T.J. Marrow

Three-dimensional grain mapping by x-ray diffraction contrast tomography and the use of Friedel pairs in diffraction data analysis

X-ray diffraction contrast tomography (DCT) is a technique for mapping grain shape and orientation in plastically undeformed polycrystals. In this paper, we describe a modified DCT data acquisition strategy which permits the incorporation of an innovative Friedel pair method for analyzing diffraction data. Diffraction spots are acquired during a 360 degrees rotation of the sample and are analyzed in terms of the Friedel pairs ((hkl) and (hkl) reflections, observed 180 degrees apart in rotation). The resulting increase in the accuracy with which the diffraction vectors are determined allows the use of improved algorithms for grain indexing (assigning diffraction spots to the grains from which they arise) and reconstruction. The accuracy of the resulting grain maps is quantified with reference to synchrotron microtomography data for a specimen made from a beta titanium system in which a second phase can be precipitated at grain boundaries, thereby revealing the grain shapes. The simple changes introduced to the DCT methodology are equally applicable to other variants of grain mapping.

X-ray microtomographic observation of intergranular stress corrosion cracking in sensitised austenitic stainless steel

Abstract Intergranular stress corrosion cracking in a sensitised type 302 stainless steel wire has been observed in situ using high resolution X-ray microtomography. Tomography enables the development and failure of crack bridging ligaments to be studied in detail in three dimensions. Direct comparison of these features has been made with scanning electron microscopy fractography. The crack bridges failed in a ductile manner, with a morphology that is consistent with non-sensitised low energy grain boundaries.

X-ray microtomography studies of localised corrosion and transitions to stress corrosion cracking

Abstract Two forms of high resolution X-ray tomographic experiments (i.e. synchrotron based X-ray microtomography and desktop microfocus computed X-ray tomography) are demonstrated in the present paper to illustrate the wide application of these techniques for qualitative and quantitative studies of localised corrosion and environmentally assisted cracking. Specifically, synchrotron based X-ray tomography was used to investigate the localised corrosion morphology within aluminium specimens when exposed in situ to a chloride environment while microfocus computed X-ray tomography was used to investigate the morphology and quantify the transition from localised corrosion to stress corrosion cracking in steel specimens exposed ex situ to a simulated corrosive condensate environment.

In situ observation of intergranular crack nucleation in a grain boundary controlled austenitic stainless steel

Grain boundary engineering has been proposed to increase the lifetime performance of sensitized austenitic stainless steel in aggressive environments. Increased microstructure resistance is typically associated with higher fractions of twin (Σ3) grain boundaries, but there is uncertainty about the properties and role of other boundaries. To develop predictive models for stress corrosion crack nucleation, more information is required about how grain boundary crystallography and the orientations of the grain boundary plane and its surrounding grains affect crack development. Digital image correlation combined with electron backscatter diffraction has been used to characterize the microstructure and to observe, in situ, the nucleation and propagation of short stress corrosion cracks in thermo‐mechanically processed type 304 stainless steel. The crack path and its growth rate have been determined and are found to be influenced by the microstructure.

X-ray tomography observation of crack propagation in nuclear graphite

Abstract X-ray microtomography has been used to investigate the mechanisms responsible for rising crack growth resistance with crack propagation (R curve behaviour) in polygranular nuclear graphite. Tomography can be used to observe changes in the crack shape with propagation, and a side grooved specimen has been developed to produce the planar straight fronted crack necessary for fracture toughness measurement. Crack bridging from frictional contact between the fracture surfaces is observed. A zone of reduced X-ray attenuation, attributed to microstructural damage, is also observed around the crack tip and in its wake. These are the first in situ observations of the mechanisms of the R curve behaviour in nuclear graphites.

Fracture behaviour of radiolytically oxidised reactor core graphites: a view

Abstract This paper provides a view on the fracture behaviour of polygranular graphites, used to moderate gas cooled nuclear reactors. Graphite is often cited as a classic example of a brittle material because failure, in tension, is associated with small strains. However, attempts to characterise the fracture behaviour of graphite by linear elastic fracture mechanics methods have been largely unsuccessful. Observations of graphite fracture show that elastic strain energy may be dissipated by the formation of distributed microcracks, and their formation may be responsible for non-linearity in the rising load–displacement curve. Progressive softening behaviour may also be observed in some specimens after the peak load. This type of load–displacement behaviour is a characteristic of quasi-brittle materials. Radiolytic oxidation increases the proportion of porosity within reactor core graphite so that the microstructure becomes increasingly skeletal. Consideration is given to the fracture of radiolytically oxidised graphite to support an argument for quasi-brittle behaviour.

