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In the current study, dislocation activity and storage during creep deformation in a nickel based superalloy (Waspaloy) was investigated, focussing on the storage of geometrically necessary (GND) and statistically stored (SSD) dislocations. Two methods of GND density calculations 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 Waspaloy yield stress) during creep on deformation micro-mechanism and dislocation density was studied. It was demonstrated that soft grains provided pure shear conditions at least on two octahedral (111) slips for easy dislocation movement reaching the grain boundary without significant geometrically necessary 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 insufficient microscopic stress level. However, the regions near grain boundaries showed high GND density.Whereas, in addition to the movement of pre-existing dislocations (SSD and GND) at higher mobility rate under 800 MPa/700C above yield creep condition, large numbers of dislocations were generated and moved toward the grain boundaries. This resulted in much higher GND density but narrower width of high intensity GND near the grain boundaries. It is concluded that although GND measurement by means of EBSD can provide a great insight of dislocation accumulation and its behaviour, it is critical however to consider SSD type which is also contributes to the strain hardening of the materials.

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Highlights • Two alloy surface treatments are compared. • The kinetics of a Ni-based superalloy are compared to pure chromia formation. • The enhancement is described in terms of Ti-doping of the surface chromia scale. • For the first time, a (Ta,Ti)O 2 phase, formed at the oxide metal interface, is identified.

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Segregation of phosphorus to grain boundaries in commercial grade 2?25Cr1Mo and A533B steels subjected to a variety of heat treatments has been examined using field emission gun scanning transmission electron microscope (FEGSTEM) with energy dispersive X-ray microanalysis. The measured grain boundary P concentrations have been used to explain the low temperature brittle fracture behaviour, which exhibits increasing levels of intergranular embrittlement as a function of aging time at 520uC. The results show that P segregation at grain boundaries has a strong effect on the intergranular area fraction, the microscopic fracture stress, and the fracture toughness. Phosphorus peak height ratios measured using auger electron spectroscopy are shown to follow a linear relationship with the FEGSTEM/X-ray values.

It is well known that titanium and its alloys are sensitive to electrolytes and thus hydrides are commonly observed in electropolished foils. In this study, focused ion beam (FIB) milling was used to prepare thin foils of titanium and its alloys for transmission electron microscopy. The results show the following: (i) titanium hydrides were observed in pure titanium, (ii) the preparation of a bulk sample in water or acid solution resulted in the formation of more hydrides and (iii) FIB milling aids the precipitation of hydrides, but there were never any hydrides in Ti64 and Ti5553.