Abstract IF steel with two grain sizes ( 70£gm and 210£gm ) strain amplitude of 2%¡B1.6%¡B1%¡B0.8%¡B0.6%¡B0.4%¡B0.3%¡B0.2%¡B0.1%¡B0.05% were fatigued in order to obtain basic fatigue properties. By use TEM , we can know that we can observe dislocation cells from £G£`t = 0.05% ~£G£`t = 2% . When £G£`t > 1.6% , hardening will occur , if not , softening will be observed . The more strain amplitude is , the more plastic deformation will be observed . When£G£`t > 0.3% , the elastic deformation will smaller than plastic deformation . When£G£`t =0.2% ~£G£`t = 0.4% , we can observe secondary hardening from the specimen of 70£gm . When £G£`t > 1% , the n¡¦ of 70£gm is more than the n¡¦ of 210£gm , that means the specimen of 70£gm has bigger hardening . By the ¡¥ Stress amplitude v.s. Plastic deformation amplitude ¡¦ plot of 70£gm and 210£gm , we can know that there is no ¡¥ pleatue ¡¦ . The more strain amplitude is , the more difference between long axis and short axis of dislocation cell will occur .

IF Steel to be used in this thesis which only have 50ppm carbon is approach Iron. It to be part of BCC. Because BCC material have much slip system when increase the cycle will induce to create multiple slip system. The dislocation structure often to become cell. We observation the same result of SEM and TEM in low cycle fatigue. The cell size is small in high plastic strain amplitude. The cell size is big in low strain amplitude. The difference of dislocation structures in front of crack tip which obtained under propagation rates o f 10-4, 10-5, 10-6 and 10-7 mm/cycle is the volume percentage occupied by the dislocation structures viz. misorientation cell, cell, wall, PSBs.

In this thesis, we use IF Steel to be the matrix which composition of carbon is 50ppm approaches Iron and belongs to the part of BCC structure. After we use the load 350kgf precrack, while the propagation rate approaching 2x10-5~3x10-5mm/cycle, we immediately drop the stress intensity factor(£Gk) to a level which is determined by the propagation rate of 9x10-7mm/cycle. Then we record the cycle number as P1, and after the crack tip continues to propagate, we record the cycle number again as P2, and between the period of (P2 ¡V P1), we take 4 sample which marks are 0.25(P2 ¡VP1), 0.5(P2 ¡VP1), 0.75(P2 ¡VP1), (P2 ¡VP1). By this way, we can find out the difference of microstructure of the crack tip from a high load level to a low one. On this experiment, we observation the vein structure, dislocation walls, and so on. It proves that the same phenomenon could also be happened on BCC material, just like FCC material. As time goes by, after drop load, the stored energy is more and more strong. And the vein structure of reverse evolution would become the structure of dislocation cells of normal evolution. Then the crack would continue to propagate on the circumstances.

The low cycle fatigue test of IF steel was controlled at 0.6%, 0.4%, 0.2%, and 0.1% strain amplitude until the specimens cracking. After 10000 cycles at 0.4% strain amplitude, changed the strain amplitude from 0.4% to 0.2%. We chose the steps of the low cycle fatigue test under reducing amplitude at 1000, 10000, and 20000 cycles. In addition, after 10000 cycles at 0.6% strain amplitude, changed the strain amplitude from 0.6% to 0.2%. We chose the steps of the low cycle fatigue test under reducing amplitude at 3000, 20000 and 100000 cycles. Then we used electron microscope to observe the dislocation structure, and knew the dislocation morphology of evolution process under reducing amplitude. The dislocation structure evolution of IF steel at low strain amplitude (0.1%, 0.2%) during low cycle fatigue developed the loop patches, dislocation walls, and dislocation cells step-by-step by increasing fatigue cycles. However, the dislocation structure evolution would be changed in the low cycle fatigue under reducing amplitude. We could observe that the dislocation cells were broken to the loop patches in different form. Attest to the dislocation morphology was changed under reducing amplitude. After 10000 cycles at 0.4% strain amplitude, change the strain amplitude from 0.4% to 0.2%., we could observe that the dislocation cells were broken to the loop patches and vein structure. And after 100000 cycles under changed loading amplitude from 0.6% to 0.2%, large area of open domains and some loop patches can be observed.

