Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Technology Student: Tisoňová Zuzana Consultant: Doc. RNDr. Milan Řehula, CSc. Compacting process is mathematically expressed by compression equations. It is characterized by various parameters of equations. The equation expresses the dependence of the volume, density and height on compacting pressure. In this paperwork, the parameters of compacting equation are evaluated and the pre-loading phase, the phase of elastic deformation and the phase of plastic deformation are studied. This thesis deals with impact of ibuprofen on the parameters of compaction equation. Five mixtures which included microcrystalline celulose and ibuprofen in different ratio 100:0, 75:25, 50:50, 25:75 and 0:100 were studied. Results were based on the three-exponential equation. They were evaluated thanks to box plots. From the results obtained, it is obvious that with decreasing amount of microcrystalline cellulose, the parameter a1 has increased and the parameter E1 also slightly has increased. The composition of the used material didn't have any huge influence on parameters 1/t1 and pH1. During the phase of elastic deformation, the parameters a2 and E2 with decreasing amount of ibuprofen have decreased. On the other hand, the...

Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Technology Student: Jakub Šmíd Consultant: Doc. RNDr. Milan Řehula, CSc. Effect of acetylsalicylic acid on the parameters of compression equation Compacting process can be expressed mathematically by compression equations. It is characterized by various parameters. The compression equation expresses the dependence of the volume, density and height on compacting pressure. This paper evaluates the parameters of the compaction equation and study pre-loading phase, the phase of elastic deformation and the phase of plastic deformation. This thesis examines effect of acetylsalicylic acid on the parameters of compaction equation. Tablets were compressed from five mixtures. Mixtures contained acetylsalicylic acid and microcrystalline cellulose in different ratios 0:100, 25:75, 50:50, 75:25 and 0:100. The results were obtained using the three-exponential equation. Evaluation was carried out by using box plots.

Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical technology Supervisor: Doc. RNDr. Milan Řehula, CSc. Title of Dissertation: Validation of a new method for the evaluation of stress relaxation of tablets Keywords: tablets, stress relaxation test, elastic and plastic deformation The theoretical part of this thesis deals with the elastic relaxation of tablets. It describes various methods used in the evaluation of elastic recovery of tablets. The present work explores the factors affecting the elastic relaxation of tablets. The experimental part is focused on the stress relaxation test. Until present only one delay was studied. This work studies the stress relaxation after relieving tablet. The parameters A2, T2 and P2 were reviewed. The relationship between the parameters P2 and compression force relief were studied. For experiments microcrystalline cellulose Avicel PH 102 (MCC) was used. Tablets were compressed in a device used for testing the strength of the material in pressure and tension T1-FRO 50. For the determination of the stress relaxation test, the tablets were compressed with 180 sec first delay. The second delay was always 60 sec but it was measured from certain decrease of pressure (7 kN, 6 kN, 5 kN, 4 kN, 3 kN, 2 kN, 1 kN and 0.1 kN). To...

Este trabalho avalia o efeito da deformação plástica sobre as propriedades magnéticas em amostras de aço elétrico de grão não orientado. O material sob estudo foi extraído de uma bobina de aço elétrico GNO, com 0,8 % Si, em estado recozido, com densidade 7781 kg/m3 e tamanho de grão 20 µm. As chapas extraídas foram laminadas a frio para a produção de amostras com deformação real entre 0,03 e 0,29. A densidade de discordâncias desses corpos de prova foi estimada através de difração de raios-X. Através da análise da largura à meia altura dos picos de difração foi possível estimar a densidade de discordâncias das amostras. Os resultados descreveram maior taxa de aumento da densidade de discordâncias para pequenas deformações. A partir de 0,12 de deformação real o incremento foi pequeno. No que tange à caracterização magnética, para os ciclos de histereses obtidos em regime quase estático, verificou-se aumento da perda histerética com o crescimento da deformação plástica. Essa relação foi descrita de acordo com a lei de dependência onde a perda histerética cresce com a raiz quadrada da deformação real. Sobre o efeito da frequência de excitação na dissipação de energia por perdas magnéticas, o material não deformado mostrou-se mais sensível que os laminados a frio ao aumento da frequência. Pois se constatou que os materiais laminados apresentaram perda de excesso desprezível. Este comportamento pode ser explicado assumindo-se que com a deformação plástica eleva-se o número de paredes de domínio por unidade de volume, diminuindo assim as perdas de excesso. Dessa forma, para a faixa de VII frequências analisada, a perda histerética é a parcela que mais contribuiu para o aumento da perda magnética com a deformação. / This study evaluates the effect of plastic deformation on the magnetic properties of electrical steel in electrical steel samples. The material under investigation was obtained from a coil of non-oriented electrical steel sheets, 0.8% Si, annealed, with density 7781 kg/m3 and grain size of 20 µm. The material was cold rolled in order to produce samples with true strain ranging from 3 to 29%. The specimens dislocation density was estimated by X-ray diffraction. Analyzing the full width at half maximum of the diffraction peaks was possible to estimate the dislocation density of the samples. The results described a large increasing rate of dislocation density for small deformations and from 12% true strain the increment was small. On the magnetic characterization, the hysteresis loops obtained at quasi static regime shown a hysteresis loss increasing with true strain. This relationship is described according to the law of dependence where the increasing is linear with the square root of the true strain. All samples suffered total loss increasing with the frequency growth. It was observed that the hysteresis loss was the main contribution for the energy dissipation, for any true strain level. The undeformed material exhibited greather sensibility to frequency excitation than any strained sample. This result occurs due to the cold rolled sheets presented negligible excess loss. This behavior can be explained assuming the hypothesis that the number of domain walls per unit volume increase due to grain fragmentation, thus reducing excess loss.

