The hydrogen embrittlement of two HSLA steels was studied in conditions typical of the marine environment. Double cantilever beam specimens, heat treated to produce the microstructure in the heat affected zone of a weld, were tested in seawater containing sulphate reducing bacteria (SRB) over a range of cathodic protection (CP) potentials and the threshold stress intensities ([Threshold Stress Intensity]) were recorded. The hydrogen concentration absorbed by the steel ([Surface Hydrogen Concentration]) was measured and shown to be higher at more negative CP potentials and significantly increased when SRB were present. An inverse relationship was established between log [Threshold Stress Intensity] and [Surface Hydrogen Concentration]. It was concluded that crack propagation occurs by a single mechanism whether or not SRB are present. Three point bend specimens of both steels were machined from welded plate. Corrosion fatigue tests were carried out in seawater with and without SRB. The presence of active SRB caused increased crack growth rates. Sediment samples were collected from the River Mersey and the base of a North Sea platform. In addition, SRB were added as an inoculum to artificial seawater. SRB numbers were enumerated and their activities assessed by measuring the concentrations of sulphide generated. Hydrogen permeation tests were performed on steel held at a range of CP potentials and exposed to each environment. Measurements were also carried out in seawater containing chemically prepared sulphides. Hydrogen absorption was shown to be enhanced when SRB were present and to be related to the total sulphide (TS) concentration in the environment. High hydrogen concentrations were produced by chemically prepared sulphides and the nature and thickness of the sulphide film appeared to be important in determining the extent of hydrogen absorption. Chemically produced sulphide gave sustained levels of absorbed hydrogen, but those generated biogenically decayed rapidly unless the TS concentration was maintained in the solution.

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Dans un contexte industriel en évolution permanente, les aciers austénitiques Fe-Mn-C sont développés afin d’obtenir une résistance mécanique élevée tout en conservant une ductilité considérable. Cependant, ces aciers présentent une sensibilité à différentes formes d'endommagement par l'hydrogène, notamment la corrosion sous contrainte. L'objectif de cette étude est de caractériser l'influence de la composition chimique et de l'état microstructural de ces alliages sur leur sensibilité aux phénomènes de fragilisation par l’hydrogène (FPH), lorsqu’ils sont soumis à des phénomènes de corrosion aqueuse. Ce travail est introduit par une présentation générale de la métallurgie des aciers austénitiques Fe-Mn-C ainsi que des méthodes expérimentales utilisées. Le traçage isotopique de l’hydrogène avec du deutérium par analyse SIMS a permis d’étudier les mécanismes de diffusion de l’hydrogène dans ces alliages. L’étude du comportement en corrosion aqueuse de ces alliages, par des tests électrochimiques et des immersions au potentiel libre dans des environnements aqueux deutérés, a mis en évidence l’influence des éléments d’addition sur la prise d’hydrogène associée à la corrosion.La sensibilité à la FPH de ces aciers a été caractérisée par des essais de traction in situ. Ils montrent que les interactions hydrogène-plasticité ont un rôle essentiel sur les mécanismes régissant la FPH. Cette étude a également montré une forte influence des éléments d’addition sur la FPH. Finalement, les résultats de cette étude nous ont permis de discuter des mécanismes associés à l’influence des éléments d’addition sur la sensibilité à la FPH de ces aciers. / The automotive industry is a sector in constant evolution, in which the lightening of structures by the use of new alloys, in order to save energy, is one of the main objectives. In this context, austenitic Fe-Mn-C steels are developed in order to obtain high mechanical strength associated with considerable ductility. However, these steels are sensitive to different forms of hydrogen damage, in particular stress corrosion cracking. The objective of this study is to characterize the influence of the chemical composition and the microstructural state of these alloys on their sensitivity to hydrogen embrittlement (HE) phenomena associated with corrosion process in aqueous media. This work starts with a general presentation of the metallurgical properties of austenitic Fe-Mn-C steels and of the experimental techniques. Then, the isotopic tracing of hydrogen with deuterium by SIMS analysis allowed studying hydrogen diffusion mechanisms in these alloys. The corrosion of these steels in aqueous media have been studied by electrochemical tests and immersions at the rest potential in deuterated solution ; the influence of alloying elements on the hydrogen absorption during corrosion war characterized in detail. In situ tensile tests were used to characterize the HE susceptibility of these steels. They show that hydrogen-plasticity interactions play a predominant role in the HE mechanisms. This study also showed a strong influence of alloying elements on HE. Finally, the results of this study allowed discussing the mechanism involved in the role of alloying elements on the HE susceptibility of these steels.

