The current work contains experimental and theoretical work about the formation of martensite from the austenitic state of the steel Hardox 450. Simulation of rolling and subsequent quenching of martensitic steel plates requires a model that can account for previous deformation, current stresses and the temperature history, therefore dilatometry experiments were performed, with and without deformation. Two austenitization schedules were used and in the standard dilatometry the cooling rates varied between 5-100 °C/s, in order to find the minimum cooling rate that gives a fully martensitic microstructure. Cooling rates larger than 40°C/s gave a fully martensitic microstructure. The cooling rate of 100 °C/s was used in the deformation dilatometry tests where the uniaxial deformation varied from 5-50 %. The theoretical work involved modelling of the martensite formation and the thermal/transformation strains they cause in the steel. Characterizations were done using light optical microscopy, hardness tests and electron backscatter diffraction technique. The parent austenite grains of the martensitic structure were reconstructed using the orientation relationship between the parent austenite and the martensite. Kurdjumov-Sachs orientation relationships have previously been proven to work well for low-carbon steels and was therefore selected. The standard implementation of the Koistinen-Marburger equation for martensite formation and a more convenient approach were compared. The latter approach does not require the storage of initial austenite fraction at start of martensite formation. The comparison shows that the latter model works equally well for the martensite formation. The results showed that the use of martensite start and finish temperatures calibrated versus experiments for Hardox 450 works better when computing thermal expansion than use of general relations based on the chemistry of the steel. The results from deformation dilatometry showed that deformation by compressive uniaxial stresses impedes the martensite transformation. The simplified incremental model works well for deformation with 5 % and 10 %. However, the waviness in the experimental curve for deformation 50 % does not fit the model due vi to large barrelling effect and the large relative expansion for the material that the sample holders are made of. Crystallographic reconstruction of parent austenite grains were performed on a hot-rolled as-received reference sample and dilatometry samples cooled with 60 °C/s and 100 °C/s. The misorientation results showed that the samples match with the Kurdjumov-Sachs orientation relationship in both hot rolled product and dilatometry samples. When misorientation between adjacent pixels are between 15° and 48°, then the boundary between them was considered as a parent austenite grain. The austenitic grain boundaries of the sample cooled at 100 °C/s is in general identical with the hot rolled sample when considering high angle boundaries (15°-48°). The results from the hardness tests showed that the rolled product exhibits higher hardness as compared to samples cooled by 100 °C/s and 60 °C/s. This can be attributed to the formation of transition-iron-carbides in the hot rolled product due to longer exposure of coiling temperature.