Amostras de nióbio de alta pureza na forma de monocristais, bicristais e policristais foram retiradas de seções longitudinais de lingotes fundidos por feixe eletrônico. As amostras foram deformadas via extrusão em canal angular (ECAE - Equal Channel Angular Extrusion) em temperatura ambiente até 8 passes, utilizando a rota Bc numa matriz com ângulo de intersecção entre os canais de  = 90º. As amostras foram caracterizadas em termos da evolução microestrutural e da textura de deformação. A caracterização microestrutural foi realizada com o auxílio de microscopias ótica, eletrônica de varredura e eletrônica de transmissão, além de medidas de difração de elétrons retroespalhados (EBSD) para determinação da microtextura e da mesotextura. Medidas de microdureza Vickers foram realizadas para acompanhar o encruamento e o amolecimento das amostras. Um outro monocristal de nióbio foi deformado em 1 passe via ensaio interrompido, utilizando uma matriz com ângulo  = 120º, a fim de estudar a evolução da textura durante a passagem pelo canal de ECAE. A textura foi determinada por meio de difração de raios X e comparada com os dados da literatura para materiais deformados via ECAE com estrutura CCC e também com as texturas simuladas pelo modelo VPSC (visco-plastic self-consistent). No estudo comparativo numa escala maior (monocristal e policristal), verificou-se que houve um refinamento microestrutural significativo após 8 passes. O espaçamento médio entre os contornos de alto ângulo medido perpendicular à direção de extrusão foi próximo nos dois casos (500 nm), maior que o observado para o monocristal deformado numa escala menor (440 nm). Os resultados mostram ainda que os grãos do policristal deformado são mais equiaxiais que os do monocristal. Amostras foram recozidas isotermicamente para avaliar o comportamento frente ao engrossamento microestrutural. Os resultados mostram que o engrossamento torna-se apreciável, em geral, a partir de 500oC com a ocorrência de recristalização descontínua. Acima de 700oC, o crescimento normal de grão passa a ser o principal mecanismo de engrossamento microestrutural. Efeitos de orientação importantes foram observados no bicristal nos estados encruado e recozido. / High-purity niobium single crystals, bicrystals and polycrystals were cut out from longitudinal sections of ingots processed by electron beam melting. Samples were deformed by Equal Angular Channel Extrusion (ECAE) at room temperature up to 8 passes, using the route Bc with a die angle  = 90o. Samples were characterized in terms of their microstructural evolution and deformation textures. Microstructural characterization was performed using optical, scanning electron, and transmission electron microscopies, as well as electron-backscatter diffraction measurements (EBSD) to determine both microtexture and mesotexture. Vickers microhardness testing was performed to follow hardening and softening behaviors in the samples. Another single crystal was deformed by 1 pass in an interrupted ECAE experiment using a die angle  = 120o to follow the changes in texture through the extrusion channel. Texture was determined by X ray diffraction and compared with those reported in the literature for deformed bcc materials and also with those predicted using the viscoplastic self-consistent model (VPSC). A comparative study in a larger scale (single and polycrystals) was also performed. It was observed that there is a significant refinement of the microstructure after 8 passes. The average spacing between high angle boundaries perpendicular to extrusion direction was close in the two cases (500 nm), larger than observed in the single crystal deformed in a smaller scale (440 nm). Results also show that ultrafine grains of the deformed polycrystal are more equiaxial compared to those found in the deformed single crystal. Samples were annealed to evaluate their behavior regarding microstructural coarsening. Results show that coarsening becomes noticeable at temperatures higher than 500oC by means of discontinuous recrystallization. Above 700oC, normal grain growth becomes the main microstructure coarsening mechanism. Important orientation effects were observed in the bicrystal in both deformed and annealed states.

