Block copolymers have attracted interests for potential application ranging from dynamic photonic sensors to solid-state ion conductors. However, due to nucleation and growth mechanism, block copolymer inherently forms granular microstructure with defects such as grain boundaries. Understanding the microstructure of block copolymer is thus crucial in many applications because the microstructure determines the transport property of functional fillers such as ions in block copolymer template. Previous research has shown that athermal filler segregated to grain boundary of lamellae block copolymer and retards the grain coarsening. However, the kinetics of this grain boundary segregation during thermal annealing has not been revealed. Polystyrene-b-polyisoprene blended with deuterated polystyrene is used for neutron scattering study on studying the kinetics of grain boundary segregation. Deuterated polystyrene will segregate to grain boundaries, therefore, decorate grain boundary. The filler segregation behavior will be studied by comparing neutron scattering of polystyrene-b-polyisoprene/deuterated polystyrene with different annealing times (at T=130 deg C, duration of 0hr, 3hr, 1day, 3day and 7day, respectively). Invariant (Q) analysis along with grain mapping is conducted to quantitatively analyze the kinetics of grain boundary segregation. This kinetic was in good agreement with the McLean’s kinetic model for grain boundary segregation in metals. By applying Langmuir-Mclean’s segregation isotherm equation, we have predicted the equilibrium concentration of filler in grain boundary by calculating the strain energy stored in grain boundary.

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Recozimentos realizados nos aços elétricos semiprocessados pelos fabricantes de motores sem um controle adequado da descarbonetação pode resultar em regiões das läminas com pequeno tamanho de grão e consequentemente aumento das perdas magnéticas com queda no rendimento dos motores elétricos. A maioria dos fabricantes de motores nacionais utilizam este tipo de aço e fazem internamente o recozimento final em fornos contínuos com atmosfera à base de nitrogênio com cerca de 5 a 10% de H2 e uma pequena fração de vapor dágua suficiente para gerar uma atmosfera que reaja com o carbono do aço, removendo-o. Caso esta descarbonetação não seja realizada com êxito há uma perda significativa no rendimento do motor pela aumento das perdas magnéticas. Amostras comerciais de diferentes aços com variados teores de carbono foram selecionadas para avaliar a influência do teor de carbono, do grau de redução, do tempo e da atmosfera do forno no aumento do tamanho de grão e nas perdas magnéticas. Foram realizados recozimentos a vácuo e em atmosfera descarbonetante. Medições de perdas magnéticas e do tamanho de grão além da avaliação da microestrutura foram efetuados para determinar esta influência. Foi verificado que no recozimento a vácuo, mesmo em variados graus de deformação, amostras com o teor de carbono inicial maior que 300 ppm, tiveram um significativo atraso no aumento do tamanho de grão. Nas situações em que não ocorreu significativo aumento do TG as perdas magnéticas apresentaram valores altos e 9 indesejáveis. Por outro lado amostras isentas de deformação não apresentaram aumento significativo do tamanho de grão mesmo com descarbonetação durante o recozimento. Foi verificado ainda que a formação de grãos colunares ocorre em faixas de deformação específicas, em recozimentos com descarbonetação para aços com mais de 300 ppm de carbono e onde haja um rápido aquecimento da amostra até a temperatura de recozimento. / Annealing applied by the motors plants that are made on the semi processed electrical steels without an exact and precisious control of the decarburization on the lamination can brings undesirable results on the grain size coarsening and as a result an increasing on the core losses with a significant depreciation on the efficiency of the electrical motors. Most of the domestic motors fabrics make use of this kind of electrical steel and they do on their process the final annealing on continuous furnaces with atmospheres based on nitrogenium with around 5 until 10% of hidrogeniun and a little fraction of water vapor enough to generate an atmosphere that reacts to the carbon from the steel, eliminating it. If this decarburization is not been made sucessfully there will be an effective loss on the motor efficiency due the incresing on the core losses. Commercial samples from different steels with several carbon contents were choosen to evaluate the influence of carbon content, strain grade, time and furnace atmosphere on the grain size coarsening and core losses. It was effetived vacumn and decarburizing annealing. Core losses and grain size measurements were made in addition to the evaluation of the microstructure to determine this influence. It was verified that on the vacumn annealing, even on differents strain reductions grades, the samples with initial carbon content bigger than 300 ppm, had a meaninfull late on the grain size increase. On the situation that do not occurred a significative increase on the grain size the core losses presented undesirable high values. On the other hand samples without strain did not presented a significative increase on the grain size even with decarburization during the annealing. It was still verified that the columnar grain formation occur on specific strain grades, on decarburizing annealing and to more than 300 ppm carbon content steels. In addition where there is a fast heating rate until the annealing temperature.