Orientador: Rubens Caram Junior / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-18T19:15:30Z (GMT). No. of bitstreams: 1 TaquireDelaCruz_ManoloMarcial_M.pdf: 61740701 bytes, checksum: 1b0f2cfa983c44d13817437ff955e827 (MD5) Previous issue date: 2011 / Resumo: Em se tratando de biomateriais ortopédicos, as ligas de titânio tipo ß apresentam diversas vantagens em relação às ligas do tipo 'alfa' + ß. Ligas contendo elementos ß estabilizadores são mais interessantes em função da alta resistência mecânica específica, da elevada resistência à corrosão e da excelente biocompatibilidade. Em adição, essas ligas exibem baixo módulo de elasticidade, característica fundamental na fabricação de implantes ortopédicos. O objetivo deste trabalho é a avaliação da estabilidade e metaestabilidade de ligas de Ti tipo ß do sistema Ti-Nb com adições de oxigênio. Amostras com composições Ti-30Nb-xO e Ti-35Nb-xO (x =0,1; 0,25; 0,5) (% em peso) foram preparadas por fusão a arco voltaico, homogeneizadas quimicamente em altas temperaturas, forjadas a quente e finalmente, submetidas a diferentes taxas de resfriamento. Tais amostras foram caracterizadas em relação à microestrutura por meio de microscopia óptica e eletrônica de varredura e de difração de raios-X, enquanto o comportamento mecânico foi avaliado por meio de ensaios de dureza Vickers, de medidas de módulo de elasticidade por meio de técnicas acústicas e de nano-dureza usando a técnica de nano-indentação. Os resultados obtidos indicam que baixas taxas de resfriamento conduzem à microestrutura formada pelas fases 'alfa' e ß e eventualmente, com a precipitação da fase 'omega'. Por outro lado, altas taxas de resfriamento conduziram à formação da estrutura metaestável martensítica 'alfa'. À medida que o teor de oxigênio foi incrementado e sob resfriamento lento, obteve-se a precipitação acentuada de fase 'alfa'. Sob elevadas taxas de resfriamento, o aumento dos teores de O e Nb resultaram na estabilização da fase ß e na redução da fração volumétrica da fase metaestável 'alfa'. As medidas de módulo de elasticidade mostram que em amostras submetidas a baixas taxas de resfriamento, a adição de oxigênio levou ao aumento do módulo de elasticidade. Para todas as taxas de resfriamento estudadas, observou-se que a dureza elevou-se com o aumento do teor de oxigênio, o que está associado à formação de solução sólida intersticial e à precipitação acentuada da fase 'alfa'. / Abstract: In the case of orthopedic biomaterials, ß-type titanium alloys have several advantages compared to the 'alfa'+ß titanium alloys. Alloys containing ß-stabilizing elements are often interesting due to high mechanical strength, high corrosion resistance and superior biocompatibility. Furthermore, due to low elastic modulus, these alloys are promising candidate in the manufacturing of ortophedic implants. The main goal of this work is to study the phase stability and metastability in ß type Ti-Nb alloys with oxygen additions. Samples with concentrations Ti-30Nb-xO and Ti-35Nb-xO (x = 0,1; 0.25 and 0.5) (wt%) were prepared by using an arc melting furnace and homogenized chemically at high temperatures, hot forged and finally, submitted to different cooling rates. These samples were characterized in relation to their microstructure by applying optical microscopy and X-ray diffraction, while the mechanical behavior was evaluated by Vickers hardness tests and elastic modulus measurements using acoustic technique. These results indicate that low cooling rates lead to 'alfa' and ß phase formation and eventually, to 'omega' phase precipitation. On the other hand high cooling rates led to 'alfa' martensitic structure formation. For lower cooling rates, as the oxygen concentration increased, the volume fraction of 'alfa' precipitates increased. At higher cooling rates O and Nb additions had an effective role in enhancing the ß phase stability and in diminishing the volume fraction of 'alfa' martensite phase. It was found that samples submitted to lower cooling rates presented an increase in the elastic modulus values as the oxygen content was increased. It was possible to observe that, for all cooling rates applied, the hardness values increased as the oxygen content was increased. These results are associated with formation of interstitial solid solution and 'alfa' phase precipitation / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica

No presente trabalho, foi realizado um estudo sobre a influência da adição do boro em um aço C-Mn, nas transformações de fases por resfriamento contínuo, através da técnica dilatométrica. Para este estudo, utilizou-se dois aços de composição química semelhante: o aço 10B22 com 30 ppm de boro e o aço sem boro é o E1522, equivalente. Foram traçadas as curvas de CCT dos dois aços, onde analisou-se o efeito de temperabilidade do boro através das curvas de resfriamento. Os materiais foram ensaiados em um dilatômetro de resfriamento rápido, utilizando corpos de prova cilíndricos, resfriados por injeção de ar e hélio. Os resultados gráficos dos processos de resfriamento foram comparados com análises metalográficas ótica estruturais e quantitativas e também por medidas de dureza. Detalhes microestruturais, tais como, contagem de fases formadas em função das taxas de resfriamento, tamanho de grão, distribuição de inclusões e precipitados, foram extraídos, através de um sistema de análise de imagens. Complementando o trabalho, foi realizado uma completa documentação fotográfica das microestruturas, com uma indicação final do tratamento térmico mais adequado aos aços C-Mn microligados ao boro. / This work presents a study about the influence of boron on phase transformation by continuous cooling in a C-Mn steel using the dilatometric technique. For this study two close chemical composition steels were applied: a 10B2 steel with 30 ppm of boron and a E1522 steel without boron. For both steels the CCT curves were obtained, where the effect of boron on hardenability was analysed throughout continuous cooling curves. Both materials were testedcin a high speed quenching dilatometer, using cilindricals samples quenched by helium blow on their surfaces. The graphics results of cooling processes were compared with microstructural and quantitative optical metallographic analysis and hardness measurements. Microstructural features as such phases fraction as a function of cooling rates, grain size, and distributions of inclusions and precipitates were obtained through an image analysis system. In addition, complete microstructural photography documentation was carried out where it was possible to indicate the best heat treatment to boron microalloyed C-Mn steels.

