As propriedades mecânicas, de corrosão e a condutividade térmica e elétrica, aliadas à relativa facilidade de fundir atribuem grande relevância ao cobre e suas ligas. Algumas destas propriedades podem ser significativamente melhoradas com a diminuição do tamanho de grão da estrutura bruta de solidificação a partir do tratamento de inoculação do banho líquido. Este tratamento aumenta o número de núcleos sólidos, diminuindo assim o tamanho médio de grão. Neste trabalho, foi realizado um estudo do refino de grão da estrutura bruta de solidificação a partir da inoculação com adições de C, P e Zr a ligas do sistema Cu-Zn com teores de até 30% de Zn. Três séries de experimentos principais foram realizadas. Na primeira, o teor de Zr na liga Cu- 30%Zn foi gradativamente aumentado até 0,4% para mostrar o efeito do Zr. Na segunda, o teor de Zr foi mantido constante em 0,08%, enquanto o teor de Zn foi elevado gradativamente até 30% para mostrar o efeito do Zn. Na terceira foram testadas adições isoladas e conjuntas de C, P e Zr para verificar o efeito de cada elemento no refinamento de grãos. As amostras foram caracterizadas e analisadas por diferentes técnicas: (a) observação da macroestrutura de grãos; (b) análise química; (c) análise térmica; (d) microscopia óptica; (e) microscopia eletrônica de varredura; (f) microanálise EDS; g) microanálise WDS e h) difração de raios X. Os resultados mostram que o tamanho médio de grão diminui significativamente nas ligas do sistema Cu-Zn (6% <= Zn <= 30%) quando Zr e P são adicionados simultaneamente. Isoladamente, estes elementos quando adicionados, não reduzem significativamente o tamanho de grão. Nota-se também que o tamanho de grão é cada vez menor à medida que o teor de Zn aumenta de 0 a 30% com a adição de 0,08%Zr, porém não se observa uma correlação entre tamanho de grão e teor de Zn quando Zr não é adicionado. Uma análise da microestrutura dos lingotes utilizando as técnicas mencionadas mostra que a diminuição do tamanho médio de grão a partir de adições de Zr e P coincide com o aparecimento de precipitados facetados ricos em Zr e P. Esta análise indica que um possível mecanismo de inoculação dos latões é a nucleação heterogênea da fase sólida Cu-µ, com estrutura cristalina cúbica de faces centradas, sobre partículas sólidas de ZrP, com estrutura hexagonal compacta, formadas no banho líquido após as adições de Zr e P. / Good mechanical and corrosion properties, large thermal and electrical conductivities, as well as relatively large castability are characteristics that contribute to the importance of copper and copper alloys. Some of these properties are enhanced when the average grain size of the as-cast structure decreases by inoculation of the melt. The inoculation treatment increases the number of solid nuclei, causing a reduction in the average grain size. In the present work, an investigation of the grain refinement by inoculation with Zr and P additions to Cu-Zn melts with contents of Zn up to 30%(mass) was carried out. Three series of experiments were conducted. In one the Zr content of the Cu-30%Zn alloy was gradually increased up to 0.4% to reveal the effects of Zr, while in the second series, the concentration of Zr was constant, equal to 0.08%, but the Zn content was gradually increased to 30% to show the effect of Zn. The third one was to test separate and conjunct addition of C, P and Zr in order to understand each elements effect on grain refinement. The resulting samples were characterized and analyzed by several techniques: (a) visual observation of the grain macrostructure; (b) chemical analysis; (c) thermal analysis; (d) optical microscopy; (e) scanning electron microscopy; (f) EDS microanalysis; (g) WDS microanalysis; and (h) X-Ray diffraction. The results show that the average grain size of the Cu-Zn alloys (6% <= Zn <= 30% mass) decreases significantly when Zr and P are both added to the melt. Nevertheless, average grain size is not reduced significantly when either Zr or P are added separately to the melt. When 0.08%Zr is added, the average grain size decreases as the concentration of Zn increases from 0 to 30%Zn, but without Zr additions, the Zn content and the average grain size are uncorrelated. The microstructural analysis with the techniques listed before show that the decrease in average grain size caused by Zr and P additions coincide with the observation of faceted precipitates rich in Zr and P. This analysis indicates that the inoculation mechanism is probably the heterogeneous nucleation of solid Cu-µ, of face-centered-cubic lattice structure, on solid particles of ZrP, with hexagonal compact structure, formed in the melt after Zr and P additions.