Recozimentos realizados nos aços elétricos semiprocessados pelos fabricantes de motores sem um controle adequado da descarbonetação pode resultar em regiões das läminas com pequeno tamanho de grão e consequentemente aumento das perdas magnéticas com queda no rendimento dos motores elétricos. A maioria dos fabricantes de motores nacionais utilizam este tipo de aço e fazem internamente o recozimento final em fornos contínuos com atmosfera à base de nitrogênio com cerca de 5 a 10% de H2 e uma pequena fração de vapor dágua suficiente para gerar uma atmosfera que reaja com o carbono do aço, removendo-o. Caso esta descarbonetação não seja realizada com êxito há uma perda significativa no rendimento do motor pela aumento das perdas magnéticas. Amostras comerciais de diferentes aços com variados teores de carbono foram selecionadas para avaliar a influência do teor de carbono, do grau de redução, do tempo e da atmosfera do forno no aumento do tamanho de grão e nas perdas magnéticas. Foram realizados recozimentos a vácuo e em atmosfera descarbonetante. Medições de perdas magnéticas e do tamanho de grão além da avaliação da microestrutura foram efetuados para determinar esta influência. Foi verificado que no recozimento a vácuo, mesmo em variados graus de deformação, amostras com o teor de carbono inicial maior que 300 ppm, tiveram um significativo atraso no aumento do tamanho de grão. Nas situações em que não ocorreu significativo aumento do TG as perdas magnéticas apresentaram valores altos e 9 indesejáveis. Por outro lado amostras isentas de deformação não apresentaram aumento significativo do tamanho de grão mesmo com descarbonetação durante o recozimento. Foi verificado ainda que a formação de grãos colunares ocorre em faixas de deformação específicas, em recozimentos com descarbonetação para aços com mais de 300 ppm de carbono e onde haja um rápido aquecimento da amostra até a temperatura de recozimento. / Annealing applied by the motors plants that are made on the semi processed electrical steels without an exact and precisious control of the decarburization on the lamination can brings undesirable results on the grain size coarsening and as a result an increasing on the core losses with a significant depreciation on the efficiency of the electrical motors. Most of the domestic motors fabrics make use of this kind of electrical steel and they do on their process the final annealing on continuous furnaces with atmospheres based on nitrogenium with around 5 until 10% of hidrogeniun and a little fraction of water vapor enough to generate an atmosphere that reacts to the carbon from the steel, eliminating it. If this decarburization is not been made sucessfully there will be an effective loss on the motor efficiency due the incresing on the core losses. Commercial samples from different steels with several carbon contents were choosen to evaluate the influence of carbon content, strain grade, time and furnace atmosphere on the grain size coarsening and core losses. It was effetived vacumn and decarburizing annealing. Core losses and grain size measurements were made in addition to the evaluation of the microstructure to determine this influence. It was verified that on the vacumn annealing, even on differents strain reductions grades, the samples with initial carbon content bigger than 300 ppm, had a meaninfull late on the grain size increase. On the situation that do not occurred a significative increase on the grain size the core losses presented undesirable high values. On the other hand samples without strain did not presented a significative increase on the grain size even with decarburization during the annealing. It was still verified that the columnar grain formation occur on specific strain grades, on decarburizing annealing and to more than 300 ppm carbon content steels. In addition where there is a fast heating rate until the annealing temperature.

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.

