Hydrogen embrittlement (HE), which results in an unpredictable failure of metals, has been a major limitation in the design of critical components for a wide range of engineering applications, given the near-ubiquitous presence of hydrogen in their service environments. However, the exact mechanisms that underpin HE failure remain poorly understood. It is known that hydrogen, when free to diffuse in these materials, can tend to concentrate at a crack tip front. In turn, this facilitates crack propagation. Hence one of the proposed strategies for mitigating HE is to limit the content of freely diffusing hydrogen within the metal atomic lattice via the introduction of microstructural hydrogen traps. Further, it is empirically known that the introduction of finely-dispersed distribution of nano-sized carbide hydrogen traps in ferritic steel matrix can improve resilience to HE. This resilience has been attributed to the effective hydrogen trapping of the carbides. However, conclusive atomic-scale experimental evidence is still lacking as to the manner by which these features can impede the movement of the hydrogen. This lack of insight limits the further progress for the optimisation of the microstructural design of this type of HE-resistant steel. In order to further understand the hydrogen trapping phenomenon of the nano-sized carbide in steel, an appropriate characterisation method is required. Atom probe tomography (APT) has been known for its powerful combination of high 3D spatial and chemical resolution for the analysis of very fine precipitates. Furthermore, previous studies have shown that the application of isotopic hydrogen (²H) loading techniques, combined with APT, facilitates the hydrogen signal associated to fine carbides to be unambiguously identified. However, the considerable experimental requirements as utilised by these previous studies, particularly the instrumental capability necessary for retention of the trapped hydrogen in the needle-shaped APT specimen, limits the study being reproduced or extended. In this APT study, a model ferritic steel with finely dispersed V-Mo-Nb carbides of 10-20 nm is investigated. Initially, existing specialised instrumentation formed the basis of a cryogenic specimen chain under vacuum, so as to retain loaded hydrogen after an electrolytic charging treatment for APT analysis. This work confirms the importance of cryogenic treatment for the retention of trapped hydrogen in APT specimen. The quality of the obtained experimental data allows a quantitative analysis on the hydrogen trapping mechanism. Thus, it is conclusively determined that interior of the carbides studied in this steel acts as the hydrogen trapping site as opposed to the carbide/matrix interface as commonly expected. This result supports the theoretical investigations proposing that the hydrogen trapping within the carbide interior is enabled by a network of carbon vacancies. Based on the established importance of the specimen cold chain in these APT experiments, this work then successfully develops a simplified approach to cryo-transfer which requires no instrumental modification. In this approach there is no requirement for the charged specimen to be transferred under vacuum conditions. The issue of environmental-induced ice contamination on the cryogenic sample surface in air transfer is resolved by its sublimation in APT vacuum chamber. Furthermore, the temperature of the transferred sample is able to be determined independently by both monitoring changes to vacuum pressure in the buffer chamber and also the thermal response of the APT sample stage in the analysis chamber. This simplified approach has the potential to open up a range of hydrogen trapping studies to any commercial atom probe instrument. Finally, as an example of the use of this simplified cryo-transfer technique, targeted studies for determining the source of hydrogen adsorption during electropolishing and electrolytic loading process are demonstrated. This research provides a critical verification of hydrogen trapping mechanism of fine carbides as well as an achievable experimental protocol for the observation of the trapping of individual hydrogen atoms in alloy microstructures. The methods developed here have the potential to underpin a wide range of possible experiments which address the HE problem, particularly for the design of new mitigation strategies to prevent this critical issue.