The objectives of this study were to examine the effect of strain and path change on the microstructural evolution of ultrafine grained interstitial free (IF) steel during equal channel angular extrusion (ECAE); to determine the mechanical properties; to observe the resulting texture; and to perform optical and electron microscopy of the resulting material. The effects of different routes of extrusion (A, B, C, C' and E), heat treatment and plastic strains from 1.15 to 18.4 were examined. Monotonous tensile testing was used to determine mechanical behavior of processed materials. X-ray diffraction and TEM analyses were performed to evaluate the effect of processing on texture and grain morphology. Hardness measurements were performed to determine recrystallization behavior of the processed material. Optical microscopy was conducted on heat treated samples to determine their grain size and refinement. Monotonous tensile testing of processed materials showed that there was significant strengthening after the first extrusion. Further processing resulted in increasing values of yield strength and ultimate tensile strength, with ductility at failure varying depending upon which processing route was used. The best tensile strength results were obtained after processing Routes 8C' and 16E, due to the significant grain refinement these routes produced. X-ray diffraction revealed increases in strength of preferred texture along the directions [111] and [001], perpendicular to the transverse plane, for all specimens that were processed using ECAE. TEM observations showed a consistent refinement of grain size as the amount of processing increased, especially within Routes C' and E. Hardness measurements of heat treated specimens showed that the onset of recrystallization occurred at approximately the same temperature of recrystallization as that of pure iron, 450°C. The recrystallization curves for all samples showed that grain growth begins at a temperature of around 700°C. The low carbon content of IF steel made optical microscopy challenging. The grain size of annealed materials becomes finer and more uniform, ranging between 60 and 90 μm2, at high strain levels under Routes C' and E, due to the many potential nucleation sites developed in highly worked material.

Conselho Nacional de Desenvolvimento CientÃfico e TecnolÃgico / CoordenaÃÃo de AperfeiÃoamento de NÃvel Superior / Os aÃos IF (Interstitial Free) foram desenvolvidos nos anos 70 objetivando obter materiais de boa conformabilidade e boa resistÃncia mecÃnica para aplicaÃÃo na indÃstria automobilÃstica. A textura cristalogrÃfica apÃs o processo de recozimento das chapas de aÃo IF tem papel determinante na boa conformabilidade destes aÃos. Neste trabalho sÃo estudadas as evoluÃÃes da microestrutura e da textura cristalogrÃfica de um aÃo IF estabilizado ao titÃnio (Ti) durante a etapa de aquecimento no recozimento. As amostras analisadas foram laminadas à quente, laminadas a frio (75% de reduÃÃo na espessura) e recozidas, respectivamente. Durante a etapa de aquecimento no recozimento foram retiradas amostras nas temperaturas de 730, 740, 750, 760, 770, 780, 790, 800, 810, 820 ÂC para anÃlise. Foi avaliada a evoluÃÃo da microestrutura de cada uma das amostras retiradas do forno por microscopia Ãtica. A avaliaÃÃo da evoluÃÃo da textura foi feita utilizando as tÃcnicas e difraÃÃo de raios-X e EBSD (Electron Back Scatter Diffraction). Os resultados mostraram a evoluÃÃo da recristalizaÃÃo dos grÃos e o tamanho de grÃo na microestrutura com o aumenta da temperatura. A evoluÃÃo da textura mostrou que em temperaturas mais baixas observa-se a presenÃa mais intensa das fibras DL e da componente Cubo Girado do que a fibra DN. Com a elevaÃÃo da temperatura ocorre a eliminaÃÃo da componente Cubo Girado e da fibra DL aumentando a intensidade da fibra DN, mas com aparecimento de direÃÃes (componentes) preferenciais. A tÃcnica de EBSD confirmou este comportamento e permitiu observar a evoluÃÃo da textura e da recristalizaÃÃo com a temperatura. / The Interstitial Free (IF) steels were developed in the 70s aiming to obtain materials of good formability and good mechanical strength for application in the automotive industry. The crystallographic texture after the annealing process of the IF steel sheet has good formability role in these steels. In this work were studied the evolution of the microstructure and crystallographic texture of a stabilized IF steel to titanium (Ti) during the heating step in annealing. The samples were hot rolled, cold rolled (75% reduction in thickness) and annealed, respectively. During the heating step in the annealed the samples were removed for temperatures of 730, 740, 750, 760, 770, 780, 790, 800, 810, 820  C for analysis. It was evaluated the evolution of the microstructure of each sample removed from the oven by optical microscopy. The evaluation of the evolution of texture was made using the techniques of X-ray diffraction and EBSD (Electron Back Scatter Diffraction). The results show the development of recrystallization grain size and grain microstructure with increasing temperature. The evolution of texture shows that in cooler temperatures it is observed the stronger presence of fibers DL component and the cube spun than the DN fiber. With the rise of temperature occurs elimination of component spun cube and elimination of DL fiber increasing the intensity of DN fiber, but with the advent of preferred directions (components). The EBSD technique confirmed this behavior and allowed us to observe the evolution of texture and recrystallization temperature.

