In this study, the goal is to predict the microstructure evolution during and after the hot working of a martensitic stainless steel with 13% chromium using a physically-based model in the form of a MATLAB toolbox. This model is based on dislocation density theory and consists of coupled sets of evolution equations for dislocation, vacancies, recovery, recrystallization, and grain growth. The focus in this work is on the flow stress calculation and the effect of second phase particles on the strengthening mechanisms in the material at elevated temperatures. Recovery and recrystallization are also studied for this alloy during deformation and following stress relaxation. The experimental part of this work was performed with a Gleeble thermo-mechanical simulator over the temperature range of 850 to 1200°C. Samples were investigated later by a light optical microscope (LOM) and a scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscope (EDS). Hardness test and phase isolation were also performed on the samples and the results are compared with the modeling results. The model can satisfactorily predict the grain growth, recovery, recrystallization, and flow stress for this alloy. Further investigation on the second phase particles showed that the measured mean size of carbides has a good agreement with what is obtained from the model and the hardness values. On the other hand, the modeled volume fraction of the carbides followed a slightly different trend comparing to hardness values, and phase isolation results at temperatures higher than 1000°C. Additionally, the Ms temperature and fraction of the martensite phase are calculated for quenched samples where the results are following the measured hardness values. Finally, the Zener-Hollomon parameter (Z) and its relation to the flow stress and the activation energy for deformation are defined. The dynamic recrystallization (DRX) kinetic is modeled and the fraction DRX was calculated at various temperatures and strain rates for this alloy. / I denna studie är målet att förutsäga mikrostrukturutvecklingen under och efter varmbearbetning i ett martensitiskt rostfritt stål med 13 % krom med hjälp av en fysisk baserad modell i form av en MATLAB verktygslåda. Denna modell är baserad på en teori för dislokationstäthet och bestårav kopplade uppsättningar av evolutionsekvationer för dislokation, vakanser, återhämtning, rekristallisation och kornstillväxt. Fokus i detta arbete är beräkning av flytespänningen och effekten av sekundärfaspartiklar på härdningsmekanismerna i materialet vid höga temperaturer. Återhämtning och rekristallisation studeras också för denna legering under deformation och efter spänningsrelaxation. Den experimentella delen av detta arbete utfördes med en Gleeble termomekanisk simulator inom temperaturområdet 850 till 1200°C. Proverna undersöktes senare med ett ljust optiskt mikroskop (LOM) och svepelektronmikroskop(SEM) utrustad med energidispersiv spektroskopi (EDS). Hårdhetstest och fasisolering utfördes också på proverna och resultaten jämförs med modelleringsresultaten. Modellen på ett tillfredsställande sätt kan förutsäga korntillväxt, återhämtning, rekristallisation och flytspänningen för denna legering. Vidare undersökning av partiklarna i sekundärfasen visade att den uppmätta medelstorleken för karbider har bra överensstämmelse med vad som erhålls från modellen och hårdhetsvärdena. Den modellerade volymfraktionen av karbiderna följde en något annorlunda trend vid temperaturerna högre än 1000°C jämfört med hårdhetsvärden och fasisoleringsresultat. Dessutom beräknas Ms temperaturen och fraktionen av martensitfasen för släckta prover där resultaten följer de uppmätta hårdhetsvärdena. Slutligen definieras Zener-Hollomon-parametern (Z) och dess förhållande till flytspänningen och aktiveringsenergin för deformation. Den kinetiska dynamiska rekristallisation (DRX) modelleras och fraktionen DRX beräknades vidolika temperaturer och töjningshastigheter för denna legering.

The aim of this work was to systematically study how the microstructure evolution is affected by the carbon activity in WC-Ni cemented carbides. Seven WC-9.59at%Ni alloys with different carbon activity were sintered at 1500 °C. From investigating these alloys, the carbon window has been experimentally evaluated using light optical microscopy and compared to theoretical carbon window calculated using Thermo-Calc. The overall microstructure of cross sections and raw surfaces have been investigated using scanning electron microscopy. Finally, the WC grain size and distribution have been evaluated using electron backscatter diffraction. It was found that the experimental carbon window was slightly wider than the theoretical carbon window. The WC grain size increased and the grain size distribution got wider with increasing carbon activity. In addition, the largest WC grains showed the largest grain growth by increasing carbon activity. By comparing the present results of grain size and distribution of WC-Ni to previous results of WC-Co, it was found that the WC grain growth was more pronounced and more influenced by the carbon activity.

