor own Bi-2212 phase. It is synthesized by a process called sol-gel. Feedstock Bi2O3, CaCO3, SrCO3 and CuSO4 was dissolved in HNO3 and transferred to a complex with ethylenediaminetetraacetic acid (EDTA, Chelaton II). With NH3 pH > 9 was maintained due to the stability of complex. The obtained gel was concentrated, calcinated in a furnace at 860 °C and crushed into powder. Pure powder was subjected to analysis dipping microscope, SEM, XRD, FT-IR, TG-DTA at different atmospheres argon, oxygen and air. Then 1 wt.% of the oxide (La, Y, Sc, Sm) was added to part of the powder precursor and the samples were examined using TG-DTA.