The nucleation and growth of η phase in nickel-based superalloy during long-term thermal exposure

The microstructure degradation and subsequent phase transformations in Waspaloy nickel-based superalloy during thermal exposure at 780 °C for 10,000 h were investigated. Two paths of η phase formation in the centre of extra-large γ’ (EL-γ’) following the formation of EL-γ’ were observed: (i) η phase directly precipitated within EL-γ’ when the coalescence of γ’ reached a critical stage; (ii) η phase precipitated at the interface of small size MC carbide and EL-γ’, with both MC and η embedded inside EL-γ’. The phase transformation process including the formation of EL-γ’ were experimentally observed and the formation sequences were schematically suggested. Two criteria of η formation and growth within EL-γ’ were established: (i) stacking faults formation in the nucleation site and (ii) sufficient atom diffusion during nuclei growth. The study of kinetics of η formation through two different paths revealed the critical role of small size carbides in promoting η nucleation and growth. It is concluded that η formation may be suppressed by controlling the size and density of MC carbides during materials processing

The hierarchy of microstructure parameters affecting the tensile ductility in centrifugally cast and forged Ti-834 alloy during high temperature exposure in air

Ductility regression is the main concern in using Ti-834 titanium alloy at temperatures above 500ºC for aerospace applications. The reduction of ductility in titanium alloys at high temperatures is strongly correlated to the exposure time. In the current study the effect of prolonged exposure at 500oC on the tensile ductility of two differently processed Ti-834 alloys was investigated. In order to simulate actual Ti-834 processing routes, forged and centrifugally cast materials were used. The tensile tests were conducted on various specimens exposed at 500ºC for 100, 200 and 500 hours to observe microstructure feature changes. Moreover, the effect of microstructure, microtexture, α-case, α2 and silicide precipitate coarsening during high temperature exposure was studied thoroughly. The cast alloy was found to have a minimum ductility and failed at 1.8% strain after exposure at 500oC/500 hour when the α-case layer was retained during testing, whilst, the ductility of the forged alloy was unaffected. The effects of individual microstructural parameters on the ductility regression in Ti-834 alloy were quantified. The results showed that 7.1% strain differences between the cast and forged alloy are related to microstructural variations including; morphology, lath widths, grain size and shape, grain orientations and microtexture. A total of 9.6 % strain loss was observed in centrifugally cast Ti-834 after aging at 500ºC/500h and quantified as follow; 3.6% due to α-case formation during high temperature exposure, 0.2% due to α2-precipitates coarsening, 4.4% due to further silicide formation and coarsening, 1.4% due to additional microstructure changes during high temperature exposure. Furthermore, silicide coarsening on α/β phase boundaries caused large void formation around the precipitates. A theoretical model supported by experimental observations for silicide precipitation in fully colony and duplex microstructures was established. The element partitioning during exposure caused Al and Ti depletion in the vicinity of the β phase in the lamellae, i.e., αs area. This resulted in lowering the strength of the alloy and facilitated the formation of Ti3(SiZr)2 precipitates. The Al depletion and nano-scale partitioning observed at the αs/β boundaries resulted in easy crack initiation and promoted propagation in the centrifugally cast colony microstructure and reduced the basal slip τcrss. Furthermore, silicides were not formed in αp (high Al, Ti and low Zr areas) in the forged duplex microstructure that promoted superior mechanical performance and ductility over the cast alloy

The microstructural development of oxide scales on low carbon steels

A doctoral thesis submitted in partial fulfilment of the requirements for the award of Doctor of Philosophy.EThOS - Electronic Theses Online ServiceGBUnited Kingdo

On the Correlation between Magnetic Domain and Crystallographic Grain Orientation in Grain Oriented Electrical Steels