High chromium cast iron (HCCI) is considered as one of the most useful wear resistance materials and their usage are widely spread in industry. The wear resistance and mechanical properties of HCCI mainly depend on type, size, number, morphology of hard carbides and the matrix structure (γ or α). The Hypereutectic HCCI with large volume fractions of hard carbides is preferred to apply in wear applications. However, the coarser and larger primary M7C3 carbides will be precipitated during the solidification of the hypereutectic alloy and these will have a negative influence on the wear resistance. In this thesis, the Ti-added hypereutectic HCCI with a main composition of Fe-17mass%Cr-4mass%C is quantitatively studied based on the type, size distribution, composition and morphology of hard carbides and martensite units. A 11.2μm border size is suggested to classify the primary M7C3 carbides and eutectic M7C3 carbides. Thereafter, the change of the solidification structure and especially the refinement of carbides (M7C3 and TiC) size by changing the cooling rates and Ti addition is determined and discussed. Furthermore, the mechanical properties of hypereutectic HCCI related to the solidification structure are discussed. Mechanical properties of HCCI can normally be improved by a heat treatment process. The size distribution and the volume fraction of carbides (M7C3 and TiC) as well as the matrix structure (martensite) were examined by means of scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD). Especially for the matrix structure, EBSD is a useful tool to classify the fcc (γ) and bcc (α) phases. In conclusion, low holding temperatures close to the eutectic temperature and long holding times are the best heat treatment strategies in order to improve wear resistance and hardness of Ti-alloyed hypereutectic HCCI. / <p>QC 20121130</p>

In the constant pursuit of better-performing cemented carbides, recent studies suggest that a combination of better hardness and toughness can be obtained by changing its WC grain size distribution. As the area is still rather unexplored, this  thesis  aims  to  broaden  the  knowledge  and  answer  whether mechanical properties can be changed by changing the WC grain size distribution, in the context of mining drill bit inserts. This was performed by producing four dual grained material as well as four single grained reference materials, for which the carbon content and presence of alloying element were varied. The materials were characterised and compared with regard to magnetic saturation, magnetic coercivity,  hardness,  fracture  toughness,  wear resistance,  energy  needed  to cause  fracture,  as  well  as  detailed microstructural  analysis  obtained  through imaging and electron backscatter diffraction analysis The results showed that mining drill bit inserts with alternative WC grain size distribution  could  successfully  be  produced,  but  that  a  traditional  bimodal distribution  with  two  peaks  could  not  be  obtained.  The  distribution instead became significantly wider as well as skewed towards larger grains for the dual grained materials compared with their references. It was further also confirmed that the alternative dual grain size distribution could be used to improve the mechanical properties of fracture toughness and wear resistance, but only for material that was not alloyed, and the magnitude of the improvement may be considered  to  be  small.  For  the  alloyed  materials,  it  turned  out  to  be more difficult to influence the mechanical properties, as the improving effect of analloying element outweighed the effect of grain size distribution. / I en ständig jakt på hårdmetall med bättre prestanda, så föreslår ny forskning att en bättre kombination av hårdhet och seghet kan erhållas genom att ändra den mikrostrukturiella  WC-kornstorleksfördelning.  Då  det  ännu  är  ett relativt outforskat område, så har denna studie för avsikt att öka kunskapen genom att besvara frågan om de mekaniska egenskaperna kan förändras genom att ändra på materialets kornstorleksfördelning inom applikationsområdet hårdmetall för bergborrning. Detta gjordes genom att producera fyra material med WC pulver av två olika storlekar, samt fyra referensmaterial med en kornstorlek. För dessa varierades parametrarna kolhalt och närvaro av legeringselement. Materialen karakteriserades och jämfördes med avseende på magnetisk mättnad, magnetisk koercivitet, hårdhet,  brottseghet,  slitstyrka,  energi  som  behövs  för  att  orsaka brott, samt  en  detaljerad  mikrostrukturanalys  som  erhölls  genom  avbildning samt elektrondiffraktionsanalys. Resultaten visade att material med alternativ WC-kornstorleksfördelning kunde produceras, men att en fullt bimodal fördelning inte gick att skapa i denna studie. Fördelningen blev istället betydligt bredare samt förskjuten mot större korn för materialen som innhöll WC av två olika storlekar. Det bekräftades också att den alternativa     kornstorleksfördelningen     kunde     förbättra     de     mekaniska egenskaperna för brottseghet och slitstyrka, men endast för de material som inte var legerade och storleken på förbättringen får dessutom anses vara relativt liten. För de legerade materialen visade det sig vara svårare att påverka de mekaniska egenskaperna,  eftersom  den  förbättring  av egenskaper  som  legeringselement tillförde överträffade effekten av kornstorleksfördelning.