27 Retrieved Yttria Stabilised Tetragonal Zirconia (Y-TZP) femoral heads were studied for the occurrence of tetragonal to monoclinic phase transformation and the effects that such transformation has on the bearing surface. The mean monoclinic percentage found is 53.6% with 25 of the samples having transformed more than 20%. This finding nullifies earlier predictions that it would take 25 to 30 years to transform to a monoclinic content of 30 to 40% inside the human body (Chevalier, Drouin&Calés 1997). It was however shown that Hot Isostatic Pressed (HIP’ed) Y-TZP femoral heads have a better, though still not adequate, resistance to phase transformation in the human body than non-HIP’ed femoral heads. Results of various investigations show that this transformation degrades the surface condition of the femoral heads, which in turn increases wear and subsequently decreases the survival rate of the prosthesis due to a greater risk of aseptic loosening. It is postulated that a great contributing factor to the phase transformation is increased temperatures inside the bearing couple, due to inadequate lubrication between the two bearing surfaces. Tetragonal to monoclinic phase transformation and its associated effects renders Y-TZP femoral heads less attractive for hip replacements. / Dissertation (MEng)--University of Pretoria, 2010. / Mechanical and Aeronautical Engineering / unrestricted

The current work contains experimental and theoretical work about the formation of martensite from the austenitic state of the steel Hardox 450. Simulation of rolling and subsequent quenching of martensitic steel plates requires a model that can account for previous deformation, current stresses and the temperature history, therefore dilatometry experiments were performed, with and without deformation. Two austenitization schedules were used and in the standard dilatometry the cooling rates varied between 5-100 °C/s, in order to find the minimum cooling rate that gives a fully martensitic microstructure. Cooling rates larger than 40°C/s gave a fully martensitic microstructure. The cooling rate of 100 °C/s was used in the deformation dilatometry tests where the uniaxial deformation varied from 5-50 %. The theoretical work involved modelling of the martensite formation and the thermal/transformation strains they cause in the steel. Characterizations were done using light optical microscopy, hardness tests and electron backscatter diffraction technique. The parent austenite grains of the martensitic structure were reconstructed using the orientation relationship between the parent austenite and the martensite. Kurdjumov-Sachs orientation relationships have previously been proven to work well for low-carbon steels and was therefore selected. The standard implementation of the Koistinen-Marburger equation for martensite formation and a more convenient approach were compared. The latter approach does not require the storage of initial austenite fraction at start of martensite formation. The comparison shows that the latter model works equally well for the martensite formation. The results showed that the use of martensite start and finish temperatures calibrated versus experiments for Hardox 450 works better when computing thermal expansion than use of general relations based on the chemistry of the steel. The results from deformation dilatometry showed that deformation by compressive uniaxial stresses impedes the martensite transformation. The simplified incremental model works well for deformation with 5 % and 10 %. However, the waviness in the experimental curve for deformation 50 % does not fit the model due vi to large barrelling effect and the large relative expansion for the material that the sample holders are made of. Crystallographic reconstruction of parent austenite grains were performed on a hot-rolled as-received reference sample and dilatometry samples cooled with 60 °C/s and 100 °C/s. The misorientation results showed that the samples match with the Kurdjumov-Sachs orientation relationship in both hot rolled product and dilatometry samples. When misorientation between adjacent pixels are between 15° and 48°, then the boundary between them was considered as a parent austenite grain. The austenitic grain boundaries of the sample cooled at 100 °C/s is in general identical with the hot rolled sample when considering high angle boundaries (15°-48°). The results from the hardness tests showed that the rolled product exhibits higher hardness as compared to samples cooled by 100 °C/s and 60 °C/s. This can be attributed to the formation of transition-iron-carbides in the hot rolled product due to longer exposure of coiling temperature.

The Bi2Sr2CaCu2O7+d, i.e. Bi2212 phase of bismuth derived high temperature superconductors (HTS), powder precursor were synthesized via sol – gel technique using ethylendiamintetraacetic acid (Chelaton II) as a chelating agent. Metal nitrate’s solutions were mixed with EDTA suspension. The pH value was adjusted to 9 by NH4OH by reason forming of stable metal’s complexes. The mixture was heated to 80 °C for gelation. Solution taken before solid gel was form is used for preparation of Bi2212 layer on to a-Al2O3 surface via spin coating deposition’s technique. Reactive powder used for bulk sample preparation was made by calcination (800 °C) of pyrolyzed xerogel (500 °C). Sintering in oxygen atmosphere was proceeding at temperature from 850 to 880 °C. Bulk sample properties were compared with sample prepared by common ceramic method. Simultaneous TG-DTA, IR spectroscopy and heating microscopy were used for sample characterization. Furthermore, construction of furnace for sintering in O2 atmosphere was described.

