The present study investigates the fracture toughness of FSW X-80 HSLA steel welds. Weld cooling rate and peak temperature were varied among welds; indirectly manipulated through FSW travel speed, rpm, and weld preheat. Fracture toughness was tested according to ASTM 1820 standard along the weld centerline using surface-notched SEB specimen cooled to -40 °C. This study resulted in a reliable, repeatable process for generating friction stir welds with CTOD’s consistently above that of the original base metal. CTOD and microstructure of friction stir welds can be selected by controlling weld cooling rate and peak temperature. Material properties and microstructure similar to the original base metal can be recreated throughout the weld stir zone. CTOD of FSW X80 has a strong inverse linear correlation with post-weld cooling rate.

This project mainly investigated how the niobium(Nb) content influences the microstructure and mechanical properties of grey cast iron. Considering the mechanism, the study also analyzes the relationship between microstructure and mechanical properties. Generally, the work is based on 127 test bars/samples from two cylinder heads and three batches of plates, which were studied by measuring tensile strength, microhardness, graphite size, carbide amount and chemistry. The result data has been evaluated with statistical methods. The experiments mainly included the preparation of the samples for test and analysis. The mechanical properties in this study are evaluated by the tensile strength of the grey cast iron. Meanwhile, various microscopies were applied to observe how niobium and cooling rate influence the microstructure. Finally, from the analysis results, it tells that the niobium does affect the tensile strength of grey cast iron. Higher the niobium content is, higher the tensile strength is. The computed result based on the data also shows niobium’s strong effect. The faster cooling rate will increase the tensile strength and pearlite microhardness of grey cast iron as well. The carbide amount of grey cast iron can be increased by the addition of niobium content. Furthermore, some future work needs to be done to explain the unsolved problem in this result. The reasons of why a specific position A-2-d of plates has high values of tensile strength demand more microstructure investigation. For the niobium influence, more experiments and data containing a larger range of niobium content also need to be done to prove the mathematics results in this report. / Detta projekt undersökte huvudsakligen hur innehållet av niob (Nb) påverkar gråstålens mikrostruktur och mekaniska egenskaper. Med tanke på mekanismen analyserar undersökningen även förhållandet mellan mikrostruktur och mekaniska egenskaper. Arbetet baseras i allmänhet på 127 provstänger / prover från två cylinderhuvuden och tre satser av plattor, vilka studerades genom mätning av draghållfasthet, mikrohårdhet, grafitstorlek, karbidmängd och kemi. Resultatdata har utvärderats med statistiska metoder. Experimenten inbegriper huvudsakligen beredningen av proven för test och analys. De mekaniska egenskaperna i denna studie utvärderas av gråstålets draghållfasthet. Under tiden applicerades olika mikroskopier för att observera hur niob- och kylhastigheten påverkar mikrostrukturen. Slutligen, från analysresultaten, berättar den att niobet påverkar draghållfastheten hos grågjutjärn. Ju högre niobinnehållet är, desto högre är draghållfastheten. Det beräknade resultatet baserat på data visar också niobins starka effekt. Den snabbare kylhastigheten ökar också draghållfastheten och pearliten-mikrohårdheten hos grågjutjärn. Karbidmängden av grågjutjärn kan ökas genom tillsats av niobhalt. Vidare måste vissa framtida arbeten göras för att förklara det olösta problemet i detta resultat. Skälen till varför en specifik position A-2-d av plattor har höga dragkrafter kräver mer mikrostrukturundersökning. För niobinpåverkan måste fler experiment och data som innehåller ett större antal niobinnehåll också göras för att bevisa matematikresultaten i denna rapport.

The objective of this research work was to understand the molecular mechanism of gas transport through amorphous glassy polymers. Especially, emphasis was placed on determining whether or not gas transport in amorphous glassy polymers is directly correlated with the free volume content. Free volume arguments are indeed commonly used to explain the gas transport process. The gas transport properties of bisphenol-A polycarbonate films were examined as a function of the cooling rate, physical aging, and orientation. Such conditions affect the free volume content and its size and shape distribution. Results obtained from permeation experiments were accompanied with dynamic mechanical and density measurements. The experimental results suggest that the diffusion coefficient of small gas molecules in glassy polycarbonate is influenced by the local dynamics or mobility of the polymer chains rather than by the overall free volume content. Indeed, the diffusion coefficient of nitrogen for instance was reduced in fast-cooled samples, despite of the fact that those samples possessed a greater overall free volume content. Fast cooling rates may generate highly restricted conformations which hinder local motions, and therefore tend to increase the activation energy of diffusion. As expected, the greater the free volume content, the greater was the solubility coefficient. The increase in the polymer relaxation times with aging time is believed to restrict the local chain motions, leading to enhanced activation energies of diffusion, and therefore to reduced diffusion coefficients. The change in the solubility coefficients with physical aging revealed that the aging process might not affect all the cavity sizes in polycarbonate equally. According to free volume arguments, one would anticipate that the physical aging of fast-cooled samples (which possess more free volume) should be enhanced compared to that of slowly-cooled samples. Quite interestingly, the decrease in the diffusion coefficient with aging was found to occur much slower in fast-cooled samples, despite of the higher initial free volume content. In contrast, properties directly related to the free volume content, such as density or isothermal DMTA measurements actually showed a greater aging rate in the sample containing the greatest amount of free volume. Slow-cooled samples that are in a low energy conformational state may loose their internal degrees of freedom more rapidly, due to the closer interchain packing and the possibly restricted segmental motions. Studies dealing with orientation and gas transport were complicated by several factors. For instance the fact that the permeation experiments were performed perpendicularly to the orientation of the chains and not along the orientation axis limited the sensitivity of the gas transport properties to orientation. This work points out that dynamic rather than static models should be developed to predict the gas transport phenomenon. / Ph. D.