Este trabalho avalia o efeito da deformação plástica sobre as propriedades magnéticas em amostras de aço elétrico de grão não orientado. O material sob estudo foi extraído de uma bobina de aço elétrico GNO, com 0,8 % Si, em estado recozido, com densidade 7781 kg/m3 e tamanho de grão 20 µm. As chapas extraídas foram laminadas a frio para a produção de amostras com deformação real entre 0,03 e 0,29. A densidade de discordâncias desses corpos de prova foi estimada através de difração de raios-X. Através da análise da largura à meia altura dos picos de difração foi possível estimar a densidade de discordâncias das amostras. Os resultados descreveram maior taxa de aumento da densidade de discordâncias para pequenas deformações. A partir de 0,12 de deformação real o incremento foi pequeno. No que tange à caracterização magnética, para os ciclos de histereses obtidos em regime quase estático, verificou-se aumento da perda histerética com o crescimento da deformação plástica. Essa relação foi descrita de acordo com a lei de dependência onde a perda histerética cresce com a raiz quadrada da deformação real. Sobre o efeito da frequência de excitação na dissipação de energia por perdas magnéticas, o material não deformado mostrou-se mais sensível que os laminados a frio ao aumento da frequência. Pois se constatou que os materiais laminados apresentaram perda de excesso desprezível. Este comportamento pode ser explicado assumindo-se que com a deformação plástica eleva-se o número de paredes de domínio por unidade de volume, diminuindo assim as perdas de excesso. Dessa forma, para a faixa de VII frequências analisada, a perda histerética é a parcela que mais contribuiu para o aumento da perda magnética com a deformação. / This study evaluates the effect of plastic deformation on the magnetic properties of electrical steel in electrical steel samples. The material under investigation was obtained from a coil of non-oriented electrical steel sheets, 0.8% Si, annealed, with density 7781 kg/m3 and grain size of 20 µm. The material was cold rolled in order to produce samples with true strain ranging from 3 to 29%. The specimens dislocation density was estimated by X-ray diffraction. Analyzing the full width at half maximum of the diffraction peaks was possible to estimate the dislocation density of the samples. The results described a large increasing rate of dislocation density for small deformations and from 12% true strain the increment was small. On the magnetic characterization, the hysteresis loops obtained at quasi static regime shown a hysteresis loss increasing with true strain. This relationship is described according to the law of dependence where the increasing is linear with the square root of the true strain. All samples suffered total loss increasing with the frequency growth. It was observed that the hysteresis loss was the main contribution for the energy dissipation, for any true strain level. The undeformed material exhibited greather sensibility to frequency excitation than any strained sample. This result occurs due to the cold rolled sheets presented negligible excess loss. This behavior can be explained assuming the hypothesis that the number of domain walls per unit volume increase due to grain fragmentation, thus reducing excess loss.