Neste trabalho foi medida a tenacidade à fratura de quatro ligas fundidas com composição química base do aço AISI M2 – uma de composição química convencional (liga I), e as demais modificadas por adições de nitrogênio (liga II), cério (liga III) e antimônio (liga IV) – submetidas a tratamentos térmicos visando a decomposição do carboneto M2C, a esferoidização e engrossamento dos carbonetos produto M6C e MC, em altas temperaturas e por diversos tempos. A metodologia empregada nesta avaliação da tenacidade à fratura foi a dos corpos de prova curtos com entalhe chevron segundo ASTM E 1304-97, de forma a superar a necessidade do pré-trincamento por fadiga, procedimento de difícil controle e custoso em materiais como os aços rápidos temperados e revenidos. Verificou-se que a metodologia utilizada para obtenção e ensaio de corpos de prova chevron foi de fácil execução (comparada à metodologia convencional) permitindo grande número de experimentos. Para verificar a consistência dos resultados, em algumas condições, também se utilizou a metodologia convencional segundo a ASTM E 399-90, cujo pré-trincamento foi feito utilizando os procedimentos propostos por Harris e Dunegan. Os resultados obtidos para os aços fundidos foram correlacionados com os obtidos para outros aços rápidos convencionais (VM2, M2 Thyssen) e um aço rápido sinterizado (SINTER 23). A microestrutura foi caracterizada utilizando-se técnicas de ataques metalográficos diferenciais, metalografia quantitativa manual e computadorizada e microscopia eletrônica de varredura. A avaliação microestrutural indica que não ocorreu precipitação eutética do carboneto M6C, em nenhuma das ligas fundidas. O carboneto M2C apresenta morfologia tanto irregular (plaquetas – tipo 1) quanto regular-complexa (lamelas – tipo 2). As ligas I, III e IV, apresentaram a predominância da morfologia tipo 1 enquanto que a liga II modificada pelo nitrogênio, apresentou apenas a morfologia tipo 2. O carboneto MC apresentou-se com morfologia regular-complexa. Medidas do espaçamento interdendrítico indicam que não houve influência significativa dos elementos modificadores sobre este parâmetro. Ensaios de resistência à flexão, indicam pouca influência dos elementos modificadores, mas forte influência dos tratamentos térmicos sobre o limite de resistência à ruptura transversal do aço fundido. Em todas as ligas, a resistência à flexão cresceu com o tempo de tratamento a 1200°C, bem como com a temperatura de decomposição em tratamentos por 2 horas. Análise das fraturas por microscopia eletrônica de varredura indicou que o crescimento das trincas se deu na região interdendrítica. O aço convencional apresentou resistência à ruptura transversal muito superior à dos aços fundidos. Os ensaios de tenacidade à fratura apresentaram resultados compatíveis com a literatura para os aços AISI M2 convencional e SINTER 23. Os resultados obtidos para o aço fundido, indicam queda nos valores de tenacidade à fratura nos materiais tratados a 1050°C com o avanço do tempo de tratamento; pouca variação dos valores com o tempo nas amostras tratadas a 1150°C; e aumento significativo da tenacidade à fratura com o tempo de tratamento a 1200°C. Os valores de tenacidade obtidos para os aços rápidos fundidos foram mais elevados que os obtidos para os materiais trabalhados e para o material sinterizado. / Fracture Toughness of four cast alloys with chemical composition based on the High-Speed Steel AISI M2 were measured. One of the alloys (alloy I) had the conventional AISI M2 composition, while the other three were modified by the addition of N (alloy II), Ce (alloy III) and Sb (alloy IV). The cast alloys were heat-treated in order to promote the decomposition of the M2C carbide as well as spheroidize and coarsen the product M6C e MC carbides. The method chosen for measuring fracture toughness was based on the use of short rod and bar chevron notched samples, according to ASTM E1304 – 97, in order to evade the need for fatigue pre-cracking, notoriously difficult for High Speed Steels quenched and tempered. The chevron-notch method proved straightforward and allowed for successful testing a great number of specimens. Conventional compact sample fracture toughness, according to ASTM E 399-90, with pre-cracking obtained using Harris-Dunegan drop-weight procedure, was used to validate the results. The results for cast alloys were compared with conventionally produced High Speed Steels (VM2, M2 Thyssen) and with a powder metallurgy High Speed Steel (SINTER 23). Microstructural