In this work phase transformations in metastable β (primarily Ti-15Mo) alloys were studied utilizing electrical resistance, dilatometry, transmission electron microscopy and X-ray and neutron diffraction. The materials Ti-15Mo, Ti-6.8Mo-4.5Fe-1.5Al (LCB), Ti-5Al-5V-5Mo-3Cr (Ti-5553), Ti-29Nb-1Fe-0.5Si (TNFS), Ti-15Mo-3Nb-3Al-0.2Si (Timetal 21S) and Ti-13Cr-1Fe-3Al (TCFA) (in wt. %) - were subjected to a solution treatment at a temperature above β transus and quenched into water. In this condition, the microstructure of the investigated materials consists of β matrix and ω particles. Samples quenched from important temperatures determined from in-situ electrical resistance and dilatometry measurements were studied by post-mortem TEM. In-situ X-ray and neutron diffraction provided direct observations of microstructure of Ti-15Mo alloy during linear heating and confirmed statements based on results of indirect methods, such as: the decrease of volume fraction of ω phase during heating at low temperatures (up to 250 ◦ C), complete dissolution of ω phase at 560 ◦ C and precipitation of α phase without ω particles serving as its direct precursors. X-ray diffraction experiment allowed to determine relative evolution of the size of ω particles while phase fraction evolution was derived from neutron diffraction. The...

[pt] O aço inoxidável hiper duplex UNS S33207 é utilizado na indústria de óleo e gás para operações de poços em águas ultraprofundas devido às suas excelentes propriedades mecânicas e resistência à corrosão. Aços inoxidáveis duplex quando submetidos a ciclos térmicos que atingem temperaturas próximas à temperatura de ferritização seguido de resfriamento rápido, apresentam matriz ferrítica e diferentes morfologias de austenita, como Widmanstätten, alotriomórfica e intragranular, além da precipitação de nitretos de cromo. É importante destacar que no caso de aços inoxidáveis duplex, entre os elementos químicos presentes em solução sólida, o nitrogênio possui extrema importância na formação da fase austenítica. Sendo também responsável pela alta resistência à nucleação de pites. Portanto as atmosferas nas quais são realizados os tratamentos térmicos ou quando ciclos térmicos são aplicados a estes aços, podem ter efeito sobre a dessorção ou absorção de nitrogênio, influenciando assim a resistência à corrosão. Nesta dissertação foi analisado o aço hiper duplex UNS S33207 tanto na condição de como recebido, assim como tratado termicamente nas temperaturas de 1380 graus Celsius e 1390 graus Celsius em quatro atmosferas diferentes: ar atmosférico, argônio, nitrogênio e argônio com 5% de nitrogênio. A caracterização microestrutural foi realizada por microscopia ótica, e eletrônica de varredura (MEV) além de difração de elétrons retro-espalhados (EBSD). Foram também realizados ensaios de dureza, microdureza e teste de corrosão de acordo com a norma ASTM G48. Após o tratamento térmico o balanço entre as fases ferrita e austenita se alterou. Devido à alta taxa de resfriamento, a fase ferrítica se tornou mais abundante na condição de termicamente tratada. A influência das atmosferas se mostrou mais evidente em relação a austenita não dissolvida após o tratamento térmico. As amostras tratadas com atmosferas de nitrogênio apresentaram maior percentual de austenita não dissolvida do que as amostras tratadas em ar atmosférico ou mesmo em argônio puro, estas últimas apresentaram menor percentual de austenita não dissolvida. O teste de corrosão ASTM G48 indicou maior perda de massa nas amostras tratadas termicamente. Dentre estas condições, as que tiveram influência das atmosferas contendo nitrogênio apresentaram melhor resistência a corrosão. Os pites em todas as amostras iniciaram na interface gama /delta com propagação para o interior dos grãos ferríticos. O objetivo principal desta dissertação é correlacionar a influência de diferentes atmosferas na porcentagem das fases transformadas em função tratamentos térmicos nas propriedades de corrosão. / [en] Hyper duplex stainless steel UNS S33207 is used in the oil and gas industry in ultra-deep well operations due to its excellent mechanical properties and corrosion resistance. When stainless steels are subjected to thermal cycles reaching temperatures close to the ferritization temperature, then followed by fast cooling, the microstructure transforms. The ferritic matrix and different austenite morphologies will occur during cooling, such as Widmanstatten, allotriomorphic, and intragranular, in addition to chromium nitride precipitation. It is essential to highlight that for duplex stainless steels, among the chemical elements in solid solution, nitrogen is vital in the austenitic phase precipitation. It is also responsible for the pitting corrosion resistance. Therefore, the atmospheres in which heat treatments are carried out or when thermal cycles are applied to these steels can affect nitrogen desorption or absorption, thus influencing corrosion resistance. In this dissertation, UNS S33207 hyper duplex stainless steel was analyzed in the asreceived condition and as heat-treated at 1380 Celsius degrees and 1390 Celsius degrees in four different atmospheres: atmospheric air, argon, nitrogen and a mixture of argon and 5 percent nitrogen. Microstructural characterization was performed by optical microscopy and scanning electron microscopy (SEM) in addition to electron backscatter diffraction (EBSD). Hardness, microhardness, and ASTM G48 corrosion tests were also performed. After the heat treatment, the balance between the ferrite and austenite phases changed. Due to the fast cooling rate, the ferritic phase became more abundant in the heat-treated condition. The atmosphere influence was more evident on the primary austenite after the heat treatment. The samples heat treated with nitrogen atmospheres presented a higher percentage of primary austenite than the samples heat-treated in atmospheric air, or even in pure argon, the latter gave the lowest fraction of remaining austenite. The ASTM G48 corrosion test indicated a more significant mass loss in the heat-treated samples. Among these samples, those that were heat-treated in atmospheres containing nitrogen presented better corrosion resistance. The pitting in all samples nucleated at the gama / delta interface. The pitting then propagated into the ferritic grains. This dissertation main objective is to correlate the influence of the different atmospheres on the percentage of phases transformed as a function of heat treatments and the effect on corrosion properties.