As ligas Al-Si hipoeutéticas têm grande importância na indústria de fundição de peças devido às excelentes propriedades de fundição, como baixo ponto de fusão e alta fluidez. A análise térmica das curvas de resfriamento medidas durante a solidificação destas ligas pode ser utilizada para controlar a formação da macroestrutura de grãos. Esta análise envolve a determinação das temperaturas de início e final de solidificação, bem como a evolução da fração de sólido com o tempo a partir da chamada análise térmica de Fourier. Apesar desta técnica ter sido aplicada a diversas ligas comerciais, existem poucos dados referentes às ligas Al-Si binárias. Os dados são ainda mais escassos quando se deseja examinar o efeito do tratamento de inoculação do metal líquido para refino de grão. O objetivo do presente trabalho é investigar o efeito do tratamento de inoculação nas ligas binárias Al-3%Si, Al-7%Si e Al-11%Si através da análise térmica e metalográfica. Foram obtidos lingotes cilíndricos a partir do vazamento da liga Al-Si líquida com ou sem a adição de inoculante na forma da liga mãe Al-3%Ti-1%B, adicionada para se obter um teor nominal de 0,05%Ti. Curvas de resfriamento foram medidas a partir de termopares inseridos no interior da cavidade do molde, composto de areia de sílica ligada com resina fenólica. Os lingotes foram seccionados e as suas micro e macroestruturas examinadas por metalografia óptica. A análise térmica das curvas de taxa de resfriamento e a análise térmica de Fourier foram aplicadas para determinar os instantes de início e final de solidificação, a magnitude da recalescência, a evolução da fração de sólido com o tempo e a fração de sólido no momento da coesão dendrítica. Os resultados mostram que o inoculante, apesar de adicionado na mesma quantidade em todas as ligas, é mais efetivo em diminuir o tamanho de grão da liga Al-3%Si do que das ligas Al-7%Si e Al-11%Si. Esta perda de eficiência é chamada de envenenamento do inoculante pelo Si. A evolução da fração de sólido mostra que a fração de coesão diminui com o aumento do teor de Si, como observado por alguns autores. A adição do inoculante diminui a fração de sólido durante a solidificação, diminuindo também a fração de coesão. Este efeito contraria dados da literatura para o ponto de coesão medido através de métodos mecânicos. / The hypoeutectic Al-Si alloys are extremely important to the foundry industry owing to their excellent fluidity and castability. The thermal analysis of the cooling curves measured during solidification of these alloys can be used to control the formation of the grain macrostructure. This analysis consists of the determination of the temperatures at the beginning and end of solidification, as well as the calculation of the time evolution of the solid fraction by more elaborate techniques, such as, the Fourier thermal analysis. Although this technique has been applied to several aluminum commercial alloys, there are very few data about binary Al-Si alloys. Available data related to the effect of melt inoculation to decrease grain size are even scarcer. The objective of the present work is to study the effect of the inoculation treatment of the binary alloys Al-3%Si, Al-7%Si, and Al-11%Si by thermal analysis and metalography. Cylindrical ingots were cast by pouring Al-Si melts with or without the addition of inoculant in the form of Al-3%Ti-1%B to obtain 0,05%Ti. Cooling curves were measured by thermocouples located within the mold cavity, made of silica sand and phenolic resin. The ingots were sectioned and their micro and macrostructures examined by optical metalography. The simple thermal analysis and the Fourier analysis were used to determine the time of beginning and end of solidification, the size of the recalescence, the time evolution of solid fraction and the solid fraction at the dendrite coherency point. The results show that, although the same amount of inoculant is added to all melts, it is more effective to decrease the grain size of the Al-3%Si than that of the Al7%Si and Al-11%Si alloys. This fading of efficiency is referred to as poisoning of the inoculant by Si. The evolution of solid fraction shows that the solid fraction at the coherency point decreases with an increase in the Si content, as observed by other authors. The addition of inoculant also causes a decrease in the solid fraction at dendrite coherency, which disagrees with some published coherency fraction obtained by mechanical methods.