characterization was performed using selective etching of polished surfaces, manual and automated quantitative metallography and SEM. Microstructural evaluation of as-cast alloys showed that there was no eutectic precipitation of M6C carbides. The M2C carbides show an irregular eutectic morphology (Type 1- plates) as well as a regular-complex eutectic morphology. Measurements of interdendritic spacing did not detect any effect of the modification. The bending test rupture strengths did not vary with the addition of modifying elements, but increased with the time and temperature of decomposition, spheroidization and coarsening of carbides. Rupture strengths increased with the heat-treatment time at 1200°C as well as with increasing temperatures for 2 h heat-treatments. SEM examination of the fracture surfaces showed that crack preferential growth path was interdendritical. Conventional High Speed Steels tested in bending presented better results for the rupture strength than cast steels. Fracture toughness results for M2 conventional steels and for the SINTER 23 steel were similar to the results from the literature. Fracture toughness results obtained for cast steels diminished with increasing decomposition time at 1050°C, did not change much with increasing decomposition time at 1150°C, increased markedly withy increasing decomposition times at 1200°C. The fracture toughness results for the as-cast steels were higher than the results obtained for the wrought steels and for the powder metallurgy steel.

Ett företag som tillverkar hydrauliska snabbkopplingar har genom regelbundna kvalitetsprover upptäckt att vissa låskulor till snabbkopplingarnas låsmekanism plötsligt fått en bristande kvalité och spricker vid belastning. Låskulorna är gjorda av rostfritt stål och har en viktig funktion i låsmekanismen. Om de spricker vid användning kan det leda till konsekvenser med materiella skador eller personskador. Företaget vill förekomma eventuella kvalitetsproblem och måste därför säkerställa att låskulorna har rätt hållfasthet. Låskulorna köps in från en underleverantör och företaget vill därför utveckla en provmetod som provar låskulornas materialegenskaper när de levereras till fabriken. Arbetet i denna rapport syftar till att hjälpa företaget utveckla en sådan provmetod. Ett första steg är att undersöka orsaken till att låskulorna spricker. Materialanalyser utförs av ett materiallaboratorium för att fastställa vilka faktorer i materialet som orsakar brott i låskulorna. Analyserna visar att låskulorna sannolikt spricker på grund av en ökad sprödhet i materialet. Sprödheten beror på att martensiten i materialet är dåligt anlöpt samt en stor mängd karbider. Med orsaken till sprickorna fastställd undersöks befintliga metoder för materialprovning. En provmetod måste prova materialet i färdigtillverkade låskulor eftersom låskulornas tillverkningsprocess påverkar materialegenskaperna. Många av de standardiserade provmetoderna är dock svåra att tillämpa på låskulorna med anledning av låskulornas geometri och små dimensioner. En form av slagprov och pressprov utförs på låskulorna. Ett av syftena med proven är att undersöka om de är lämpliga att använda som provmetod. Genom proven framträder olika materialegenskaper för olika låskulor. Resultaten är dock inte jämförbara låskulorna emellan och proven anses inte vara lämpliga som provmetod. Även ett utmattningsprov utförs på låskulorna genom en upprepande belastning i en snabbkoppling. Detta prov är inte heller lämpligt att använda som provmetod då provet är mycket tidskrävande samt att det finns vissa osäkerheter kring provresultatet. I detta arbete undersöks även två nyligen framtagna provmetoder för kulor till kullager och möjligheten att tillämpa dessa provmetoder på låskulorna. I undersökningen jämförs de båda provmetoderna med avseende på utförande samt framtagning av provkropp. Även en spänningsanalys av en låskula belastad i en snabbkoppling utförs för att ta reda på i vilket område av låskulan de maximala spänningarna uppstår. Undersökningen ger att enbart en provmetod är intressant för fortsatt arbete.   