Ferritic stainless steel is typically used in the automotive industry to fabricate welded tube that is plastically deformed for flanging, bending and necking. The effect of welding parameters during autogenous gastungsten arc welding (GTAW) of thin sheet on the weld metal structure and tensile properties were determined. Two grades of ferritic stainless steels, a titanium-containing Grade 441 and a titanium-free molybdenum-containing Grade 436, were used as base metal. Statistical analysis was used to determine the influence of welding parameters on the microstructure of autogenous GTAW welds. The results of Grade 441 indicated that the welding speed and peak welding current had a statistically significant influence on the amount of equiaxed grains that formed. For Grade 436, the same welding parameters (welding speed and peak welding current) had a statistically significant influence on the grain size of the weld metal grains. The ductility of a tensile test coupon machined parallel to the weld direction, for both base metal grades, was unaffected by the welding parameters or the weld metal microstructure. The elongation was determined by the amount of weld metal in the gauge area of a tensile coupon. The titanium content of the base material seems to have the most significant effect on the formation of equiaxed grains. / Dissertation (MEng)--University of Pretoria, 2019. / Materials Science and Metallurgical Engineering / MEng / Unrestricted

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Materials to be used in thermal power plants have to resist creep deformation for time periods up to 30 years. The role of alloying elements for creep strength of 9-12% Cr steels is analysed. The creep strength in these steels relies on minor additions of alloying elements. Precipitates give rise to the main strengthening and remaining elements produce solid solution hardening. Nucleation, growth and coarsening of particles are predicted by thermodynamic modelling. Phase fractions and size distributions of M23C6 carbides, MX carbonitrides and Laves phase are presented. The size distributions are needed in order to determine the particle hardening during creep. At elevated temperatures the climb mobility is so high that the dislocations can climb across particles instead of passing by making Orowan loops. By solving Fick's second law the concentration profile around a moving dislocation can be determined. The results show an accumulation of solutes around the dislocation that slows down dislocation movement. When Laves phase grows a decrease in creep strength is observed due to a larger loss in solid solution hardening than strength increase by particle hardening. Solid solution hardening also gives an explanation of the low dislocation climb mobility in 9-12% Cr steels. Three different dislocation types are distinguished, free dislocations, immobile dislocation and immobile boundary dislocations. This distinction between types of dislocations is essential in understanding the decreasing creep with strain during primary creep. The empirical relation with subgrain size inversely proportional to stress has been possible to predict. The total creep strength can be predicted by adding the contribution from individual mechanisms. / QC 20101112

Nanostructured ferritic alloy and silicon carbide composite materials (NFA-SiC) were sintered with spark plasma sintering (SPS) method and systematically investigated through X-ray diffraction (XRD), scanning electron microscopy (SEM), as well as density and Vickers hardness tests. Pure NFA, pure SiC, and their composites NFA-SiC with different compositions (2.5 vol% NFA-97.5 vol% SiC, 5 vol% NFA-95 vol% SiC, 97.5 vol% NFA-2.5 vol% SiC, and 95 vol% NFA-5 vol% SiC) were successfully sintered through SPS. In the high-NFA samples, pure NFA and NFA-SiC, minor gamma-Fe phase formation from the main alfa-Fe matrix occurred in pure NFA 950 degree C and 1000 degree C. The densities of the pure NFA and NFA-SiC composites increased with sintering temperature but decreased with SiC content. The Vickers hardness of the pure NFA and NFA-SiC composites was related to density and phase composition. In the high-SiC samples, NFA addition of 2.5 vol% can achieve full densification for the NFA-SiC samples at relative low temperatures. With the increase in sintering temperature, the Vickers hardness of the pure SiC and NFA-SiC composite samples were enhanced. However, the NFA-SiC composites had relative lower hardness than the pure SiC samples. A carbon layer was introduced in the NFA particles to prevent the reaction between NFA and SiC. Results indicated that the carbon layer was effective up to 1050 degree C sintering temperature. Green samples of gradient-structured NFA-SiC composites were successfully fabricated through slip casting of an NFA-SiC co-suspension. / Master of Science