Masters of Science / Nampak packages millions of cans a year and a very small percentage of these cans fail due to many reasons. One of the main reasons that cause 2- piece food cans to fail is split flanges. Split Flanges arises due to a number of reasons which will be discussed in detail.The focus of this thesis was based on the causes of split flanges in 2-piece food cans. A study on manufacturing the steel and can making together with packaging fish in these cans was conducted. Another study on the reasons for split flanges occurring in 2 piece cans was conducted done as well.The purpose of the investigation was to check if hydrogen embrittlement could be the cause for split bodies forming in 2 piece food cans. 2 piece cans are drawn and wall ironed from tinplate; the cans were made up of a top and a shaped body. It was this shaped body that went through a considerable amount of stress during manufacture especially at the top of the can, which gave an explanation to why the cans split at the curved area near the flange of the can.According to previous studies done at Nampak R&D more complaints about split bodies were coming from the Fish canneries on the West Coast than the Vegetable canneries. These canneries used the exact same cans to package their product. The difference between the processes at these canneries was the exhaust boxes at the fish canneries. The exhaust box is a long tunnel filled with steam used to precook the fish; the vegetables are not precooked in exhaust boxes. Non metallic inclusions (NMI) was one of the main reason for these split flanges to occur and a reason of particular interest in this research.NMI’s were distributed throughout the steel of the cans and since the same cans were used for the fish and vegetable canneries, they should be failing at the same rate. Yet only complaints came from the fish canneries. So the primary focus of the research was to check if the additional steam process contributed to the formation of split bodies / flanges. We proposed to investigate if hydrogen atoms collect at grain boundaries, vacancies and non metallic inclusions and also to check if the steam accelerated embrittlement. Hydrogen is believed to penetrate right into the bare steel of the cans that were exposed to steam.Hydrogen atoms are being investigated because of their small size, their ability to diffuse through a metal lattice and form hydrogen molecules within the intermetallic vacancies of the metal. The molecules of hydrogen, once formed within the internal structure of the metal, remain trapped because of their larger size and can generate a significant pressure that can contribute to the formation of split bodies. [1] The first step to prove whether H-embrittlement was present in the cans was to check if hydrogen was present. A spectroscopic method namely, elastic recoil detection analysis (ERDA) was used to check if H could be detected using the Elastic Recoil Detection Analysis technique. Several experiments were designed to make sure the technique was suitable for the detection of H. Even though it is known that all metals are susceptible to corrosion and Hembrittlement, the tinplate metals had to be checked in an environment similar to the exhaust box (suspected area causing hydrogen embrittlement) in the factories.Further characterization was done using X-Ray Diffraction to measure the residual stress and relate it to the effects of H-embrittlement. If the H had penetrated into the metal it would cause some distortion in the atomic distances between the atomic planes in Fe atoms and can be measured using XRD.Another effect of hydrogen embrittlement is to reduce the strength in the metal. Tensile tests were performed to measure the strengths of the metal.

M. S.

Acoustic emission activity resulting from plastic deformation of mild steel disks that were clamped and then pressurized from one side with either hydrogen or nitrogen was recorded and analyzed. It was found that during monotonic pressurization of disks in nitrogen gas, more cumulative counts were recorded than for similar disks pressurized in hydrogen gas. Possible signatures of the "births" of cracks were observed during hydrogen pressurization of disks that typically failed by leaking. The records of the nitrogen tests show very high energy and high count events occurring early in the deformation process. These events are believed to be the result of the breaking away of near-surface dislocations that had been pinned by nitrogen. The disks tested in nitrogen typically failed by bursting (ductile failure) while those tested in hydrogen typically failed by leaking ("brittle" failure). / M.S.

Electrolytic charging of hydrogen, at room temperature and in the absence of externally applied stress, induced surface cracking in 316 stainless steel and cobalt based ZIMALOY. Hot Isostatic Pressed (H.I.P.) ZIMALOY showed less susceptibility to surface cracking than 316 stainless steel samples. The susceptibility of 316 stainless steel to surface cracking was determined with samples in the High Energy Rate Forged (HERF), the sensitized, the annealed, and the annealed and sensitized conditions. Investigations showed that surface cracking typically occurred at specific microstructural features. Hence, the relative susceptibilities of twin boundaries, slip bands, grain boundaries, and heavily sensitized regions was established. It was observed that twin boundaries crack most readily in non-sensitized samples, and that both grain boundaries and twin boundaries crack easily in sensitized structures. These observations, coupled with the similarity between hydrogen embrittlement and failure of orthopedic implants, suggest that orthopedic applications should use H.I.P. ZIMALOY in preference to 316 stainless steel whenever possible, and that when the use of 316 stainless steel is unavoidable, HERFed parts should be used. Further investigations are recommended to better assess the hydrogen compatibility of sensitized 316 stainless steel, and to determine the influence of sensitization on the suitability of 316 stainless steel for orthopedic application. / Master of Science

M.S.