Im Rahmen der vorliegenden Arbeit wurde der Einfluss der Korngröße und der Gefügestabilität auf die zyklische Plastizität von mikro- und submikrokristallinem Nickel, hergestellt durch ECAP und PED, untersucht. Zur Gefügecharakterisierung kamen verschiedene elektronenmikroskopische und röntgenographische Methoden zum Einsatz. Die Untersuchungen zur Gefügestabilität zeigten, dass (i) die Stabilität der Korn- und Substruktur bei der zyklischen Verformung empfindlich vom Gefüge im Ausgangszustand abhängt, (ii) generell die Tendenz zur Umwandlung der vorhandenen Substruktur in eine universelle ermüdungstypische Substruktur besteht, diese Transformation jedoch durch die lokale Gefügebeschaffenheit be- bzw. verhindert sein kann und (iii) zur Erklärung des Entfestigungsverhaltens der ECAP-Materialien sowohl die Transformation der Substruktur als auch die Vergröberung der Kornstruktur berücksichtigt werden müssen. Auf der Basis der Ergebnisse der vorliegenden Arbeit und unter Hinzunahme von Resultaten aus der Literatur lassen sich Schlussfolgerungen zum Einfluss der Korngröße auf die zyklische Plastizität in einem vier Größenordnungen umfassenden Korngrößenbereich ziehen. In grob- und feinkörnigem Nickel bilden sich bei der zyklischen Verformung ermüdungstypische Versetzungsstrukturen, deren Abmessungen kaum von der Korngröße abhängen. Der Versetzungslaufweg in diesen Materialien ist wesentlich kleiner als die Kornabmessungen. Dementsprechend besteht höchstens ein schwacher Einfluss der Korngröße auf das sich bei der Wechselverformung einstellende Spannungsniveau. Bei mikro- und submikrokristallinem Nickel, wo der Versetzungslaufweg in der Größenordung der Kornabmessungen liegt, wird ein deutlicher Umschlag bei der Versetzungsmusterbildung und dem zyklischen Verformungsverhalten beobachtet. In diesem Korngrößenbereich entstehen entweder qualitativ andere (D<DS1=5µm) oder keine Versetzungsstrukturen (D<DS2=1µm) und das Spannungsniveau steigt mit sinkender Korngröße entsprechend einer HALL-PETCH-Beziehung.

Im Rahmen der vorliegenden Arbeit wurde der Einfluss der Korngröße und der Gefügestabilität auf die zyklische Plastizität von mikro- und submikrokristallinem Nickel, hergestellt durch ECAP und PED, untersucht. Zur Gefügecharakterisierung kamen verschiedene elektronenmikroskopische und röntgenographische Methoden zum Einsatz. Die Untersuchungen zur Gefügestabilität zeigten, dass (i) die Stabilität der Korn- und Substruktur bei der zyklischen Verformung empfindlich vom Gefüge im Ausgangszustand abhängt, (ii) generell die Tendenz zur Umwandlung der vorhandenen Substruktur in eine universelle ermüdungstypische Substruktur besteht, diese Transformation jedoch durch die lokale Gefügebeschaffenheit be- bzw. verhindert sein kann und (iii) zur Erklärung des Entfestigungsverhaltens der ECAP-Materialien sowohl die Transformation der Substruktur als auch die Vergröberung der Kornstruktur berücksichtigt werden müssen. Auf der Basis der Ergebnisse der vorliegenden Arbeit und unter Hinzunahme von Resultaten aus der Literatur lassen sich Schlussfolgerungen zum Einfluss der Korngröße auf die zyklische Plastizität in einem vier Größenordnungen umfassenden Korngrößenbereich ziehen. In grob- und feinkörnigem Nickel bilden sich bei der zyklischen Verformung ermüdungstypische Versetzungsstrukturen, deren Abmessungen kaum von der Korngröße abhängen. Der Versetzungslaufweg in diesen Materialien ist wesentlich kleiner als die Kornabmessungen. Dementsprechend besteht höchstens ein schwacher Einfluss der Korngröße auf das sich bei der Wechselverformung einstellende Spannungsniveau. Bei mikro- und submikrokristallinem Nickel, wo der Versetzungslaufweg in der Größenordung der Kornabmessungen liegt, wird ein deutlicher Umschlag bei der Versetzungsmusterbildung und dem zyklischen Verformungsverhalten beobachtet. In diesem Korngrößenbereich entstehen entweder qualitativ andere (D<DS1=5µm) oder keine Versetzungsstrukturen (D<DS2=1µm) und das Spannungsniveau steigt mit sinkender Korngröße entsprechend einer HALL-PETCH-Beziehung.