As ligas de cobre têm grande importância na fabricação de produtos metálicos que necessitam de boa resistência à corrosão e/ou alta condutividade térmica e elétrica. A sua estrutura de grãos bruta de solidificação define diversas propriedades requeridas em serviço/processamento e o refino desta estrutura pode ser realizado a partir da inoculação do banho metálico antes do início da solidificação, aumentando o número de núcleos sólidos formados. A inoculação e os mecanismos de refino de grão em ligas de cobre foram pouco investigados e não são entendidos suficientemente para permitir o projeto de inoculantes. O presente trabalho tem como principal objetivo identificar os mecanismos fundamentais de inoculação e refino de grão das ligas do sistema Cu-Sn a partir de adições de Zr aos banhos líquidos antes da solidificação. Amostras cilíndricas foram produzidas a partir da solidificação das ligas a uma taxa de resfriamento de ~ 0,8 ?C/s. Estas amostras foram analisadas por diferentes técnicas: (a) observação da macroestrutura de grãos; (b) análise térmica das curvas de resfriamento obtidas durante a solidificação; (c) análise química; (d) exame da microestrutura em microscopia óptica, microscopia eletrônica de varredura (MEV) com emissão de campo (FEG), microscopia eletrônica de transmissão (MET) com e sem o feixe de íons (FIB) e (e) microanálise por espectroscopia de energia dispersiva (EDS). Observa-se que adições de Zr na faixa de 0,04 a 0,4% a banhos da liga Cu-8%Sn com cobertura de pó de grafita reduzem o tamanho médio de grão em até 90%, mas não causam efeito significativo sem a cobertura de grafita. Este efeito da diminuição do tamanho de grão com a adição de Zr torna-se significativo somente para teores de Sn >=4%. Esta redução de tamanho médio de grão é acompanhada do aparecimento de partículas facetadas na microestrutura, identificadas como ZrC a partir de padrões de difração de elétrons e microanálises EDS. Uma análise teórica mostra desajustes entre os reticulados do ZrC e do Cu? tão pequenos quanto 1,9%, indicando que estas partículas podem funcionar como centros efetivos para a nucleação heterogênea e causar o refino de grão em ligas de Cu. Parâmetros extraídos da recalescência das curvas de resfriamento, como a diferença entre as temperaturas mínima e máxima da recalescência, apresentaram boa correlação com o tamanho médio de grão final, indicando a possibilidade do controle do tamanho de grão em ligas Cu-Sn com adições de Zr a partir da análise térmica. / Copper alloys are important to the production of metallic parts with good corrosion resistance and high thermal and electrical conductivity. The as-cast grain structures of these alloys are closely related to the properties required in service or during processing. The refining of the grain structure can be achieved by inoculation of the metallic melt, before the beginning of solidification, increasing the number of solid nuclei. The inoculantion and grain refining of copper alloys have been poorly investigated and are not sufficiently understood to enable the design of inoculants. The objective of the present work is to identify the fundamental mechanisms underlying the inoculation and grain refining of Cu-Sn alloys by additions of Zr to the melt prior to solidification. Cylindrical samples of these alloys were cast at a cooling rate of ~0,8 ?C/s. These samples were analyzed using different techniques: (a) observation of the grain macrostructure; (b) thermal analysis of the cooling curves collected during solidification; (c) chemical analysis; (d) observation of the microstructure in the optical microscope, scanning electron microscope (SEM) with field emission gun (FEG), trasmission electron microscope (TEM) with and without the focused ion beam (FIB) for sample preparation and (e) energy dispersive spectroscopy (EDS) microanalysis. The results show that additions of Zr in the range between 0,04 and 0,4% to melts of a Cu-8%Sn alloy with a graphite powder cover decrease the average grain size by up to 90%, but have no effect without the graphite cover. The decrease in grain size obtained with Zr additions become significant only for alloys with %Sn >==4 and is followed by the appearance of faceted particles in the microstructure, identified as ZrC after examining electron difraction patterns and EDS microanalyses of the particles.

This thesis examines the influence of inoculation and modification on the internal structure and properties of aluminium-silicon alloys. The effect of inoculation by titanium and boron and modification by sodium and strontium is investigated in experimental part of the thesis. All these metallurgical interventions in the melt are tested on three types of hypoeutectic Al-Si alloys (AlSi10Mg(a), AlSi8Cu3, AlSi7Mg0,3). The experiment was carried out in cooperation with the foundry of non-ferrous metals, Aluminium Group, a.s. in Sloup.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第18987号 / 工博第4029号 / 新制||工||1620(附属図書館) / 31938 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 白井 泰治, 教授 松原 英一郎 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第19708号 / 工博第4163号 / 新制||工||1642(附属図書館) / 32744 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 白井 泰治, 教授 乾 晴行 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第20367号 / 工博第4304号 / 新制||工||1667(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 田中 功, 教授 乾 晴行 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

No description available.