Neste trabalho foram determinadas as propriedades monotônicas e de fadiga de baixo-ciclo em chapa fina de um aço livre de intersticiais (aço IF) com adição de titânio, utilizado na indústria automobilística. Os ensaios de fadiga foram realizados sob controle de deformação com R&#949 = -1 e com o auxílio de um sistema de alinhamento de garras. O material apresenta diferentes comportamentos de fadiga nas direções transversal e longitudinal (em relação à direção de laminação). Comparação entre a curva tensão-deformação monotônica e a curva tensão-deformação cíclica mostra que os corpos de prova transversais têm endurecimento cíclico para as amplitudes de deformação estudadas. A relação deformação-vida obtida para a direção transversal é dada por &#916&#949t/2 = 0,0186(2Nf)-0,262 + 0,235(2Nf)-0,476 com ponto de transição em 2Nt = 1,4x105 reversos, não sendo possível obtê-la para a direção longitudinal devido a problemas de flambagem. Vários métodos estimativos de propriedades de fadiga a partir de propriedades monotônicas foram comparados aos resultados experimentais. Os métodos da correlação quatro pontos e inclinação universal modificada apresentando boa correlação para a região de baixo-ciclo. Análise fratográfica por microscopia eletrônica de varredura mostrou a presença de estrias de propagação do estágio II, evidenciando a alta dutilidade do material. / In the present work, the monotonic and low cycle fatigue properties of thin sheet of interstitial free steel containing titanium additions, used in the automotive industry, were investigated. Fatigue tests were conducted under deformation control (R&#949 = -1) using a grip alignment fixture. The material exhibits different fatigue behavior for the transverse and longitudinal directions (in relation to the rolling direction). A comparison between the monotonic stress-strain curve and the cyclic stress-strain curve in the transverse direction showed that the material exhibits cyclic hardening in all strain amplitudes tested. The strain-life relationship obtained for transverse direction is given by &#916&#949t/2 = 0,0186(2Nf)-0,262 + 0,235(2Nf)-0,476 with transition point in 2Nt = 1,4x105 reverses; buckling of longitudinal specimens made impossible to obtain such relationship. Several prediction methods of fatigue properties from monotonic properties were compared to the experimental results. The Four Point Correlation and the Modified Universal Slopes Methods showed a good correlation for the low cycle region. Fractographic analysis through Scanning Eletronic Microscopy showed the presence of Stage II striations, giving support to the high ductility of the material.

Neste trabalho foram determinadas as propriedades monotônicas e de fadiga de baixo-ciclo em chapa fina de um aço livre de intersticiais (aço IF) com adição de titânio, utilizado na indústria automobilística. Os ensaios de fadiga foram realizados sob controle de deformação com R&#949 = -1 e com o auxílio de um sistema de alinhamento de garras. O material apresenta diferentes comportamentos de fadiga nas direções transversal e longitudinal (em relação à direção de laminação). Comparação entre a curva tensão-deformação monotônica e a curva tensão-deformação cíclica mostra que os corpos de prova transversais têm endurecimento cíclico para as amplitudes de deformação estudadas. A relação deformação-vida obtida para a direção transversal é dada por &#916&#949t/2 = 0,0186(2Nf)-0,262 + 0,235(2Nf)-0,476 com ponto de transição em 2Nt = 1,4x105 reversos, não sendo possível obtê-la para a direção longitudinal devido a problemas de flambagem. Vários métodos estimativos de propriedades de fadiga a partir de propriedades monotônicas foram comparados aos resultados experimentais. Os métodos da correlação quatro pontos e inclinação universal modificada apresentando boa correlação para a região de baixo-ciclo. Análise fratográfica por microscopia eletrônica de varredura mostrou a presença de estrias de propagação do estágio II, evidenciando a alta dutilidade do material. / In the present work, the monotonic and low cycle fatigue properties of thin sheet of interstitial free steel containing titanium additions, used in the automotive industry, were investigated. Fatigue tests were conducted under deformation control (R&#949 = -1) using a grip alignment fixture. The material exhibits different fatigue behavior for the transverse and longitudinal directions (in relation to the rolling direction). A comparison between the monotonic stress-strain curve and the cyclic stress-strain curve in the transverse direction showed that the material exhibits cyclic hardening in all strain amplitudes tested. The strain-life relationship obtained for transverse direction is given by &#916&#949t/2 = 0,0186(2Nf)-0,262 + 0,235(2Nf)-0,476 with transition point in 2Nt = 1,4x105 reverses; buckling of longitudinal specimens made impossible to obtain such relationship. Several prediction methods of fatigue properties from monotonic properties were compared to the experimental results. The Four Point Correlation and the Modified Universal Slopes Methods showed a good correlation for the low cycle region. Fractographic analysis through Scanning Eletronic Microscopy showed the presence of Stage II striations, giving support to the high ductility of the material.