The deviation angle of the easy magnetisation -axes from the rolling direction (RD) strongly affects the magnetic domain configuration within individual grains and hence the overall magnetic properties in grain oriented electrical steels (GOES). In the current study, both angles of deviations; α: the angle between and in-plane rolling direction, and β: the angle between and out-plane rolling direction, where calculated using electron backscatter diffraction (EBSD) raw data to investigate the exact correlation between the crystal orientation and magnetic domain structure. Further, EBSD combined with forescatter detector (FSD) is used to reveal the magnetic domain configuration within individual oriented grains. The microstructure and microtexture of various GOESs with different chemical compositions and magnetic properties were characterised. The magnetic domain patterns were directly imaged and correlated to the crystal orientation and α and β deviation angles. It is demonstrated that the crystal orientation has a great impact on the magnetic domain patterns, width, and configurations. It was also shown that the grain boundary characteristics have a significant influence on the magnetic domain transfer between neighbouring grains. It was evident that low angle grain boundaries allowed domain transfer without a significant change in the domain pattern, whereas high angle grain boundaries perturbed the magnetic domain pattern, width, and configuration. Furthermore, it was demonstrated that the size of the deviated orientation grains from ideal (110) GOSS orientation is a critical microtexture parameter for the optimisation of magnetic property. Finally, it is concluded that the magnetic domain patterns and α and β angle of deviations are strongly correlated to the magnetic losses in GOES

Mechanistic approach of Goss abnormal grain growth in electrical steel: Theory and argument

The first Si-Fe electrical steel was produced in 1905, and the grain-oriented steel was discovered in 1930 after Goss demonstrated how optimal combinations of heat treatment and cold rolling could produce a texture giving Si-Fe strip good magnetic properties when magnetised along its rolling direction. This technology has reduced the power loss in transformers greatly and remains the basis of the manufacturing process today. Since then many postulations reported on the mechanism on abnormal grain growth (AGG) which is the key for Si-Fe superior magnetic properties, however, none have provided a concrete understanding of this phenomenon. Here, we established and demonstrated a new theory that underlines the fundamental mechanistic approach of abnormal grain growth in 3% Si-Fe steel. It is demonstrated, that the external heat flux direction applied during annealing and Si atom positions in the solid solution disordered α-Fe cube unit cell that cause lattice distortions and BCC symmetry reduction are the most influential factors in the early stage of Goss AGG than what was previously thought to be dislocation related stored energy, grain boundary characteristics and grain size/orientation advantages

The effects of grain size, dendritic structure and crystallographic orientation on fatigue crack propagation in IN713C nickel-based superalloy

The polycrystalline IN713C produced via investment casting is one of the widely-used nickel-based superalloy in automotive and aerospace industries. This alloy, however, has an apparent inhomogeneous microstructure generated during casting and contains dendritic structure that gives rise to strain localisation during loading. Yet, the effect of dendritic structure, grain size and shape as well as crystallographic orientation, which directly influence fatigue property and deformation micromechanism in the components, is rarely studied. In the present study, IN713C cast bars are tailored with three different grain structures, i.e., transition, equiaxed and columnar, with substantial grain size variations. The produced bars were tested under strain controlled LCF (Low Cycle Fatigue) and stress controlled HCF (High Cycle Fatigue) conditions at 650 °C. The results showed that most of fatigue cracks initiated from casting pores and fatigue life extended in the microstructure with a small grain size during both HCF and LCF loadings. It is also demonstrated that fatigue striations were mainly observed within dendritic areas during crack propagation, whereas the higher GND (Geometrically Necessary Dislocation) density were predominantly observed in the interdendritic areas. Here, we propose a concept of ‘Crack Propagation Unit (CPU)’ for better description of deformation mechanism at local scale during fatigue loading by combining fracture surface characteristic methodology and dislocation distribution analyses within the dendritic structural unit. Furthermore, this model to understand the deformation micromechanism can provide a new perspective on the interpretation of Hall-Petch relationship in casting materials that contain dendritic structure. This is further demonstrated via direct correlation of the high crack propagation resistance with the crack path divergence instead of the dislocation pile-up at the grain boundary or in-between the γ/γ′ channels. Moreover, by utilising serial sectioning method followed by layered EBSD scanning, quasi-3-D grain orientation mappings were obtained, and crystallographic texture information were directly correlated with the fracture surface observations. This allowed an investigation of the influence of orientation of individual grains and micro/macro texture on crack propagation rate. The critical stage of crack propagation in fatigue life and its correlations with microstructural features is established, offering potential practical applications by controlling the investment casting process parameters