Crystallisation is gaining a lot of interest in pharmaceutical industry to help designing active ingredients with tailored physicochemical properties. Many factors have been found to affect the crystallisation process, including process parameters and material attributes. Several studies in the literature have discussed the role of these parameters in the crystallisation process. A comprehensive study is still missing in this field where all the significant terms are taken into consideration, including the square effect and the interaction terms between different parameters. In this study, a thorough investigation into the main factors affecting crystallisation of a polymeric system, processed via injection moulding, was presented and a sample of response optimisation was introduced which can be mimicked to suite a specific need. Three grades of pure polyethylene oxide; 20K, 200K and 2M, were first characterised using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD) and shear rheometry. The onset of degradation and the rate varied according to molecular weight of polyethylene oxide (PEO). The peak melting temperature and the difference in enthalpy between melting and crystallisation were both in a direct proportion with PEO molecular weight. PEO200K and PEO2M struggle to recrystallise to the same extent of the original state at the tested cooling rates, while PEO20K can retain up to a similar crystallinity degree when cooled at 1 °C/min. Onset of crystallisation temperature (Tc1) was high for PEO2M and the difference between the 20K and 200K were pronounced at low cooling rate (20K is higher than 200K). The rheometer study showed that PEO2M has a solid-like structure around melting point which explains the difficulty in processing this grade at a low temperature via IM. PEO20K was almost stable within the strain values studied (Newtonian behaviour). For higher grades, PEO showed a shear thinning behaviour. The complex viscosity for PEO2M is characterised by a steeper slope compared to PEO200K, which indicates higher shear thinning sensitivity due to higher entanglement of the longer chains. For binary blends of PEO, the enthalpy of crystallisation studied by DSC was in direct proportion to the lowest molecular weight PEO content (PEOL %) in PEO20K/200K and PEO20K/2M blends. The effect of PEOL% on Tc1 became slightly pronounced for PEO20K-2M blends where Tc1 exhibited slight inverse proportionality to PEOL% and it became more significant for PEO200K-2M blends. It was interesting to find that Tc1 for the blends did not necessarily lie between the values of the homopolymers. In all binary blends, Tc1 was inversely proportional to cooling rate for the set of cooling rates tested. Thermal analysis using hot stage polarised light microscopy yields different behaviours of various PEO grades against the first detection of crystals especially where the lowest grade showed highest detection temperature. Visual observation of PEO binary blends caplets processed at various conditions via injection moulding (IM) showed the low-quality caplets processed at mould temperature above Tc1 of the sample. The factors affecting crystallisation of injection moulded caplets were studied using response surface methodology for two responses; peak melting temperature (Tm) and relative change in crystallinity (∆Xc%) compared to an unprocessed sample. Mould temperature (Tmould) was the most significant factor in all binary blend models. The relationship between Tmould and the two responses was positive non-linear at the Tmould ˂ Tc1. Injection speed was also a significant factor for both responses in PEO20K-200K blends. For Tm, the injection speed had a positive linear relationship while the opposite trend was found for ∆Xc%. The interaction term found in the RSM study for all models was only between the injection speed and the PEOL % which shows the couple effect between these two factors. Molecular effect was considered a significant factor in all ∆Xc% models across the three binary blends. The order of ∆Xc% sensitivity to the change in PEOL% was 3, 5 and 7 % for 20K-200K, 200K-2M and 20K-2M.