Den provmetod som föreslås i detta arbete kallas "the notched ball test" (NBT). Provmetoden innebär att en djup och smal skåra bearbetas i en låskula som sedan belastas med en tryckande kraft vinkelrätt mot skåran tills brott uppstår. Den maximala spänningen som verkar vid brottet beräknas med en enkel ekvation och används som mått för låskulans hållfasthet. Provmetoden är lämplig då den går att utföra med befintlig utrustning på företaget, den provar materialet i färdigtillverkade låskulor samt i samma område som de maximala spänningarna i en låskula belastad i en snabbkoppling uppstår. NBT nyttjar även dragspänningar vilket är fördelaktigt när sprödhet ska upptäckas i ett material. För att fastställa hur olika materialegenskaper samt geometrier för provkroppen påverkar provresultaten utförs en djupare analys av provmetoden. Analysen ger även vilka geometrier som bör användas vid utförandet av NBT samt värdet för den konstant som används vid beräkning av brottspänningen. Praktiska prov av NBT utförs inte i detta arbete men rapporten innefattar slutsatser om provmetoden och rekommendationer till företaget hur ett fortsatt arbete med NBT kan utföras. / A company that manufactures hydraulic quick-couplings has discovered through regular quality checks that the quality of some of the locking balls for the locking mechanism in the quick couplings suddenly has become insufficient and the locking balls rupture under load. The locking balls are made of stainless steel and if they rupture during usage the consequences can be material damage or even personal injury. The company wants to prevent any quality problems and must therefore ensure that the strength of the locking balls is sufficient. The locking balls are purchased from a subcontractor and the company would therefore like to develop a method for strength testing locking balls delivered to the factory. This thesis aims to help the company in developing such a method.  A first step is to investigate the cause of the locking balls rupture. Material analyses are executed by a material laboratory in order to determine what features in the material that causes the ruptures. The analyses shows that rupture is probably caused by an increased brittleness in the material and the brittleness is a consequence of less tempered martensite and a high amount of carbides. With the cause of rupture determined, existing methods for testing material properties is studied. It is important that strength testing is carried out with test specimens prepared from the actual locking balls. Otherwise the influence of the locking balls manufacturing process on the material properties is not taking into account. Many of the standardized methods for testing material properties, however, are hard to apply to the locking balls due to the geometry and small dimensions of the locking balls. A kind of impact test and compression test is performed. One of the purposes with the tests is to investigate if they are adequate for strength testing the locking balls. The results of the tests, however, are not suitable for comparison. Also, a fatigue test of the locking balls is performed by a repetitive loading of a quick coupling. The fatigue test is, however, time consuming and there are uncertainties in the test results. None of these tests is considered suitable as a strength testing method. In this thesis, two recently developed methods for strength testing ceramic balls and the possibility to apply these methods on the locking balls is studied. The study includes an analysis of the stress distribution in a locking ball under load to determine in which region the highest stresses occur. The study provides that only one of the methods is suitable for the locking balls due to differences in preparing the test specimen and which region of the locking ball that is tested in each method. The strength testing method that is proposed in this thesis is called the notched ball test (NBT). In NBT a long and narrow notch is cut in a locking ball which is then loaded in compression perpendicular to the notch until rupture occurs. The maximum stress acting at the rupture is calculated and used to determine the strength of the locking ball. NBT is suitable because it can be performed with existing equipment at the company, the test specimen is prepared from actual locking balls and the test uses tensile stresses which is an advantage when brittleness is to be detected in a material. An analysis of NBT is performed to determine how material properties and different notch geometries is affecting the test results. The analysis also gives some recommendations for notch geometries that should be used when performing NBT as well as a constant that is used when calculating the maximum stress. Practical experiments of NBT are not carried out in this thesis. Instead, conclusions regarding NBT and recommendations for the company on how they should proceed with NBT are given.

