Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

The dramatic decline of the native red squirrel in the UK has been attributed to both direct and disease-mediated competition with the grey squirrel where the competitor acts as a reservoir host of squirrelpox virus (SQPV). SQPV is threatening red squirrel conservation efforts, yet little is known about its epidemiology. We analysed seroprevalence of antibody against SQPV in grey squirrels from northern England and the Scottish Borders in relation to season, weather, sex, and body weight using Generalized Linear Models in conjunction with Structural Equation Modelling. Results indicated a heterogeneous prevalence pattern which is male-biased, increases with weight and varies seasonally. Seroprevalence rose during the autumn and peaked in spring. Weather parameters had an indirect effect on SQPV antibody status. Our findings point towards a direct disease transmission route, which includes environmental contamination. Red squirrel conservation management options should therefore seek to minimize squirrel contact points.

Red squirrels are declining in the United Kingdom. Competition from, and squirrel poxvirus (SQPV) disease carried by, grey squirrels are assumed to be determining the decline. We analyse the incidence of disease and changes in distribution of the two species in Cumbria, from 1993 to 2003 and compare these to the predictions of an individual-based (IB) spatially explicit disease model simulating the dynamics of both squirrel species and SQPV in the landscape. Grey squirrels increased whilst red squirrels declined over 10 years. The incidence of disease in red squirrels was related to the time since grey squirrels arrived in the landscape. Analysis of rates of decline in red squirrel populations in other areas showed that declines are 17–25 times higher in regions where SQPV is present in grey squirrel populations than in those where it is not. The IB model predicted spatial overlap of 3–4 years between the species that was also observed in the field. The model predictions matched the observed data best when contact rates and rates of infection between the two species were low. The model predicted that a grey squirrel population control of >60% effective kill was needed to stop the decline in red squirrel populations in Cumbria.

Grain boundary structure and composition is assessed in austenitic stainless steels along with its influence on intergranular stress corrosion cracking (IGSCC) in high-temperature water. Brief examples are presented illustrating effects of grain boundary character and segregation on behavior in specific light-water-reactor environments. Although grain boundary engineering can produce an increased fraction of “special” boundaries in austenitic stainless alloys, practical benefits depend on the boundary orientation distribution. It is critical to recognize that only ∑3s appear to be more resistant to SCC and the behavior of other low ∑ boundaries is uncertain. Grain boundary composition can have a dominant effect on IGSCC under certain conditions, but altered interfacial chemistry is not required for cracking. In high-potential oxidizing environments, IGSCC susceptibility is a direct function of the boundary Cr concentration. Non- equilibrium thermal segregation of Cr and Mo is often present in mill-annealed stainless steels and may influence cracking susceptibility. This initial grain boundary composition alters subsequent radiation-induced segregation and delays irradiation-assisted SCC susceptibility to higher doses. Other alloying elements and impurities in 300-series stainless steels have been seen to enrich grain boundaries, but few have any significant impact on IGSCC susceptibility. One exception is Si that strongly segregates during irradiation. Recent results suggest that Si may accelerate crack propagation in both low- and high-potential water environments. Critical research is still needed to isolate individual grain boundary characteristics and quantitatively link them to IGSCC.

The objective of this work is to investigate the addition of misfit elements in both size and mass on the evolution of irradiated microstructure in 316 SS. Alloys were modified by the addition of Pt and Hf to suppress the radiation damage. Pt and Hf were added as a lattice perturbation to catalyze defect recombination within the early stage of cascade formation and defect migration. Irradiations were conducted with 5 MeV Ni-ions at 500 °C to doses up to 50 dpa or with 3.2 MeV protons at 400 °C. Microstructures were characterized using transmission electron microscopy. While no beneficial effect was seen for Pt addition, Hf appears to effectively alter the microstructural response to irradiation.

Analysis of the effect of annealing on change in void and loop size distributions provided insights that complement microstructural characterization using transmission electron microscopy (TEM). The predictions of concurrent vacancy-type and interstitial-type damage annealing are applied to measurements in neutron-irradiated austenitic stainless steels. Irradiation at 330°C produces void and loop microstructures for which the measured annealing response is in accord with predictions. Irradiation at 275° produces only Frank loop microstructure for which the annealing response cannot be predicted from measured microstructures. The model predictions are based on an assumed vacancy source not detected using TEM. The measured loop microstructure is typically reported to be interstitial in character but this analysis suggests that a significant component of the loop population is vacancy-type damage based on defect inventory and kinetic arguments.

Our understanding of radiation effects in stainless steels irradiated at temperatures below annealing stage V (<573K) remains unclear. The microstructure under these conditions has been loosely described in terms of Frank loops and “black spot” damage, the latter of which is typically considered to be 4-5 nm or less in size. To further clarify the nature of these defects, 6 stainless steels heats neutron irradiated at 550K from 0.6 to 13.3 dpa have been characterized by TEM. The microstructure is comprised of a very high density of small Frank loops present in sizes as small as 1 nm and perhaps lower, which could be of both vacancy and interstitial-type. The density of the visible loops is already established at the lowest dose available, however, the microstructure continues to evolve as the dose increases. The size distributions of the Frank loops change from a narrow symmetric distribution to a much broader size distribution with a bimodal distribution beginning to form at the higher doses.