As velocidades críticas de resfriamento necessárias à obtenção de percentuais definidos de martensita, presentes em amostras de aços temperados em óleo, foram determinadas por meio de curvas de resfriamento. As amostras constituíram-se de barras de aço AISI 4140 e 8640 com seções circulares de 25,4; 38,1 e 50,8 mm e barras quadradas com 25,4 e 38,1 mm de lado e comprimento igual a 5 vezes o diâmetro ou lado. Visando-se à obtenção de padrões de comparação para essas velocidades, foram também obtidas as curvas em U das durezas ao longo das seções transversais das barras e as curvas Jominy desses aços. Os resultados apresentaram boa coerência, o que garantiu a eficiência do processo. Os resultados concernentes ao teor específico de 50% de martensita foram comparados com os obtidos a partir de equações constantes na literatura. As equações não se mostraram diretamente adequadas, requerendo a obtenção de um fator de correção, que uma vez obtido mostrou-se eficiente na adequação dos valores empíricos de velocidade crítica aos determinados por meio das curvas de resfriamento. / The criticaI cooling velocities necessary to obtaining specific contents of martensite, present in test specimens of hardened steels in oil, were evaluated by means of cooling curves. The samples were constituted of bars of AISI 4140 and 8640 steels with 25,4; 38,1 and 50,8 mm diameter and squared bars with 25,4 and 38,1 mm in side by 5 times the diameter or side long. Aiming at obtaining comparison patterns for those velocities, they were also obtained the curves in U of the hardness along the traverse sections of the bars and the Jominy curves of those steels. The results presented good agreement, what guaranteed the efficiency of the process. The concerning results achieving a 50 pct martensitic microstructure were compared with those obtained from equations presented in the literature. The equations did not show good approaches, requesting the determination of a correction factor, that once obtained it was shown efficient in the adaptation of the empirical values of critical velocities to those determined by means of the cooling curves.

Made available in DSpace on 2017-07-21T20:42:45Z (GMT). No. of bitstreams: 1 Tiago Boni Comisso.pdf: 10111078 bytes, checksum: 8216bf27a8a3e1b801b4d8d101212fd8 (MD5) Previous issue date: 2011-10-03 / In the present study the warpage of rotationally molded parts of a linear low density polyethylene (LLDPE) was investigated. The effect of different processing factors as part thickness, cooling condition and diameter of the venting tube was evaluated. In addition to the rotational molding experiments, an alternative experimental technique, denominated “Hot Press”, was also applied to investigate the warpage of two different grades of LLDPE under typical rotational molding conditions, which means slow cooling from only one side. Crystallinity and spherulitic morphology along the thickness of the rotationally molded parts were studied by Differential Scanning Calorimetry and Polarized Light Optical Microscopy. It is shown that the warpage increases with the increase of the cooling rate. Increase of diameter of the venting tube is more effective in reducing the warpage of rotationally molded parts mainly for lower cooling rates. In hot press experiments the grade of LLDPE with lower melt flow index and higher flexural strength presented lower warpage. Part thickness affects the warpage in hot press experiments only for faster cooling rates. In general, crystallinity and spherulitic diameter are lower in positions along the rotationally molded part thickness where the cooling rate is faster. / No presente estudo o empenamento de peças de polietileno linear de baixa densidade (PELBD) moldadas por rotomoldagem foi investigado. O efeito de diferentes fatores como espessura da peça, taxa de resfriamento e diâmetro de tubo de ventilação foi avaliado. Em adição aos experimentos de rotomoldagem, uma técnica alternativa denominada “Hot Press” foi também aplicada para investigar o empenamento de dois diferentes PELBD sob condições típicas da rotomoldagem quanto ao resfriamento assimétrico. Cristalinidade e morfologia esferulítica ao longo da espessura das peças rotomoldadas foram avaliadas por Calorimetria Exploratória Diferencial (DSC) e Microscopia Ótica de Luz Polarizada. Verificou-se que o grau de empenamento aumenta com o aumento da taxa de resfriamento. O aumento do diâmetro do tubo de ventilação é mais efetivo na redução do empenamento principalmente em menores taxas de resfriamento. Nos experimentos de “Hot Press” o PELBD com menor índice de fluidez e maior módulo de flexão apresentou menor empenamento. Nos experimentos de “Hot Press” a espessura das peças afetou o empenamento somente para taxas de resfriamento mais rápidas. Em geral, a cristalinidade e o tamanho de esferulitos se mostraram menores nas posições ao longo da espessura das peças rotomodadas onde as taxas de resfriamento eram mais rápidas.