QC 20100927

La technique Imagerie par Contraste de Canalisation d'Electron (ECCI) est utilisée en microscopie électronique à balayage (MEB) pour visualiser et caractériser des défauts cristallins tels que les dislocations. L’ECCI nécessite l'orientation, avec grande précision (meilleure que 0,1°), du cristal à analyser par rapport au faisceau d’électrons pour satisfaire les conditions très strictes de canalisation d'électrons. À cause de la limitation en résolution spatiale et angulaire des techniques actuelles permettant de déterminer l’orientation cristallographique, la caractérisation des défauts cristallins par ECCI est actuellement appliquée à des monocristaux (ou des polycristaux possédant des gros grains) et les conditions de canalisation ne sont pas toujours satisfaites. Dans ce projet de thèse, un mode de balayage Précession de faisceau (Rocking Beam en anglais) a été développé dans un microscope électronique à balayage. Il permet l’acquisition de diagrammes pseudo-Kikuchi haute résolution spatiale (500nm) et angulaire (0,04°) (High Resolution Selected Area Channeling Pattern en anglais (HR-SACP)) et de contrôler les conditions de canalisations nécessaire à l’ECCI. Ceci a permis d’améliorer considérablement la précision de l’ECCI (Accurate ECCI A-ECCI) et d’élargir son domaine d’application aux matériaux polycristallins à grains fins. Dans un deuxième temps, l’A-ECCI assistée par HR-SACP a été utilisé pour caractériser des défauts cristallins (dislocations, sous joint de grain, domaine d’ordre) dans des matériaux massifs polycristallins (Acier IF, UO2, TiAl). Des procédures similaires à celles utilisées dans la microscopie électronique en transmission (MET) sont alors appliquées en s’affranchissant de la préparation fastidieuse de lames minces et en profitant des autres avantages du MEB / Electron Channeling Contrast Imaging (ECCI) is a Scanning Electron Microscope (SEM) technique used to observe and characterize crystallographic defects. ECCI requires the crystal to be oriented relative to the electron beam with high accuracy (0.1°) in order to control the electron channeling conditions. The SEM techniques used to determine the crystallographic orientation, such as conventional Electron BackScattered Diffraction (EBSD) or Rocking Beam, don’t satisfy the high accuracy required for ECCI. Therefore, the characterization of crystallographic defects by ECCI is used only in single crystals or polycristals with large grains and channeling conditions are not always satisfied. In this thesis, a development of a new Rocking Beam mode in SEM is presented. It allows the collection of High spatial (500nm) and angular (0.04°) Resolution Selected Area Channeling Pattern (HR-SACP) and the control of channeling conditions required for ECCI with high accuracy (Accurate ECCI A-ECCI). In a second phase of this thesis, A-ECCI assisted by HR-SACP is used to characterize crystallographic defects like dislocation, sub-grains and order domains in fine grained bulk materials (IF-Steel, UO2, TiAl). In order to achieve this, several procedures (invisibility criteria) normally used in Transmission Electron Microscopy are applied. Using A-ECCI in SEM has many advantages over TEM such as the possibility of analyzing large areas and the relative easiness in sample preparation