A study of low cycle fatigue life and its correlation with microstructural parameters in IN713C nickel based superalloy

Up to date, IN713C Nickel-based superalloy has been continued to be the best alloy candidate for turbocharger wheel applications due to its adequate fatigue property and resistance to degradation under harsh operating environments. Throughout this study, three different batches of as-cast IN713C nickel based superalloys with different microstructures including columnar, equiaxed and transition microstructures were investigated. Strain control Low Cycle fatigue (LCF) tests were conducted for the three different microstructures, achieving fatigue life between 100 and runout at 100,000 cycles, depending on the testing parameters. The fracture mechanics and failure mechanism were correlated to the alloy's microstructure, texture and chemical composition under various LCF conditions using optical microscopy, SEM, EDX and EBSD. In the current study an exact correlation between alloy's microstructure/microtexture and LCF endurance is established. The results showed that equiaxed microstructure has a superior fatigue life than the transition microstructure by 10% and columnar microstructure by > 200% at a given temperature and strain rate. This large discrepancy was mainly due to the grain size differences between the studied microstructures. Here, it was evidenced that the grain size controls the dendrites length. It is also demonstrated that all microstructures exhibited a longer fatigue life at room temperature than at 650 °C, doubling or tripling the fatigue life of the tested IN713C. Furthermore, the high presence of precipitates between dendritic arms in all three microstructures was found to have great influence on crack propagation path. It was apparent that segregated carbides in between dendritic arms caused secondary crack initiation and crack path undulations during the LCF tests

The dislocation behaviour and GND development in a nickel based superalloy during creep

In the current study, dislocation activity and storage during creep deformation in a nickel based superalloy (Waspaloy) were investigated, focussing on the storage of geometrically necessary (GND) and statistically stored (SSD) dislocations. Two methods of GND density calculation were used, namely, EBSD Hough Transformation and HR-EBSD Cross Correlation based methods. The storage of dislocations, including SSDs, was investigated by means of TEM imaging. Here, the concept of GND accumulation in soft and hard grains and the effect of neighbouring grain orientation on total dislocation density was examined. Furthermore, the influence of applied stress (below and above the yield stress of Waspaloy) during creep on deformation micro-mechanism and dislocation density was studied. It was demonstrated that soft grains provided pure shear conditions on at least two octahedral (111) slip systems for easy dislocation movement. This allowed dislocations to reach the grain boundary without significant geometrically necessary dislocation accumulation in the centre of the grain. Hence, the majority of the soft grains appeared to have minimum GND density in the centre of the grain with high GND accumulation in the vicinity of the grain boundaries. However, the values and width of accumulated GND depended on the surrounding grain orientations. Furthermore, it was shown that the hard grains were not favourably oriented for octahedral slip system activation leading to a grain rotation in order to activate any of the available slip systems. Eventually, (i) the hard grain resistance to deformation and (ii) neighbouring grain resistance for the hard grain reorientation caused high GND density on a number of octahedral (111) slip systems. The results also showed that during creep below the yield stress of Waspaloy (500 MPa/700 °C), the GND accumulation was relatively low due to the insufficient macroscopic stress level. However, the regions near grain boundaries showed high GND density. At 800 MPa/700 °C (above yield at this temperature), in addition to the movement of pre-existing dislocations (SSD and GND) at a higher mobility rate, large numbers of dislocations were generated and moved toward the grain boundaries. This resulted in a much higher GND density but narrower width of high intensity GNDs near the grain boundaries. It is concluded that although GND measurement by means of EBSD can provide great insight into dislocation accumulation and its behaviour, it is critical to consider SSD type which also contributes to the strain hardening of the material