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Incremental step load testing was used in accordance with ASTM F1940 to rank a number coating processes used in the fastener industry for their propensity to cause internal hydrogen embrittlement. The results showed that coating permeability has a first order effect, while the quantity of hydrogen introduced by the process has a second order effect. Pure zinc electroplating processes, alkaline and acid, were found to be the most embrittling, owing to the low permeability of zinc. The least embrittling processes were zinc-nickel, alkaline and acid, owing to the high permeability of Zn-Ni coatings. Non-electrolytic processes, namely phosphating, mechanical galvanising, DacrometRTM and Magni 555RTM were found to be non-embrittling. Hot dip galvanising was found to be highly embrittling, evidently due to trapped hydrogen being released by the thermal shock of up-quenching upon immersion in molten zinc. The full effect of up-quenching on the metallurgical and mechanical properties of high strength steel requires further investigation.

Pulse plated nickel and nickel based superalloys have been used extensively in the Ariane 5 space launcher engines. Large structural Ariane 5 space launcher engine components such as combustion chambers with complex microstructures have usually been manufactured using electrodeposited nickel with advanced pulse plating techniques with smaller parts made of nickel based superalloys joined or welded to the structure to fabricate Ariane 5 space launcher engines. One of the major challenges in manufacturing these space launcher components using newly developed materials is a fundamental understanding of how different materials and microstructures react with hydrogen during welding which can lead to hydrogen induced cracking. The main objective of this research has been to examine and interpret the effects of microstructure on hydrogen diffusion and hydrogen embrittlement in (i) nickel based superalloy 718, (ii) established and (iii) newly developed grades of pulse plated nickel used in the Ariane 5 space launcher engine combustion chamber. Also, the effect of microstructures on hydrogen induced hot and cold cracking and weldability of three different grades of pulse plated nickel were investigated. Multiscale modelling and experimental methods have been used throughout. The effect of microstructure on hydrogen embrittlement was explored using an original multiscale numerical model (exploiting synthetic and real microstructures) and a wide range of material characterization techniques including scanning electron microscopy, 2D and 3D electron back scattering diffraction, in-situ and ex-situ hydrogen charged slow strain rate tests, thermal spectroscopy analysis and the Varestraint weldability test. This research shows that combined multiscale modelling and experimentation is required for a fundamental understanding of microstructural effects in hydrogen embrittlement in these materials. Methods to control the susceptibility to hydrogen induced hot and cold cracking and to improve the resistance to hydrogen embrittlement in aerospace materials are also suggested. This knowledge can play an important role in the development of new hydrogen embrittlement resistant materials. A novel micro/macro-scale coupled finite element method incorporating multi-scale experimental data is presented with which it is possible to perform full scale component analyses in order to investigate hydrogen embrittlement at the design stage. Finally, some preliminary and very encouraging results of grain boundary engineering based techniques to develop alloys that are resistant to hydrogen induced failure are presented. Keywords: Hydrogen embrittlement; Aerospace materials; Ariane 5 combustion chamber; Pulse plated nickel; Nickel based super alloy 718; SSRT test; Weldability test; TDA; SEM/EBSD; Hydrogen induced hot and cold cracking; Multiscale modelling and experimental methods.

