MoSiB alloys show promise as the next-generation turbine blade material due to their high-temperature strength and oxidation resistance afforded by a protective borosilicate surface layer. Powder processing and reactive synthesis of these alloys has proven to be a viable method and offers several advantages over conventional melt processing routes. Microstructures obtained have well-dispersed intermetallics in a continuous matrix of molybdenum solid-solution (Mo-ss). However, bend testing of pure Mo and Mo-ss samples has shown that, while the powder processing route can produce ductile Mo metal, the hardening effect of Si and B in solid-solution renders the matrix brittle. Testing at elevated temperatures (200°C) was performed in order to determine the ductile-to-brittle transition temperature of the metal as an indication of ductility. Methods of ductilizing the Mo-ss matrix such as annealing and alloying additions have been investigated.

Mo-Si-B alloys are a leading candidate for the next generation of jet turbine engine blades and have the potential to raise operating temperatures by 300-400°C. The alloys of interest are a three-phase mixture of the molybdenum solid solution (Moss) and two intermetallic phases, Mo3Si (A15) and Mo5SiB2 (T2). A novel powder metallurgical method was developed which uses the reaction of molybdenum, silicon nitride (Si3N4) and boron nitride (BN) powders to synthesize a fine dispersion of intermetallics in a Moss matrix. The covalent nitrides are stable in oxidizing environments up to 1000ºC, allowing for fine particle processing. The process developed uses standard powder processing techniques to create Mo-Si-B alloys in a less complex and expensive manner than previously demonstrated. This powder metallurgy approach yields a fine dispersion of intermetallics in the Moss matrix with average grain sizes of 2-4μm. Densities up to 95% of theoretical were attained from pressureless sintering at 1600°C and full theoretical density was achieved by hot-isostatic pressing (HIP). Sintering and HIPing at 1300°C reduced the grain sizes of all three phases by over a factor of two. Microstructure examination by electron back-scatter diffraction imaging was used to precisely define the location of the phases and to measure the volume fractions and grain size distributions. Microstructural quantification techniques including two-point correlation functions were used to quantify microstructural features and correlate the BN reactant powder size and morphology to the distribution of the intermetallic phases. High-temperature tensile tests were conducted and yield strengths of 580MPa at 1100°C and 480MPa at 1200°C were measured for the Mo-2Si-1Bwt.% alloy. The yield strength of the Mo-3Si-1Bwt.% alloy was 680MPa at 1100°C and 420MPa at 1300°C. A review of the pertinent literature reveals that these are among the highest yield strengths measured for these compositions. The oxidation resistance in air at 1000 and 1100°C was examined. The protective borosilicate surface layer formed quickly due to the close spacing of intermetallic particles and pre-oxidation treatment was developed to further limit the transient oxidation behavior. An oxidation model was developed which factors in the different stages of oxidation to predict compositions that minimize oxidation.

No / Alpha phase sintering, sinter hardening, and mechanical properties of prealloyed Fe-1.5Mo base powder with and without additions of elemental Si, ferrosilicon, and carbon under various process conditions have been investigated. Liquid paraffin, as a new lubricating agent, was found to be useful in reducing segregation, interparticle and die wall frictions, as well as reducing ejection forces and die and tool wear. It was found that addition of Si to the base powder enhanced the sintering process by stabilisation of the ¿-phase and formation of two kinds of liquid phase at ~1045 and ~1180°C, corresponding to the solidus and liquidus temperatures, respectively. This addition increased the tensile strength of the as sintered Fe-1.5Mo from 174 to 445 MPa owing to massive solid solution strengthening effect of Si. An optimum sinter hardenable alloy, of composition Fe-1.5Mo + 3Si + 1.2C, provided a high sintered density of 7.55 g cm-3, tensile and bend strengths of 764 and 1405 MPa, respectively, with 2.5% elongation, after sintering at 1250°C for 1 h under hydrogen or vacuum using moderate cooling rates of ¿ 20 K min-1. Faster cooling rates caused brittleness and very low UTS for the high carbon steel. Full heat treatment improved the UTS by 200 MPa which was useful only for the high carbon steel with high cooling rates ¿ 30 K min-1. Depending on the cooling rate, the as sintered microstructures consisted of mainly fine or coarse pearlite, bainite, martensite, and some retained austenite with hardness in the range 250-720 HV10. Some proeutectoid grain boundary cementites were also present in the as sintered high carbon steel. This work, therefore, has shown that high densities with acceptable microstructures and good mechanical properties are achievable with single stage compaction and single sintering operations by using the optimum process conditions and alloying composition without the need for a post-sintering heat treatment.

Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2016-11-11T17:33:21Z No. of bitstreams: 0 / Made available in DSpace on 2016-11-11T17:33:21Z (GMT). No. of bitstreams: 0 / O desenvolvimento de sistemas laser com pulsos ultracurtos trouxe a possibilidade de usinagem de estruturas muito pequenas em praticamente qualquer tipo de material. Neste trabalho foi dada continuidade a estudos já iniciados no Centro de Lasers e Aplicações (CLA) com os materiais dielétricos, introduzindo a largura temporal dos pulsos laser como mais uma variável e utilizando os conhecimentos adquiridos para a determinação de limiares de ablação e parâmetros de incubação em alguns metais como: aço AISI 1045, aço inoxidável VI138, cobre eletrolítico e molibdênio. A ausência de calor no processo de ablação dos metais torna-se muito difícil, pois a criação de uma camada de íons é muito prejudicada pela mobilidade eletrônica ao seu redor. Assim a ablação de metais com pulsos ultracurtos, tem como principal mecanismo a explosão de fase associada a outros processos que também contribuem na ablação, porém em menor escala, como a explosão coulombiana e a fusão ultrarrápida. Além disso, propriedades como a constante de acoplamento elétron-fônon e a condutividade térmica assumem um papel importante e devem ser levadas em conta na investigação do processo de ablação dos metais. Este trabalho possibilitou a obtenção de parâmetros de operação nos quais o calor transferido para a rede é minimizado, possibilitando a microusinagem de precisão e alterações controladas na morfologia da superfície de diversos metais. Os resultados propiciaram assim condições para novos desenvolvimentos e aplicações práticas de usinagem com pulsos ultracurtos. / Tese (Doutorado em Tecnologia Nuclear) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Submitted by Marco Antonio Oliveira da Silva (maosilva@ipen.br) on 2017-11-01T17:11:09Z No. of bitstreams: 0 / Made available in DSpace on 2017-11-01T17:11:09Z (GMT). No. of bitstreams: 0 / Este trabalho tem por objetivo estudar as propriedades mecânicas e a caracterização microestrutural de espécimes da liga de Co-Cr-Mo obtidos por manufatura aditiva fusão seletiva a laser (do inglês Selective Laser Melting SLM) e por fundição de precisão, visando a confecção de próteses odontológicas. A partir de pós de Co-Cr-Mo atomizados a gás foram realizadas as seguintes etapas: 1) investigação das propriedades físicas, químicas e térmicas dos pós atomizados em diferentes faixas granulométricas (denominadas: D1 < 15 &mu;m, D2 de 20-50 &mu;m e D3 > 75 &mu;m); 2) confecção de espécimes, em dimensões padronizadas, por meio das técnicas de consolidação; 3) caracterização dos consolidados por análise de: citotoxicidade, porosidade, difração de raios X e dilatometria; 4) caracterização mecânica de tração, flexão em três pontos, dureza (macro e micro Vickers) e caracterização microestrutural (microscopia óptica e eletrônica de varredura). De modo geral, os resultados obtidos foram: a granulometria D2 (20-50 &mu;m) é a que melhor se enquadra nas análises de empacotamento para a consolidação por meio de SLM; a biocompatibilidade das amostras obteve resultado positivo para ambas técnicas de processamento; a avaliação mecânica dos espécimes evidencia que a técnica de fusão seletiva a laser propicia propriedades mecânicas (tensão de escoamento, tensão de ruptura, tensão máxima, alongamento e dureza) superiores as obtidas pela técnica de fundição de precisão; a microestrutura obtida pelo processo SLM é composta por grãos ultrafinos e de elevada homogeneidade química. Conclui-se que, o desenvolvimento do presente estudo evidenciou que na fabricação de componentes odontológicos customizados (coroas) a técnica SLM apresenta qualidade superior quando comparada a fundição de precisão. / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP

Today’s steelmaking industry is highly dependent on steel scrap supply. In order to reduce the greenhouse gas emissions (GHGs) deriving from the steel industry, it is of utmost importance to ensure that high percentages of steel scrap are recycled, reducing the reliance on the traditional ore-based steelmaking, which is significantly more environmentally impactful. To reach this goal, a better steel scrap quality has to be achieved during the sorting process. This thesis work aims to propose an optimized sorting process able to separate the stainless steel scrap from the carbon steel scrap, both obtained in the ferrous fraction after a magnetic separation. This improved sorting process would be able to sort different types of stainless steel scraps according to their alloying content, ensuring a better recovery of chromium, nickel and molybdenum for stainless steel production. This would lead to a considerable reduction of CO2 emissions for the stainless steel production. In addition, an economic benefit could be obtained from the optimized sorting process, obtaining steel scrap of higher quality and thus selling the scrap at higher price. In this thesis work, technological considerations are addressed in order to select the most suitable technology to reach significant improvements in alloy recoveries in steel scrap. An economic and environmental model is then used in order to showcase the possible economic and environmental impacts resulting from the implementation of the proposed optimized sorting process. The results obtained are encouraging, showing that this improved sorting would save high amounts of CO2 emissions deriving from raw materials extraction and production, and showing that good profits can be obtained from the selling of the different stainless steel scrap sorted. In the future, where an increased production of steel is expected, this process would be even more beneficial both for the economy and for the environment. / Dagens stål tillverkningsindustri är starkt beroende av utbudet av stålskrot. För att minska utsläppen av växthusgaser (GHG) från stålindustrin är det av yttersta vikt att säkerställa att höga andelar stålskrot återvinns, vilket minskar beroendet av den traditionella malmbaserade ståltillverkningen, som är betydligt mer miljöpåverkande. För att nå detta mål måste en bättre stålskrotskvalitet uppnås under sorteringsprocessen. Detta examensarbete syftar till att föreslå en optimerad sorteringsprocess som kan separera det rostfria stålskrotet från kolstålsskrotet, båda erhållna i järnfraktionen efter magnetisk separation. Denna förbättrade sorteringsprocess skulle kunna sortera olika typer av rostfritt stålskrot efter deras legeringsinnehåll, vilket säkerställer en bättre återvinning av krom, nickel och molybden för produktion av rostfritt stål. Detta skulle leda till en avsevärd minskning av CO2-utsläppen för produktionen av rostfritt stål. Dessutom skulle en ekonomisk fördel kunna erhållas från den optimerade sorteringsprocesser, att få stålskrot av högre kvalitet och därmed sälja skrotet till ett högre pris. I detta examensarbete behandlas tekniska överväganden för att välja den mest lämpliga tekniken för att uppnå betydande förbättringar av legeringsåtervinning av stålskrot.En ekonomisk och miljömässig modell används sedan för att visa upp de möjliga ekonomiska och miljömässiga effekterna av implementeringen av den föreslagna optimerade sorteringsprocessen. Resultaten som erhålls är uppmuntrande, och visar att denna förbättrade sortering skulle spara stora mängder CO2-utsläpp från råvaruutvinning och produktion, och visar att goda vinster kan erhållas från försäljning av olika sorterade rostfritt stålskrot. I framtiden, där en ökad produktion av stål förväntas, skulle denna process vara ännu mer fördelaktig både för ekonomin och för miljön.