Les aciers bainitiques sont utilisés industriellement pour leur bon compromis entre résistance, ductilité et ténacité. Cependant, après obtention de sa microstructure d'emploi, l’acier peut subir des maintiens additionnels en température (soit en fin de fabrication et/ou lors de son utilisation), susceptibles de dégrader ses propriétés. Ces travaux de thèse cherchent à comprendre les origines microstructurales de cette dégradation. Pour ce faire, des traitements thermiques contrôlés ont été appliqués à des aciers de nuances modèles FeNiC et FeNiMnC. Une première série de traitements a permis de fabriquer des microstructures bainitiques supérieure, inférieure, martensitique et mixtes. Ces produits de transformation bruts ont été caractérisés et analysés en détail, en particulier par EBSD en résolution angulaire améliorée. Les données ont été exploitées pour reconstruire les ex-grains austénitiques et distinguer les différents produits de transformation par l'organisation spatiale de leurs variants cristallographiques. Une deuxième série de traitements a consisté à soumettre ces microstructures à des maintiens isothermes prolongés. Nous avons montré que ces microstructures bainitiques en lattes ne sont pas stables dans certaines conditions ultérieures de maintien isotherme. Dans les cas les plus sévères, nous avons observé un processus de « granularisation » de la microstructure en lattes avec disparition des variants fortement désorientés et une maturation des carbures. Ces phénomènes sont observés sur nos alliages modèles y compris sur des temps courts (<1h) à basses températures (300°C). Ces évolutions ainsi que leurs cinétiques ont été investiguées à différentes échelles en couplant des observations en MEB, EBSD, MET et aussi in situ par DRX Haute Energie sur grands instruments. La composition chimique et la microstructure initiale affectent sensiblement les cinétiques. Mais nous avons surtout pointé le rôle majeur de la présence (même résiduelle) de bainite dite supérieure dans la microstructure initiale pour amorcer le processus de granularisation, indépendamment de la température de dénaturation. L’ensemble des résultats permet de discuter les possibles mécanismes sous-jacents et leurs forces motrices et ouvre une discussion plus large sur la classification des bainites / Bainitic steels are widely used in industry thanks to their good combinations of strength, toughness and ductility. Meanwhile, after obtaining the targeted microstructure, the steel can undergo additional isothermal holdings (either during manufacturing and/or during usage) prone to degrade its properties. The thesis work aims at understanding the microstructural origins of this degradation. To achieve this, we applied controlled heat treatments on model FeNiC and FeNiMnC steel grades. A first set of heat treatments allowed us to obtain different microstructures; upper and lower bainites, martensite and mixed concepts. These transformation products were characterized and analyzed in detail, particularly by EBSD with improved angular resolution. Data was operated to reconstruct prior austenitic grains and to distinguish the different transformation products according to their crystallographic variant spatial organization. A second set of heat treatments consisted in aging these microstructures by extended isothermal holdings. We show that lath-like bainitic microstructures are not stable under certain isothermal conditions. In the most advanced cases, we observed a « granularization » process of the lath microstructure, associated with high misoriented variant disappearance and carbides ripening. These phenomena were observed for the studied model alloys, even within short holding times (<1h) and at low temperatures (300°C). These highlighted evolutions as well as their kinetics were investigated at different scales, coupling SEM observations, EBSD, TEM and in situ XRD High Energy on large instruments. The initial microstructure and the steel chemical composition affect significantly the « granularization » kinetics. But we have above all put the light on the major role of the presence of an upper bainite fraction (even a residual one) in the initial microstructure, to start the granularization phenomenon, independently of aging temperature. All of these results allow discussing possible mechanisms with their respective driving forces and opening larger discussion about bainite classification