No description available.

Titanium alloys are highly resistant to all types of corrosion due to their excellent ability to form an oxide film on the surface. However, under certain circumstances, these alloys may experience an environmental degradation which could potentially, under the application of mechanical stress, lead to a complete failure of the material. One of these cracking processes is stress-corrosion cracking (SCC). SCC has an embrittling effect on otherwise ductile materials under tensile stress. Since titanium alloys are frequently used in the aerospace industry and it is therefore of interest to test these alloys in different environment in order to prevent any future accidents. SCC testing is frequently tested at GKN Aerospace and a new testing method is of interest. The main objective with this work was to gain knowledge of the testing method. Bent-beam testing method has been used to investigate stress-corrosion cracking (SCC) of titanium alloys in a laboratory based experiment. The bent-beam testing method was of type 2-point bent beam test, where a saline solution was applied at the apex of the specimen. The specimens were loaded to a range of stresses from 40%, to 95% of the materials yield strength and the salt concentration in the saline solution was 1wt% and 3wt%. By doing so, a relative susceptibility of the different alloys could be established. Three different titanium alloys were tested: Ti-6Al-4V, Ti-8Al-1Mo-1V, and Ti-6Al-2Sn-4Zr-2Mo. The testing method was able to cause cracking on all titanium alloys, where Ti-6Al-4V was found to be the least susceptible to SCC. Ti-8Al-1Mo-1V, and Ti-6Al-2Sn-4Zr-2Mo showed an overall high susceptibility to SCC as cracking occurred in all testing configurations. Cracking was observed on both the surface of the specimen as well as in the cross sections, where the cracks grew perpendicular to the surface. SEM was also used to evaluate the crack propagation in Ti-8Al-1Mo-1V, and Ti-6Al-2Sn-4Zr-2Mo, and it was found that the cracks grew mostly along the grain boundaries.

Thesis (Sc.D.)--Massachusetts Institute of Technology, Dept. of Mechanical Engineering, 1981. / MICROFICHE COPY AVAILABLE IN ARCHIVES AND ENGINEERING. / Includes bibliographical references. / by Subramanian Suresh. / Sc.D.

Hydrogen embrittlement is a mechanism by which hydrogen enters a metal, causing a loss in strength and ductility. This phenomenon is of great concern to the oil and gas industry as deep-sea wells operate in high temperature, highly acidic and high stress conditions. Nickel-based superalloys are ideal for use in such environments due to their high strength and exceptional resistance to both corrosion and hydrogen embrittlement. Alloy 945X is a newly developed nickel-based superalloy that has been specifically designed for use in downhole applications. This thesis compares the performance of hydrogenated Alloy 945X with the more established oil and gas grade Alloy 718. The hydrogenating environment of an oil well was simulated via cathodic polarisation. The effect of hydrogen content on the tensile performance of both alloys was studied, alongside fracture and microstructural analysis. A new video-recording technique was employed to investigate the crack initiation and propagation behaviour of both alloys, alongside in-SEM tensile testing. The diffusive nature of hydrogen in Alloy 945X and Alloy 718 was explored. With the use of a ppm-sensitive hydrogen analyser, it was possible to measure the rate at which hydrogen enters and outgassed from both materials as well as the saturation conentrations. Outgassing behaviour was also examined using X-ray diffraction and nano-indentation. The depth of brittle fracture in cathodically charged tensile specimens was correlated with Fick’s diffusion calculations and the critical concentration for embrittlement calculated. In a similar method, a parameter (based on diffusion coefficient calculations) that describes the rate of embrittlement in a material was proposed.