Este trabalho visa analisar a influência das taxas de resfriamento e temperatura no último passe de laminação a quente de fio máquina de um aço DIN 41Cr4 sobre a microestrutura obtida após a laminação e a sua correlação com aquela resultante do tratamento térmico de esferoidização. Foi avaliado a influência da microestrutura prévia de laminação nos tempos e taxa de resfriamento do tratamento térmico necessários para garantir adequada microestrutura do aço DIN 41Cr4. Foram aplicados conceitos de laminação termomecânica através da variação dos parâmetros: temperatura no último passe de laminação (acabador) e após o último passe de laminação (formador de espiras); velocidade das esteiras do “cooling conveyor” e consequente tempo de permanência das espiras sobre a região de ventiladores e alguns parâmetros no ciclo de tratamento térmico: tempo em patamar e taxa de resfriamento durante a produção de fio máquina redondo de bitolas entre 15,88mm e 16,15mm. A avaliação da resposta às variações impostas ao processo foi realizada através de análises metalográficas de microestrutura no material laminado e no material esferoidizado (grau de esferoidização), descarbonetação e de ensaios de propriedades mecânicas como dureza e tração. A partir dos resultados buscou-se determinar a influência dos parâmetros de laminação na microestrutura do material laminado e a influência desta na resposta ao tratamento térmico de esferoidização. Foram analisadas oito diferentes condições e os resultados mostraram que maiores taxas de resfriamento resultam em microestruturas mais refinadas proporcionando uma simplificação no tratamento térmico, atendendo as propriedades desejáveis no produto final (fio máquina redondo esferoidizado). / This work aims to analyze the influence of the cooling rate, the temperature of the finishing pass and at the coil-forming during hot rolling of DIN 41Cr4 steel wire rod on the microstructure and its influence on plateau times and cooling rate during the spheroidizing heat treatment. For this study thermomechanical rolling concepts were applied through the variation of some hot rolling parameters such as: temperature at the finishing pass and at the coils-former, the cooling conveyor belts velocity and some parameters in the heat treatment cycle: soak temperature and cooling rate during the production of round wire rod with 15,88 mm and 16,15 mm diameter. The evaluation response to changes imposed on the process was evaluated by metallographic analysis of microstructure in hot rolled and spheroidized material (spheroidizing degree), hardness, decarburization and tensile test. Eight rolling conditions and cooling rates were analyzed and results showed that higher cooling rates result in finer microstructures allowing a reduction in heat treatment time to achieve the desirable properties in the final product (spheroidized round wire rod).

The aim of the study was to investigate the crystallization kinetics and solidification behaviour of Fe60Co8Mo5Zr10W2B15 bulk glass forming alloy. The solidification behaviour in near-equilibrium and non-equilibrium cooling conditions was studied. The eutectic and peritectic reactions were found to exist in the solidification sequence of the alloy. The bulk metallic glass formation was achieved by using two methods: quenching from the liquid state and quenching from the semi-state. Scanning electron microscopy, x-ray diffraction and thermal analysis techniques were utilized in the characterization of the samples produced throughout the study. The choice of the starting material and the alloy preparation method was found to be effective in the amorphous phase formation. The critical cooling rate was calculated as 5.35 K/s by using the so-called Barandiaran and Colmenero method which was found to be comparable to the best glass former known to date. The isothermal crystallization kinetics of the alloy was studied at temperatures chosen in the supercooled liquid region and above the first crystallization temperature. The activation energies for glass transition and crystallization events were determined by using different analytical methods such as Kissinger and Ozawa methods. The magnetic properties of the alloy in the annealed, amorphous and as-cast states were characterized by using a vibrating sample magnetometer. The alloy was found to have soft magnetic properties in all states, however the annealed specimen was found to have less magnetic energy loss as compared to the others.

The aim of this study is to investigate the bulk glass forming ability (BGFA) of Ti-based alloy systems. These investigations were carried out in two main parts that are complementary to each other: theoretical and experimental. For theoretical studies, which are based on electronic theory of alloys in pseudopotential approximation, Ti-Zr, Ti-Co and Ti-Cu alloys were chosen as the binary systems. Alloying element additions were performed to each binary for the investigation of the BGFA of multicomponent Ti-based alloys. Among the three studied binary systems, Ti-Cu was found to exhibit better BGFA, and Mn, Al and Ni elements were found to be suitable for improving the BGFA of Ti-Cu binary alloy system. BGFA of Ti-Cu binary and Ti-Cu-(Mn, Al, Ni) multicomponent alloys were investigated with the experimental studies that were carried out with performing arc melting and centrifugal casting operations. The characterizations of these alloys were done with scanning electron microscopy, X-ray diffraction analysis and differential scanning calorimetry. Ti60Cu35Mn5, Ti60Cu35Al5 and Ti60Cu35Ni5 alloys were produced and characterized as examples for ternary systems. Among them, Ti60Cu35Mn5 system was found to have better indications regarding to BGFA. Therefore, it was chosen as the main composition and multicomponent alloys of Ti59Cu35Mn5Al1, Ti59Cu35Mn5Ni1 and Ti58Cu35Mn5Al1Ni1 were synthesized and characterized.

No description available.