Amostras de nióbio de alta pureza na forma de monocristais, bicristais e policristais foram retiradas de seções longitudinais de lingotes fundidos por feixe eletrônico. As amostras foram deformadas via extrusão em canal angular (ECAE - Equal Channel Angular Extrusion) em temperatura ambiente até 8 passes, utilizando a rota Bc numa matriz com ângulo de intersecção entre os canais de  = 90º. As amostras foram caracterizadas em termos da evolução microestrutural e da textura de deformação. A caracterização microestrutural foi realizada com o auxílio de microscopias ótica, eletrônica de varredura e eletrônica de transmissão, além de medidas de difração de elétrons retroespalhados (EBSD) para determinação da microtextura e da mesotextura. Medidas de microdureza Vickers foram realizadas para acompanhar o encruamento e o amolecimento das amostras. Um outro monocristal de nióbio foi deformado em 1 passe via ensaio interrompido, utilizando uma matriz com ângulo  = 120º, a fim de estudar a evolução da textura durante a passagem pelo canal de ECAE. A textura foi determinada por meio de difração de raios X e comparada com os dados da literatura para materiais deformados via ECAE com estrutura CCC e também com as texturas simuladas pelo modelo VPSC (visco-plastic self-consistent). No estudo comparativo numa escala maior (monocristal e policristal), verificou-se que houve um refinamento microestrutural significativo após 8 passes. O espaçamento médio entre os contornos de alto ângulo medido perpendicular à direção de extrusão foi próximo nos dois casos (500 nm), maior que o observado para o monocristal deformado numa escala menor (440 nm). Os resultados mostram ainda que os grãos do policristal deformado são mais equiaxiais que os do monocristal. Amostras foram recozidas isotermicamente para avaliar o comportamento frente ao engrossamento microestrutural. Os resultados mostram que o engrossamento torna-se apreciável, em geral, a partir de 500oC com a ocorrência de recristalização descontínua. Acima de 700oC, o crescimento normal de grão passa a ser o principal mecanismo de engrossamento microestrutural. Efeitos de orientação importantes foram observados no bicristal nos estados encruado e recozido. / High-purity niobium single crystals, bicrystals and polycrystals were cut out from longitudinal sections of ingots processed by electron beam melting. Samples were deformed by Equal Angular Channel Extrusion (ECAE) at room temperature up to 8 passes, using the route Bc with a die angle  = 90o. Samples were characterized in terms of their microstructural evolution and deformation textures. Microstructural characterization was performed using optical, scanning electron, and transmission electron microscopies, as well as electron-backscatter diffraction measurements (EBSD) to determine both microtexture and mesotexture. Vickers microhardness testing was performed to follow hardening and softening behaviors in the samples. Another single crystal was deformed by 1 pass in an interrupted ECAE experiment using a die angle  = 120o to follow the changes in texture through the extrusion channel. Texture was determined by X ray diffraction and compared with those reported in the literature for deformed bcc materials and also with those predicted using the viscoplastic self-consistent model (VPSC). A comparative study in a larger scale (single and polycrystals) was also performed. It was observed that there is a significant refinement of the microstructure after 8 passes. The average spacing between high angle boundaries perpendicular to extrusion direction was close in the two cases (500 nm), larger than observed in the single crystal deformed in a smaller scale (440 nm). Results also show that ultrafine grains of the deformed polycrystal are more equiaxial compared to those found in the deformed single crystal. Samples were annealed to evaluate their behavior regarding microstructural coarsening. Results show that coarsening becomes noticeable at temperatures higher than 500oC by means of discontinuous recrystallization. Above 700oC, normal grain growth becomes the main microstructure coarsening mechanism. Important orientation effects were observed in the bicrystal in both deformed and annealed states.

The objective of the research presented in this thesis has been to develop a physics-based dislocation density-based numerical framework to simulate microstructure evolution in severe plastic deformation (SPD) manufacturing processes for different materials. Different mechanisms of microstructure evolution in SPD manufacturing processes were investigated and summarized for different materials under dynamic or high strain rates over a wide temperature range. Thorough literature reviews were performed to clarify discrepancies of the mechanism responsible for the formation of nanocrystalline structure in the machined surface layer under both low-temperature and high-temperature conditions. Under this framework, metallo-thermo-mechanically (MTM) coupled finite element (FE) models were developed to predict the microstructure evolution during different SPD manufacturing processes. Different material flow stress responses were modeled subject to responsible plastic deformation mechanisms. These MTM coupled FE models successfully captured the microstructure evolution process for various materials subjected to multiple mechanisms. Cellular automaton models were developed for SPD manufacturing processes under intermediate to high strain rates for the first time to simulate the microstructure evolution subjected to discontinuous dynamic recrystallization and thermally driven grain growth. The cellular automaton simulations revealed that the recrystallization process usually cannot be completed by the end of the plastic deformation under intermediate to high strain rates. The completion of the recrystallization process during the cooling stage after the plastic deformation process was modeled for the first time for SPD manufacturing processes at elevated temperatures.

