Pipeline steels that carry oil and natural gas in severe environments suffer from two important modes of failure: stress corrosion cracking (SCC) and hydrogen-induced cracking (HIC). The SCC has been studied extensively in the literature; however, HIC phenomenon in pipeline steels is less investigated by researchers. Nevertheless, HIC is recognized as the most important damage mode in sour environment. Hydrogen atoms produced due to surface corrosion of the steel diffuse into it through microstructural defects. When a critical amount of hydrogen is accumulated in such defects, HIC cracks initiate and propagate. The main objectives of this thesis are to find the HIC crack nucleation and propagation sites, evaluate a role of texture and grain boundary character distribution in crack growth and finally establish the effect of different microstructural parameters contributing to the HIC related failure in pipeline steel. In this thesis, HIC standard test and electrochemical hydrogen-charging experiments were used to induce HIC cracks in pipeline steels. HIC cracks at the cross section of tested samples were observed using scanning electron microscope (SEM). The SEM observations clearly indicate that the investigated X60 and X70 steels are susceptible to HIC while the X60SS steel showed a higher resistance to HIC. This experiment also proved that the X70 steel has higher susceptibility to HIC than the other investigated steel. Energy dispersive spectroscopic (EDS) analyses indicated that two types of inclusion namely manganese sulfide and carbonitiride precipitates serve as crack nucleation sites. HIC cracks were observed to propagate at the center of cross section where the segregation of some elements such as carbon and manganese occurred. Moreover, two other experiments were carried out in order to evaluate the capability of pipeline steels for hydrogen-trapping. The first test, hydrogen-permeation experiment, showed that all pipeline steel specimens, such as X70, X60 and X60SS steels, contain both reversible and irreversible hydrogen traps. However, the density of traps at the center of cross section was higher than other regions in all tested specimens. The hydrogen-discharging experiments also showed that all specimens keep a considerable amount of hydrogen inside their traps. The hydrogen traps, based on their binding energy with the metal matrix, are categorized as reversible (weak) and irreversible (strong) traps and the roles of each type of traps are explained. Electron backscatter diffraction (EBSD) measurements were done along the HIC crack in X70 steel after standard HIC test. The results showed that the {100} texture was strong while the {111} texture was weak. Some special texture components, such as the {110}, {332} and {112}, were observed after the HIC crack-stoppage. EBSD results also documented that fine grain colonies were prone to intergranular HIC crack propagation and IPF and PF, calculated in both sides of HIC cracks, showed the preferences of ND||<100> orientation. Both susceptible X60 and non-susceptible X60SS steel to HIC were compared based on the EBSD results. It was observed that the high amount of recrystallization fraction with no stored energy is one of the main reasons for a higher HIC resistance of X60SS steel to HIC. Moreover, Kernel Average Misorientation (KAM) data showed that the deformation is more concentrated in the as-received and HIC tested X60 specimens. The effect of hydrogen-charging during tensile/fatigue loading of X60SS steel was studied and it was observed that some HIC cracks at the cross section of X60SS steel were appeared after hydrogen-charging at stresses below the yield stress. Experiments were carried out to understand the effect of cold-rolling and annealing on HIC susceptibility in pipeline steels. The results documented that the {100} dominant texture is more pronounced in 50% and 90% cold-rolled and annealed specimens. The effect of different factors such as KAM degree and recrystallized fraction affecting HIC susceptibility on cold-rolled and annealed specimens was investigated. The obtained results showed that the cold-rolling and annealing process may not be considered as an effective method to increase HIC resistance in pipeline steels.