Made available in DSpace on 2014-10-09T12:51:50Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:08:58Z (GMT). No. of bitstreams: 0 / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Made available in DSpace on 2014-10-09T12:51:50Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:08:58Z (GMT). No. of bitstreams: 0 / Zircônia 3YTZP apresenta propriedades excelentes à temperatura ambiente, mas estas propriedades são afetadas pelo aumento da temperatura pois esta age negativamente sobre o mecanismo de transformação de fase induzida por tensão, que fortalece a tenacidade da matriz. A adição de Si3N4 e SiC em uma matriz de 3YTZP é muito interessante porque conduz à formação de oxinitreto de silício, melhorando as propriedades mecânicas tais como dureza e tenacidade, mas esta adição está limitada por várias dificuldades que se apresentam durante o processamento e sinterização destes materiais. Neste trabalho foi estudada a obtenção, por sinterização sem pressão, do compósito Y-TZP/Si2N2O, partindo-se da adição de 20vol%Si3N4-SiC em uma matriz de zircônia dopada com 3mol% de Y2O3 - 3YTZP, utilizando-se Al2O3 e Y2O3 como aditivos de sinterização. A mistura foi moída e moldada por prensagem isostática a frio. Amostras foram sinterizadas a 1500º, 1600º e 1700ºC por 2h sem pressão e em atmosfera ambiente, utilizando-se um leito de nitreto de silício. Após sinterização, as amostras foram caracterizadas por difração de raios-X. Foram medidas a densidade, tenacidade, dureza e resistência mecânica à flexão em temperatura ambiente. A estrutura do material foi observada em microscopia eletrônica de varredura e de transmissão, com mapeamento químico, para verificar a homogeneidade e morfologia das fases do compósito. A formação de Si2N2O foi observada no material sinterizado devido à reação entre os pós adicionados. O material obtido apresentou aumento de tenacidade e dureza com o aumento de temperatura de sinterização. As amostras apresentaram boa resistência à oxidação a 1000ºC. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Neste trabalho foi medida a tenacidade à fratura de quatro ligas fundidas com composição química base do aço AISI M2 – uma de composição química convencional (liga I), e as demais modificadas por adições de nitrogênio (liga II), cério (liga III) e antimônio (liga IV) – submetidas a tratamentos térmicos visando a decomposição do carboneto M2C, a esferoidização e engrossamento dos carbonetos produto M6C e MC, em altas temperaturas e por diversos tempos. A metodologia empregada nesta avaliação da tenacidade à fratura foi a dos corpos de prova curtos com entalhe chevron segundo ASTM E 1304-97, de forma a superar a necessidade do pré-trincamento por fadiga, procedimento de difícil controle e custoso em materiais como os aços rápidos temperados e revenidos. Verificou-se que a metodologia utilizada para obtenção e ensaio de corpos de prova chevron foi de fácil execução (comparada à metodologia convencional) permitindo grande número de experimentos. Para verificar a consistência dos resultados, em algumas condições, também se utilizou a metodologia convencional segundo a ASTM E 399-90, cujo pré-trincamento foi feito utilizando os procedimentos propostos por Harris e Dunegan. Os resultados obtidos para os aços fundidos foram correlacionados com os obtidos para outros aços rápidos convencionais (VM2, M2 Thyssen) e um aço rápido sinterizado (SINTER 23). A microestrutura foi caracterizada utilizando-se técnicas de ataques metalográficos diferenciais, metalografia quantitativa manual e computadorizada e microscopia eletrônica de varredura. A avaliação microestrutural indica que não ocorreu precipitação eutética do carboneto M6C, em nenhuma das ligas fundidas. O carboneto M2C apresenta morfologia tanto irregular (plaquetas – tipo 1) quanto regular-complexa (lamelas – tipo 2). As ligas I, III e IV, apresentaram a predominância da morfologia tipo 1 enquanto que