An ever increasing demand to exploit oil and natural gas reserves has significantly increased extraction activities even in the remotest regions of the Arctic and sub-Arctic regions of the Canadian North. Steel pipelines are the most efficient mode for transporting and distributing these resources. These pipelines, particularly buried in cold region, often subjected to extreme geo-environmental conditions, where significant inelastic deformation may occur resulting in localized wrinkles. Under continued deformation, there is a possibility of excessive cross-sectional deformation at wrinkle locations, eventually leading to fracture or damage in the pipe wall jeopardizing pipeline safety and integrity . Prior research indicated that occurrence of fracture in pipe wrinkle is rare under monotonic load-deformation process. However, a recent field fracture was observed within the wrinkle location of an energy pipeline. Similar failure mode was observed in a laboratory specimen at the University of Alberta. Both field and laboratory observations had indicated that the final failure was a “tearing” failure at the fold of the telescopic wrinkles resulting from monotonic application of axial load not aligned with pipe axis. This research program was designed to study this specific failure mode and to develop design tool for pipeline engineers. This research started with examining the failed field and test specimens. A preliminary investigation was carried out using nonlinear finite element (FE) model to simulate test and field behaviour. Numerical results have indicated that even under monotonic loading, significant strain reversals could occur at the wrinkle fold . Presence of these strain reversals was proposed as the preliminary failure criterion responsible for this unique failure mechanism. In next phase, a full-scale ‘pipe-wrinkling’ test program was carried out concurrent to this research to better understand the loading condition responsible for this type of failure. Results of this test program have shown the presence of tearing fracture or rupture in the pipe walls of several of test specimens. A series of FE analyses was then carried out to predict and verify the behaviour of these test specimens. After successful simulation of the test behaviour, further numerical analyses were carried out using tension coupon model developed herein to simulate the material behaviour using the material test data and hence to formulate the limiting conditions in terms of critical strain responsible for the tearing failure. Based on these numerical results, a double criterion  ‘Strain Reversal’ and ‘Critical Equivalent Plastic Strain Limit’, were proposed to predict tearing fracture of wrinkled pipe under monotonic loading. Results of these numerical analyses have demonstrated that the proposed criteria predict this failure mode with reasonable accuracy. In the final phase of this research, a parametric study was carried out to consider the effect of different parameters on failure modes of wrinkled pipe. Results of this parametric study describe the range of parameters under which the tearing mechanism can/may exhibit. / Structural Engineering

NiTiHf alloys have attracted considerable attention as potential high temperature Shape Memory Alloy (SMA) but the instability in transformation temperatures and significant irrecoverable strain during thermal cycling under constant stress remains a major concern. The main reason for irrecoverable strain and change in transformation temperatures as a function of thermal cycling can be attributed to dislocation formation due to relatively large volume change during transformation from austenite to martensite. The formation of dislocations decreases the elastic stored energy, and during back transformation a reduced amount of strain is recovered. All these observations can be attributed to relatively soft lattice that cannot accommodate volume change by other means. We have used Equal Channel Angular Extrusion (ECAE), hot rolling and marforming to strengthen the 49.8Ni-42.2Ti-8Hf (in at. %) material and to introduce desired texture to overcome these problems in NiTiHf alloys. ECAE offers the advantage of preserving billet cross-section and the application of various routes, which give us the possibility to introduce various texture components and grain morphologies. ECAE was performed using a die of 90º tool angle and was performed at high temperatures from 500ºC up to 650ºC. All extrusions went well at these temperatures. Minor surface cracks were observed only in the material extruded at 500 °C, possibly due to the non-isothermal nature of the extrusion. It is believed that these surface cracks can be eliminated during isothermal extrusion at this temperature. This result of improved formability of NiTiHf alloy using ECAE is significant because an earlier review of the formability of NiTiHf using 50% rolling reduction concluded that the minimum temperature for rolling NiTi12%Hf alloy without cracks is 700°C. The strain level imposed during one 90° ECAE pass is equivalent to 69% rolling reduction. Subsequent to ECAE processing, a reduction in irrecoverable strain from 0.6% to 0.21% and an increase in transformation strain from 1.25% to 2.18% were observed at a load of 100 MPa as compared to the homogenized material. The present results show that the ECAE process permits the strengthening of the material by work hardening, grain size reduction, homogeneous distribution of fine precipitates, and the introduction of texture in the material. These four factors contribute in the increase of stability of the material. In this thesis I will be discussing the improvement of mechanical behavior and stability of the material achieved after various passes of ECAE.