Silicon carbide and nanostructured ferritic alloy (SiC-NFA) composites have the potential to maintain the outstanding high temperature corrosion and irradiation resistance and enhance the mechanical integrity for nuclear cladding. However, the formation of detrimental silicide phases due to reaction between SiC and NFA remains a major challenge. By introducing a carbon interfacial barrier on NFA (C@NFA), SiC-C@NFA composites are investigated to reduce the reaction between SiC and NFA. In a similar way, the effect of chromium carbide (Cr3C2) interfacial barrier on SiC (Cr3C2@SiC) is also presented for Cr3C2@SiC-NFA composites. Both the coatings were successful in suppressing silicide formation. However, despite the presence of coatings, SiC was fully consumed during spark plasma sintering process. TEM and EBSD investigations revealed that spark plasma sintered SiC-C@NFA and Cr3C2@SiC-NFA formed varying amounts of different carbides such as (Fe,Cr)7C3, (Ti,W)C and graphite phases in their microstructure. Detailed microstructural examinations after long term thermal treatment at 1000oC on the microstructure of Cr3C2@SiC-NFA showed precipitation of new (Fe,Cr)7C3, (Ti,W)C carbides and also the growth of existing and new carbides. The results were successfully explained using ThermoCalc precipitation and coarsening simulations respectively. The oxidation resistance of 5, 15 and 25 vol% SiC@NFA and Cr3C2@SiC-NFA composites at 500-1000oC temperature under air+45%water vapor containing atmosphere is investigated. Oxidation temperature effects on surface morphologies, scale characteristics, and cross-sectional microstructures were investigated and analyzed using XRD and SEM. SiC-C@NFA showed reduced weight gain but also showed considerable internal oxidation. Cr3C2@SiC-NFA composites showed a reduction in weight gain with the increasing volume fraction of Cr3C2@SiC (5, 15 and 25) without any indication of internal oxidation in the microstructure. 25 vol% SiC-C@NFA and 25 vol% Cr3C2@SiC-NFA showed over 90% and 97% increase in oxidation resistance (in terms of weight gain) as compared to NFA. The results were explained using the fundamental understanding of the oxidation process and ThermoCalc/DICTRA simulations. Finally, the irradiation performance of SiC-C@NFA and Cr3C2@SiC-NFA composites was assessed in comparison with NFA using state-of-the-art TEM equipped with in-situ ion irradiation capability. Kr++ ions with 1 MeV energy was used for irradiation experiments. The effect of ion irradiation was recorded after particular dose levels (0-10 dpa) at 300oC and 450oC temperatures. NFA sample showed heavy dislocation damage at both 300oC and 450oC increasing gradually with dose levels (0-10 dpa). Cr3C2@SiC-NFA showed similar behavior as NFA at 300oC. However, at 450oC, Cr3C2@SiC-NFA showed remarkably low dislocation loop density and loop size as compared to NFA. At 300oC, microstructures of NFA and Cr3C2@SiC-NFA show predominantly 1/2<111> type dislocation loops. At 450oC, NFA showed predominantly <100> type loops, however, Cr3C2@SiC-NFA composite was still predominant in ½<111> loops. The possible reasons for this interesting behavior were discussed based on the large surface sink effects and enhanced interstitial-vacancy recombination at higher temperatures. The molecular dynamics simulations did not show considerable difference in formation energies of ½<111> and <100> loops for NFA and Cr3C2@SiC-NFA composites. The additional Si element in the SiC-NFA sample could have been an important factor in determining the dominant loop types. SiC-C@NFA composites showed heavy dislocation damage during irradiation at 300oC. At 450oC, SiC-C@NFA showed high dislocation damage in thicker regions. Thinner regions near the edge of TEM samples were largely free from dislocation loops. The precipitation and growth of new (Ti,W)C carbides were observed at 450oC with increasing irradiation dose. (Fe,Cr)7C3 precipitates were largely free from any dislocation damage. Some Kr bubbles were observed inside (Fe,Cr)7C3 precipitates and at the interface between α-ferrite matrix and carbides ((Fe,Cr)7C3, (Ti,W)C). The results were discussed using the fundamental understanding of irradiation and ThermoCalc simulations. / Doctor of Philosophy / With the United Nations describing climate change as 'the most systematic threat to humankind', there is a serious need to control the world's carbon emissions. The ever increasing global energy needs can be fulfilled by the development of clean energy technologies. Nuclear power is an attractive option as it can produce low cost electricity on a large scale with greenhouse gas emissions per kilowatt-hour equivalent to wind, hydropower and solar. The problem with nuclear power is its vulnerability to potentially disastrous accidents. Traditionally, fuel claddings, rods which encase nuclear fuel (e.g. UO2), are made using zirconium based alloys. Under 'loss of coolant accident (LOCA) scenarios' zirconium reacts with high temperature steam to produce large amounts of hydrogen which can explode. The risks associated with accidents can be greatly reduced by the development of new accident tolerant materials. Nanostructured ferritic alloys (NFA) and silicon carbide (SiC) are long considered are leading candidates for replacing zirconium alloys for fuel cladding applications. In this dissertation, a novel composite of SiC and NFA was fabricated using spark plasma sintering (SPS) technology. Chromium carbide (Cr3C2) and carbon (C) coatings were employed on SiC and NFA powder particles respectively to act as reaction barrier between SiC and NFA. Microstructural evolution after spark plasma sintering was studied using advanced characterization tools such as scanning electron microscopy (SEM), electron backscattered diffraction (EBSD), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) techniques. The results revealed that the Cr3C2 and C coatings successfully suppressed the formation of detrimental reaction products such as iron silicide. However, some reaction products such as (Fe,Cr)7C3 and (Ti,W)C carbides and graphite retained in the microstructure. This novel composite material was subjected to high temperature oxidation under a water vapor environment to study its performance under the simulated reactor environment. The degradation of the material due to high temperature irradiation was studied using state-of-the-art TEM equipped with in-situ ion irradiation capabilities. The results revealed excellent oxidation and irradiation resistance in SiC-NFA composites as compared to NFA. The results were discussed based on fundamental theories and thermodynamic simulations using ThermoCalc software. The findings of this dissertation imply a great potential for SiC-NFA based composites for future reactor material designs.