Submitted by Alison Vanceto (alison-vanceto@hotmail.com) on 2017-06-08T17:59:02Z No. of bitstreams: 1 DissTMG.pdf: 5915699 bytes, checksum: 6ec0af39899ad70e102eda93fa21e0e0 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-06-14T13:47:59Z (GMT) No. of bitstreams: 1 DissTMG.pdf: 5915699 bytes, checksum: 6ec0af39899ad70e102eda93fa21e0e0 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-06-14T13:48:05Z (GMT) No. of bitstreams: 1 DissTMG.pdf: 5915699 bytes, checksum: 6ec0af39899ad70e102eda93fa21e0e0 (MD5) / Made available in DSpace on 2017-06-14T13:55:25Z (GMT). No. of bitstreams: 1 DissTMG.pdf: 5915699 bytes, checksum: 6ec0af39899ad70e102eda93fa21e0e0 (MD5) Previous issue date: 2015-02-27 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / The morphology of extruded multiphase polymer systems is usually assessed through off-line characterization methods such as microscopy, which require much time for sample preparation and analysis of the results. This work aimed to the improvement of an optical detector to measure in real time the morphology of blends and polymeric composites in processing by extrusion, by laser light scattering at low angle (LALLS). Such equipment includes hardware and software and is based on measuring the intensity of light from a laser and is spread across and under the melt flow. The signals are collected by an array 91 of photodetectors sent to a computer, and displayed in real time on a three- dimensional plot of scattered light intensity to form a surface defined by 321 points. When analyzing the scattering profile valuable information can be determined that help to elucidate the morphology of the second phase particles. The LALLS detector was tested on bench using standard samples, which were prepared so that one of its parameters (orientation, second phase concentration, dispersed particle size or type of dispersed particle) were known. This allowed the systematic study of these samples and the detector device validation. Finally, the device was tested in real time on the extrusion process, and under different materials and operating conditions. Thus, the LALLS detector device created by the group was improved making it possible to evaluate in a practical way and in real time polymer blends in solid films and morphology of some blends and polymeric composites during extrusion. / A morfologia de sistemas poliméricos polifásicos é usualmente avaliada através de métodos de caracterização off-line, tal como a microscopia, os quais demandam muito tempo para a preparação das amostras e para a análise dos resultados. Este trabalho teve como principal objetivo o aperfeiçoamento de um detector óptico para medida em tempo real da morfologia de misturas e compostos poliméricos no processamento por extrusão, através do espalhamento de luz laser em baixo ângulo (LALLS). Tal equipamento inclui hardware e software e baseia-se na medida da intensidade da luz que provém de um laser e que é espalhada através do material fundido e sob fluxo. Os sinais são coletados por um arranjo de 91 fotodetectores, enviados a um computador, e apresentados em tempo real num gráfico tridimensional da intensidade de luz espalhada formando uma superfície definida por 321 pontos. Ao se analisar o perfil de espalhamento tem-se valiosas informações que ajudam elucidar a morfologia das partículas de segunda fase presentes. O detector de LALLS foi testado em bancada com o uso de amostras-padrão, as quais foram elaboradas de maneira que um de seus parâmetros (orientação, concentração de segunda fase, tamanho de partícula dispersa ou tipo de partícula dispersa) tivesse sido alterado de forma conhecida. Isso permitiu o estudo sistematizado dessas amostras e a validação do dispositivo detector. Por fim, o dispositivo foi testado em tempo real no processo de extrusão, sob diferentes condições materiais e de operação. Com isso, o dispositivo detector de LALLS criado pelo grupo foi aperfeiçoado possibilitando avaliar-se de forma prática e em tempo real: a morfologia de misturas poliméricas na forma de filmes sólidos e algumas misturas e compostos poliméricos durante a extrusão.

The current study focus on investigating a relationship between processing variables and microstructure evolution mechanism in 304L stainless steel subjected to hot torsion. The Gleeble 3800 with Mobile Torsion Unit (MTU) is utilized in the current study to conduct hot torsion test of 304L stainless steel. Samples are rotated at 1100℃ in the shear strain rate range of 0.02s-1 to 4.70s-1 and the shear strain range of 0.5 to 4. Orientation imaging microscopy (OIM) technique is used to collect and analyze the microstructure. At low strains (≤1) and strain rate (0.02s-1), average grain size remains relatively constant, but the lengths of DSs and LABs increase within grains. These are characteristics of the dynamic recovery (DRV). With increasing strain and strain rate, the lengths of DSs, LABs and HABs increase, accompanied by the decrease of average grain size. Subgrains with HAB segments are observed. These are characteristics of continuous dynamic recrystallization (CDRX). At strain rates greater than or equal to 0.94s-1, the fraction of deformation texture is about 3 times higher than that of rotated cube texture. The average grain size increases relative to that at a strain rate of 0.20s-1, accompanied by the increase of twin length per area. This indicates that grain growth take place after CDRX. Sigma phase is not observed in the current study due to the lack of static recrystallization (SRX) and the higher cooling rate.