Microstructure refinement was observed in the fusion zone of AZ31 magnesium (Mg) alloy resistance spot welds when an inoculant was added, either Ti, Al8Mn5, or Mn. The dependence of inoculant potency on the lattice disregistry between inoculants and matrix, and on the liquid cooling rate was studied. Microstructural characterization was performed via optical microscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Thin foils containing the interface of the inoculant particles and Mg matrix were prepared using a focused ion beam (FIB) technique. Columnar dendritic structures in the vicinity of the fusion boundary and equiaxed dendritic structures in the central area were observed in the fusion zone of welds in the SA and SB AZ31Mg alloys from different suppliers. However, the columnar dendritic zone (CDZ) was well restricted, and the width of the CDZ and the diameters of equiaxed dendrites were much smaller in the SA alloy than those in the SB alloy due to the earlier columnar-equiaxed-transition (CET) in the SA alloy. The refined microstructure in the fusion zone of the SA alloy welds is attributed to the pre-existence of the larger Al8Mn5 particles of 4-10 microns in length in the SA alloy which act as an inoculant for alpha-Mg heterogeneous nucleation. Fatigue life and dislocation substructure were compared between the SA and SB welds. The SA welds with the refined microstructure displayed an enhanced fatigue resistance compared to the SB welds, when the interfacial failure took place across the fusion zone. The increased number and dispersion of slip systems in the fine-grained SA welds contributed to the improvement of fatigue life. The well-developed columnar dendritic grains were successfully restricted and the coarse equiaxed dendritic grains were efficiently refined by intentionally adding Ti or Mn inoculant particles into the as-received SB alloy welds. The Ti and Mn particles of about 8μm diameter were observed to promote the nucleation of alpha-Mg grains during welding. TEM examinations showed the existence of local orientation relationships between the respective inoculants Ti, Mn, and Al8Mn5 with the Mg matrix. The further lattice matching was observed between the Al8Mn5 particles and Mg. The diameter of the added inoculant should be larger than 1.8 microns to make it a potent inoculant based on the thermodynamic calculation. Microstructural examinations of samples with different inoculant additions and under different cooling rates showed that the inoculant potency was high for the Ti inoculant, medium for the Al8Mn5, but low for the Mn, when the cooling rate was low. This order in the decrease of grain refinement efficiency is inversely proportional with the order of crystallographic lattice disregistry between inoculants and matrix, which is calculated based on a crystallographic matching model. This implies that the lattice disregistry determines the potency of inoculants at the low cooling rates. In comparison, the lattice disregistry did not influence the heterogeneous nucleation, when the cooling rate was high. It could be inferred that an extremely high cooling rate produces a large supercooling, and provides a sufficient driving force for heterogeneous nucleation.

High strain rate plastic deformation of metals results in the formation of localized zones of severe shear strain known as adiabatic shear bands (ASBs), which are a precursor to shear failure. The formation of ASBs in a high-strength low alloy steel, namely AISI 4340, was examined based on prior heat treatments (using different austenization and tempering temperatures), testing temperatures, and impact strain rates in order to map out grain size and grain deformation behaviour during the formation of ASBs. In the current experimental investigation, ASB formation was shown to be a microstructural phenomenon which depends on microstructural properties such as grain size, shape, orientation, and distribution of phases and hard particles—all controlled by the heat treatment process. Each grain is unique and its material properties are heterogeneous (based on its size, shape, and the complexity of the microstructure within the grain). Using measurements of grain size at various heat treatments as well as dynamic stress-strain data, a finite element model was developed using Matlab and explicit dynamic software LSDYNA to simulate the microstructural deformation of grains during the formation of ASBs. The model simulates the geometrical grain microstructure of steel in 2D using the Voronoi Tessellation algorithm and takes into account grain size, shape, orientation, and microstructural material property inhomogeneity between the grains and grain boundaries. The model takes advantage of the Smooth Particle Hydrodynamics (SPH) meshless method to simulate highly localized deformation as well as the Johnson-Cook Plasticity material model for defining the behavior of the steel at various heat treatments under high strain rate deformation.The Grain Model provides a superior representation of the kinematics of ASB formation on the microstructural level, based on grain size, shape and orientation. It is able to simulate the microstructural mechanism of ASB formation and grain refinement in AISI 4340 steel, more accurately and realistically than traditional macroscopic models, for a wide range of heat treatment and testing conditions.