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The aim of this research is to identify problematic microstructural features as hydrogen traps in linepipe steel that serve to increase the hydrogen embrittlement susceptibility. A comparison is made between the hydrogen trapping capacity and associated hydrogen embrittlement susceptibility of Ca-treated X60 grade steel skelp and X70 grade steel skelp: the latter typically being more susceptible to hydrogen-induced cracking in sour environments. Through-thickness variations in the steel skelp microstructure were characterized across multi-length scales using light optical microscopy (LOM) and scanning electron microscopy (SEM) equipped with X-ray energy dispersive spectroscopy (EDS). Key features under study include the composition, shape, and distribution of non-metallic inclusions, as well as differences in features present between the quarterline (¼ and ¾ depths) and centerline (½ depth) microstructures. The type, count, and average size of inclusions present in both steel skelp grades were analyzed using an automated SEM-EDS technique called ASPEX®. Major types of inclusions detected in both grades of steel skelp include those containing Ca, Al, Mn, Mg and Ti as major elements. Overall, the area fraction of inclusions detected in the X70 steel was larger than those detected in the X60 with the exception of Ti-containing inclusions, which had a larger area fraction within the X60 steel. Comparing the number of detected inclusions shows that there was overall slightly less Ca-containing inclusions and significantly less Ti-containing inclusions detected in the X70 steel but there was generally more Al-containing, Mg-containing, and Mn-containing inclusions than those detected in the X60 steel. Thermal desorption spectroscopy (TDS) measurements were made on samples prepared from the ¼, ½, and ¾ depths of X60 and X70 steel skelps after galvanostatic cathodic charging in an As2O3-containing solution using an applied current density of −10 mA/cm2. Hydrogen release was measured using a HYDROSEEL® probe while the sample was heated from 20°C to 650°C to detect temperature values at which hydrogen gas release peaks occurred, and thus provide information on types of reversible and/or irreversible traps present. The TDS results suggests that non-metallic inclusions indeed serve as irreversible traps along with grain boundaries and dislocations, which serve as reversible traps. Hydrogen permeation measurements were also made on samples prepared from the ¼, ½, and ¾ depths after galvanostatic cathodic charging in an As2O3-containing solution using an applied current density of −10 mA/cm2. Hydrogen gas release was measured using a HYDROSEEL® probe while the sample remained at room temperature (~20°C), providing information regarding the potency of reversible hydrogen traps when subjected to a flux of hydrogen. Only reversible traps can be detected at room temperatures due to their low binding energies. Higher temperatures are required to overcome the larger binding energies associated with irreversible traps. The hydrogen permeation results indicate no significant effect of through-thickness variations in the X60 steel, but the centreline depth of the X70 steel skelp trapped a larger quantity of hydrogen than either of the two quarterline depths, indicating the presence of a distinct problematic trap. The X70 steel skelp was also observed to trap more hydrogen than the X60 steel skelp. The observed hydrogen trapping capacity was linked to the hydrogen embrittlement susceptibility by comparing the uniaxial tensile behaviour of centreline samples with and without hydrogen charging applied as a pre-treatment step. Hydrogen charging was achieved by galvanostatic cathodic polarization at an applied current density of −10 mA/cm2 for 24 h in an NH4SCN-containing solution while simultaneously loading the samples to 85% of the yield strength using a proof ring tensile test cell. An increase in hydrogen embrittlement as a result of pre-charging was confirmed through tensile plots by comparing the area of reduction and failure strain of charged samples to uncharged samples. A decrease in both values was observed in the charged samples indicating a loss in ductility as a result of hydrogen charging. Fracture surfaces were imaged using SEM and inclusions of interest were analyzed for elemental composition using EDS. Inclusions observed along the fracture surfaces include oxysulfides of Ca and Al, oxides of Mg, Al-Ca-Si oxides, and Al2O3-containing inclusions which are likely to be heterogeneous Al-Ca-O inclusions. / Thesis / Master of Applied Science (MASc)