The mechanical behavior of structural materials used in nuclear applications is significantly degraded as a result of irradiation, typically characterized by an increase in yield stress, localization of inelastic deformation along narrow dislocation channels, and considerably reduced strains to failure. Further, creep rates are accelerated under irradiation. These changes in mechanical properties can be traced back to the irradiated microstructure which shows the formation of a large number of material defects, e.g., point defect clusters, dislocation loops, and complex dislocation networks. Interaction of dislocations with the irradiation-induced defects governs the mechanical behavior of irradiated metals. However, the mechanical properties are seldom systematically correlated to the underlying irradiated microstructure. Further, the current state of modeling of deformation behavior is mostly phenomenological and typically does not incorporate the effects of microstructure or defect densities. The present research develops a continuum constitutive crystal plasticity framework to model the mechanical behavior and deformed microstructure of bcc ferritic/martensitic steels exposed to irradiation. Physically-based constitutive models for various plasticity-induced dislocation migration processes such as climb and cross-slip are developed. We have also developed models for the interaction of dislocations with the irradiation-induced defects. A rate theory based approach is used to model the evolution of point defects generated due to irradiation, and coupled to the mechanical behavior. A void nucleation and growth based damage framework is also developed to model failure initiation in these irradiated materials. The framework is used to simulate the following major features of inelastic deformation in bcc ferritic/martensitic steels: irradiation hardening, flow localization due to dislocation channel formation, failure initiation at the interfaces of these dislocation channels and grain boundaries, irradiation creep deformation, and temperature-dependent non-Schmid yield behavior. Model results are compared to available experimental data. This framework represents the state-of-the-art in constitutive modeling of the deformation behavior of irradiated materials.

This thesis describes the metallurgical and environmental factors that influence hydrogen embrittlement of super duplex stainless steels and presents a model to predict the rate at which embrittlement occurs. Super duplex stainless steel has an austenite and ferrite microstructure with an average fraction of each phase of approximately 50%. An investigation was carried out on the metallurgical and environmental factors that influence hydrogen embrittlement of super duplex stainless steels. Tensile specimens of super duplex stainless steel were pre-charged with hydrogen for two weeks in 3.5% NaCl solution at 50º C at a range of applied potentials to simulate the conditions that exist when subsea oilfield components are cathodically protected in seawater. The pre-charged specimens were then tested in a slow strain rate tensile test and their susceptibility to hydrogen embrittlement was assessed by the failure time, reduction in cross-sectional area and examination of the fracture surface. The ferrite and austenite in the duplex microstructures were identified by analysing their Cr, Ni, Mo and N contents in an electron microscope, as these elements partition in different concentrations in the two phases. It was shown that hydrogen embrittlement occurred in the ferrite phase, whereas the austenite failed in a ductile manner. An embrittled region existed around the circumference of each fracture surface and the depth of this embrittlement depended on the hydrogen charging time and the potential at which the charging had been carried out. The depth of embrittlement was shown to correlate with the rate of hydrogen diffusion in the alloy, which was measured electrochemically using hydrogen permeation and galvanostatic methods. A two-dimensional diffusion model was used to calculate the hydrogen distribution profiles for each experimental condition and the model could be employed to provide predictions of expected failure times in stressed engineering components.

In this thesis, the heat affected zone (HAZ) of Gleeble simulated welds, the weldments and the creep specimens for several types of 9%-12% Cr ferritic steels were studied by focusing on the Type IV cracking in the fine grained zone (FZ). The field emission gun transmission electron microscopy (FEGTEM) and scanning electron microscopy (SEM) were used to measure the phosphorus segregation on the grain boundary (GB) and the creep fracture morphologies respectively. Meanwhile the well-developed grain boundary segregation and precipitation (GBSP) model was applied to simulate the experimental results. The experimental results have showed that the HAZ zone was characterised by softening and Type IV cracking. All the high Cr ferritic steel welds gave a microstructure of mainly tempered martensite and M23C6 precipitates after the post weld heat treatment (PWHT). There was no δ-ferrite observed in the HAZ. The Type IV cracking exhibited a mixed cracking mechanism in which the intergranular grain boundary separation is dominant due to the crack initiation by voids and the faster M23C6 growth with the service time. A new model on the mechanism of the Type IV cracking is established. The FEGTEM research has also showed obvious non-equilibrium phosphorus segregation at the grain boundaries, which is affected significantly by the quenching temperature. The phosphorus GB segregation deteriorates the weak grain boundaries. The experimental results were well in agreement with the GBSP modelling.