Effect of mean stress on hydrogen assisted fatique crack propagation in duplex stainless steel

Hydrogen assisted subcritical cleavage of the ferrite matrix occurs during fatigue of a duplex stainless steel in gaseous hydrogen. The ferrite fails by a cyclic cleavage mechanism and fatigue crack growth rates are independent of frequency between 0.1 and 5 Hz. Macroscopic crack growth rates are controlled by the fraction of ferrite grains cleaving along the crack front, which can be related to the maximum stress intensity, Kmax. A superposition model is developed to predict simultaneously the effects of stress intensity range (ΔK) and K ratio (Kmin/Kmax). The effect of Kmax is rationalised by a local cleavage criterion which requires a critical tensile stress, normal to the {001} cleavage plane, acting over a critical distance within an embrittled zone at the crack tip.

Hydrogen-assisted stable crack growth in iron-3 wt% silicon steel

Observations of internal hydrogen cleavage in Fe3Si are reported. Hydrogen-assisted stable crack growth (H-SCG) is associated with cleavage striations of a 300 nm spacing, observed using scanning electron microscopy (SEM) and atomic force microscopy (AFM). High resolution SEM revealed finer striations, previously undetected, with a spacing of approximately 30 nm. These were parallel to the coarser striations. Scanning tunnelling microscopy (STM) also showed the fine striation spacing, and gave a striation height of approximately 15 nm. The crack front was not parallel to the striations. Transmission electron microscopy (TEM) of crack tip plastic zones showed {112} and {110} slip, with a high dislocation density (around 1014 m−2). The slip plane spacing was approximately 15–30 nm. Parallel arrays of high dislocation density were observed in the wake of the hydrogen cleavage crack. It is concluded that H-SCG in Fe3Si occurs by periodic brittle cleavage on the {001} planes. This is preceded by dislocation emission. The coarse striations are produced by crack tip blunting and the fine striations by dislocations attracted by image forces to the fracture surface after cleavage. The effects of temperature, pressure and yield strength on the kinetics of H-SCG can be predicted using a model for diffusion of hydrogen through the plastic zone.

The influence of low-strain thermo-mechanical processing on grain boundary network characteristics in type 304 austenitic stainless steel

Grain boundary engineering of austenitic stainless steel, through the introduction of plastic strain and thermal annealing, can be used to develop microstructures with improved resistance to inter‐granular degradation. The influence of low‐strain thermo‐mechanical processing on grain boundary network development, with systematic variations of annealing treatments, has been investigated. Three stages of the microstructure development during grain boundary engineering in low‐strain processing conditions are identified, and correlated with changes in grain boundary character and deviation distributions. Low‐energy connected length segments at triple junctions, which have been proposed to be responsible for crack bridging during inter‐granular stress corrosion cracking, can be influenced by the choice of the annealing treatment parameters. The development of individual grain boundary length segments of different character showed consistent trends with increasing grain size. Crack length predictions are consistent with the beneficial effect of designing microstructures with high fractions of twin grain boundaries and smaller grain size.

Temperature effects on the mechanism of time independent hydrogen assisted fatigue crack propagation in steels

The effects of temperature on hydrogen assisted fatigue crack propagation are investigated in three steels in the low-to-medium strength range; a low alloy structural steel, a super duplex stainless steel, and a super ferritic stainless steel. Significant enhancement of crack growth rates is observed in hydrogen gas at atmospheric pressure in all three materials. Failure occurs via a mechanism of time independent, transgranular, cyclic cleavage over a frequency range of 0.1-5 Hz. Increasing the temperature in hydrogen up to 80°C markedly reduces the degree of embrittlement in the structural and super ferritic steels. No such effect is observed in the duplex stainless steel until the temperature exceeds 120°C. The temperature response may be understood by considering the interaction between absorbed hydrogen and micro-structural traps, which are generated in the zone of intense plastic deformation ahead of the fatigue crack tip.