No description available.

The Reduced Enrichment for Research and Test Reactor (RERTR) now known as the Material Minimization and Management Reactor Control program (MMMRC) seeks to replace the use of highly enriched uranium (HEU) fuels used in research and test nuclear reactors around the world. The low enriched uranium (LEU) fuels must have fissionable uranium densities comparable to the HEU fuels. After extensive investigation by various researchers around the world, the U-Mo alloys were selected as a promising candidate. The Mo alloyed with U allows for the stabilization of the face-centered cubic ?-U phase, which demonstrated favorable irradiation behavior. However, deleterious diffusional interaction between the fuel and the cladding, typically Al-base alloy, remain a challenge to overcome for application of U-Mo alloys as the LEU fuel. Zr has been identified as a potential diffusion barrier between monolithic U-10 wt.% Mo (U10Mo) metallic fuel and AA6061 cladding alloys for the development of a LEU fuel system. However, interdiffusion and reaction between the Zr barrier and U10Mo fuel can produce phases such as Mo2Zr, and promote the destabilization of ?-U phase into ?'-U (U2Mo) and ?-U. In order to better understand this phenomenon, this study examined the phases that are present in the U10Mo alloys with varying Zr concentration, 0, 0.5, 1.0, 2.0, 5.0, 10.0, 20.0 wt.% at room temperature after heat treatment at 900°C for 168 hours and 650°C for 3 hours. These two temperatures are relevant to fuel plate fabrication process of homogenization and hot-rolling, respectively. Scanning electron microscopy and X-ray diffraction were employed to identify and quantitatively document the constituent phases and microstructure to elucidate the nature of phase transformations. For U10Mo alloys containing less than 1.0 wt.% Zr, there was no significant formation of Mo2Zr after 900?C homogenization and subsequent heat treatment at 650?C for 3 hours. The ?-U phase also remained stable correspondingly for these alloys containing less than 1.0 wt.% Zr. For U10Mo alloys containing 2 wt.% or more Zr, a significant amount of Mo2Zr formation was observed after 900?C homogenization and subsequent heat treatment at 650?C for 3 hours. For these alloys, destabilization of ?-U into ?'-U (U2Mo), UZr2 and ?-U was observed. The alloy containing 20 wt.% Zr, however, did not demonstrate ?-U decomposition even though Mo2Zr was observed after heat treatments. The formation of Mo2Zr effectively reduced the stability of the metastable ?-U phase by depleting the ?-stabilizing Mo. The destabilization of ?-U phase into the ?-U phase is not favorable due to anisotropic and poor irradiation behavior of ?-U phase. Therefore the formation of Mo2Zr at the interface between U10Mo fuel and Zr diffusion barrier must be carefully controlled during the fabrication of monolithic LEU fuel system for successful implementation.