<p>Low angle grain boundary (LAGB) mobility is an essential parameter for developing the analytical models that describe the kinetics of recovery and predict the nucleation of recrystallized grains. The thesis is aimed at the molecular dynamics (MD) simulations study of LAGB mobility determination in pure Al and Al-Mg alloys. All the previous experimental studies reported that the presence of several defects, such as solutes and dislocations, retard the boundary motion and provide lower mobility. However, very few studies have been conducted in MD simulation to capture the interactions of those defects with the migrating grain boundary. This thesis is focused on providing complete understanding of LAGB determination along with a comprehensive explanation of solute and dislocation retarding effects on boundary motion.</p> <p>The LAGB mobility in pure Al was computed from two different MD techniques as a function of temperature and misorientation. Within numerical uncertainties, both techniques provide the same magnitude of mobility at 300K for 7.785^o boundary and at 700K for 23.07^o boundary. It was observed that ADF method is not applicable to determine LAGB mobility at high temperature due to failure of order parameter computation. The MD derived activation energy is found to be approximately ten times lower than the experimental observations.</p> <p>A strong solute pinning effect on boundary motion was observed at all misorientations and solute concentrations studied in Al-Mg alloys. An approximate linear relationship is found between the restraining force and the solute concentration in a distributed solute approach. In addition, the extrinsic dislocations are found to completely pin both 7.785^o and 23.07^o boundary motion at low driving forces in pure Al at 300K. The MD results do not reveal significant qualitative differences of the pinned boundary structure for the low and high angle boundaries and will be discussed in terms of the previous experimental observations.</p> / Doctor of Philosophy (PhD)

In the present work, deformation behavior, texture and microstructure evolution of commercially pure titanium (CP Ti) are investigated by electron backscattered diffraction (EBSD) after compression tests at elevated temperatures. By analysing work hardening rate vs. flow stress, the deformation behaviour can be divided into three groups, viz. three-stage work hardening, two-stage work hardening and flow softening. A new deformation condition map is presented, dividing the deformation behavior of CP Ti into three distinct zones which can be separated by two distinct values of the Zener-Hollomon parameter. The deformed microstructures reveal that dynamic recovery is the dominant deformation mechanism for CP Ti during hot working. It is the first time that the Schmid factor and pole figures are used to analyse how the individual slip systems activate and how their activities evolve under various deformation conditions. Two constitutive equations are proposed in this work, one is for single peak dynamic recrystallization (DRX), the other is specially for CP Ti deformed during hot working. After the hot compression tests, some stress-strain curves show a single peak, leading to the motivation of setting up a DRX model. However, the examinations of EBSD maps and metallography evidently show that the deformation mechanism is dynamic recovery rather than DRX. Then, the second model is set up. The influence of the deformation conditions on grain size, texture and deformation twinning is systematically investigated. The results show that {10-12} twinning only occurs at the early stage of deformation. As the strain increases, the {10-12} twinning is suppressed while {10- 11} twinning appears. Three peaks are found in the misorientation frequency-distribution corresponding to basal fiber texture, {10-11} and {10-12} twinning, respectively. A logZ-value of 13 is found to be critical for both the onset of {10-11} compressive twinning and the break point for the subgrain size. The presence of {10-11} twinning is the key factor for effectively reducing the deformed grain size. The percentage of low angle grain boundaries decreases with increasing Z-parameter, falling into a region separated by two parallel lines with a common slope and 10% displacement. After deformation, three texture components can be found, one close to the compression direction, CD, one 10~30° to CD and another 45° to CD. / QC 20100819