a liga II modificada pelo nitrogênio, apresentou apenas a morfologia tipo 2. O carboneto MC apresentou-se com morfologia regular-complexa. Medidas do espaçamento interdendrítico indicam que não houve influência significativa dos elementos modificadores sobre este parâmetro. Ensaios de resistência à flexão, indicam pouca influência dos elementos modificadores, mas forte influência dos tratamentos térmicos sobre o limite de resistência à ruptura transversal do aço fundido. Em todas as ligas, a resistência à flexão cresceu com o tempo de tratamento a 1200°C, bem como com a temperatura de decomposição em tratamentos por 2 horas. Análise das fraturas por microscopia eletrônica de varredura indicou que o crescimento das trincas se deu na região interdendrítica. O aço convencional apresentou resistência à ruptura transversal muito superior à dos aços fundidos. Os ensaios de tenacidade à fratura apresentaram resultados compatíveis com a literatura para os aços AISI M2 convencional e SINTER 23. Os resultados obtidos para o aço fundido, indicam queda nos valores de tenacidade à fratura nos materiais tratados a 1050°C com o avanço do tempo de tratamento; pouca variação dos valores com o tempo nas amostras tratadas a 1150°C; e aumento significativo da tenacidade à fratura com o tempo de tratamento a 1200°C. Os valores de tenacidade obtidos para os aços rápidos fundidos foram mais elevados que os obtidos para os materiais trabalhados e para o material sinterizado. / Fracture Toughness of four cast alloys with chemical composition based on the High-Speed Steel AISI M2 were measured. One of the alloys (alloy I) had the conventional AISI M2 composition, while the other three were modified by the addition of N (alloy II), Ce (alloy III) and Sb (alloy IV). The cast alloys were heat-treated in order to promote the decomposition of the M2C carbide as well as spheroidize and coarsen the product M6C e MC carbides. The method chosen for measuring fracture toughness was based on the use of short rod and bar chevron notched samples, according to ASTM E1304 – 97, in order to evade the need for fatigue pre-cracking, notoriously difficult for High Speed Steels quenched and tempered. The chevron-notch method proved straightforward and allowed for successful testing a great number of specimens. Conventional compact sample fracture toughness, according to ASTM E 399-90, with pre-cracking obtained using Harris-Dunegan drop-weight procedure, was used to validate the results. The results for cast alloys were compared with conventionally produced High Speed Steels (VM2, M2 Thyssen) and with a powder metallurgy High Speed Steel (SINTER 23). Microstructural characterization was performed using selective etching of polished surfaces, manual and automated quantitative metallography and SEM. Microstructural evaluation of as-cast alloys showed that there was no eutectic precipitation of M6C carbides. The M2C carbides show an irregular eutectic morphology (Type 1- plates) as well as a regular-complex eutectic morphology. Measurements of interdendritic spacing did not detect any effect of the modification. The bending test rupture strengths did not vary with the addition of modifying elements, but increased with the time and temperature of decomposition, spheroidization and coarsening of carbides. Rupture strengths increased with the heat-treatment time at 1200°C as well as with increasing temperatures for 2 h heat-treatments. SEM examination of the fracture surfaces showed that crack preferential growth path was interdendritical. Conventional High Speed Steels tested in bending presented better results for the rupture strength than cast steels. Fracture toughness results for M2 conventional steels and for the SINTER 23 steel were similar to the results from the literature. Fracture toughness results obtained for cast steels diminished with increasing decomposition time at 1050°C, did not change much with increasing decomposition time at 1150°C, increased markedly withy increasing decomposition times at 1200°C. The fracture toughness results for the as-cast steels were higher than the results obtained for the wrought steels and for the powder metallurgy steel.