Grain boundary compositions and near-boundary microstructures have been measured in complex Fe-Cr-Ni alloys after neutron irradiation at intermediate temperatures where nanometer-scale damage promotes structural integrity problems in nuclear reactor systems. Radiation-induced segregation (RIS) and dislocation loop microstructures have been determined as a function of irradiation dose up to 13 dpa and at temperatures near 280°C. The most significant effect on RIS was the grain boundary structure (low-energy special boundaries versus high-energy random boundaries) and composition (enrichment of Cr and Mo) before irradiation. Grain boundary character distribution did not change with irradiation and only high-energy boundaries exhibited significant radiation-induced changes. The initial grain boundary composition in mill-annealed stainless steels was difficult to remove during subsequent irradiation and retarded the development of Cr- and Mo-depleted regions.

Identical Al-Mg-Mn-Sc alloys without and with 0.034-wt% Sn additions were fabricated, heat-treated, and tensile tested in a fine-grain (d < 6 pm) condition at four strain rates from 10−2 to 10−4 s−1 and at temperatures from 723K to 823K. Alloys with Sn additions exhibited reduced failure strains at 723K but higher failure strains at 823K for the slowest strain rates. The effect of Sn on flow stress, activation energy for flow stress, and strain rate exponent was explored and was found to be small. The main effect of Sn was suggested to be in reducing cavitation by allowing a redistribution of stress at critical hetero-junctions in the alloys.

Interactions between point defects and major solute strongly influence grain boundary concentrations during heat treatment, irradiation and annealing of austenitic stainless steels. Previous approaches to nonequilibrium segregation emphasize only elastic defect-solute interactions. The present evaluation of nonequilibrium concentrations at grain boundaries indicates chemical interactions unique to solution annealing and cooling during thermal nonequilibrium segregation (TNES). Subsequent to TNES, radiation-induced segregation and post-irradiation annealing are modeled and compared with measured changes in grain boundary composition. The latter two mechanisms are controlled by exchanges between vacancies and major solute such as Cr.

Microstructural evolution and deformation behavior of austenitic stainless steels are evaluated for neutron, heavy-ion and proton irradiated materials. Radiation hardening in austenitic stainless steels is shown to result from the evolution of small interstitial dislocation loops during lightwater-reactor (LWR) irradiation. Available data on stainless steels irradiated under LWR conditions have been analyzed and microstructural characteristics assessed for the critical fluence range (0.5 to 10 dpa) where irradiation-assisted stress corrosion cracking susceptibility is observed. Heavy-ion and proton irradiations are used to produce similar defect microstructures enabling the investigation of hardening and deformation mechanisms. Scanning electron, atomic force and transmission electron microscopies are employed to examine tensile test strain rate and temperature effects on deformation characteristics. Dislocation loop microstructures are found to promote inhomogeneous planar deformation within the matrix and regularly spaced steps at the surface during plastic deformation. Twinning is the dominant deformation mechanism at rapid strain rates and at low temperatures, while dislocation channeling is favored at slower strain rates and at higher temperatures. Both mechanisms produce highly localized deformation and large surface slip steps. Channeling, in particular, is capable of creating extensive dislocation pileups and high stresses at internal grain boundaries which may promote intergranular cracking.

The dissociation of extrinsic grain boundary dislocations in Al, Al-Mg and Al-Mg-Sn alloys was studied at various temperatures to examine the compositional effect on the dissociation process. It was found that both alloying elements (Mg and Sn) hinder the dissociation, however the effect of Sn is more significant even at a very low concentration due in part to grain boundary segregation.

Measurement of minor element compositions at irradiated grain boundaries in austenitic stainless steels indicates that Si is the only element that significantly responds to radiation-induced segregation. Other minor elements, such as P or S, do not exhibit elevated grain boundary concentrations after irradiation. A rate theory evaluation of segregation is in accord with ioninduced Si enrichment, but reveals complexities in the interpretation of extrapolating behavior from ion-irradiation to neutron-irradiation behavior. The model calibrated to measured high-rate, ioninduced segregation greatly overestimates measured low-rate, neutron-irradiation segregation of Si.

Recrystallization and grain growth studies of Al-Mg-Mn-Zr alloys have been carried out in-situ in the transmission electron microscope. Nucleation sites were primarily on large (>I μm diameter) eutectic constituent particles. The sub-micron A16Mn dispersoids were observed to be effective as nuclei if present in clusters, and were effective at retarding grain boundary migration and dislocation motion. The smaller A13Zr precipitates seemed to have little effect on nucleation and growth, but were effective in pinning dislocations. These results have been analyzed in terms of precipitate size and shape in both the as-cold-worked microstructure and during recrystallization. The implications on the microstructural refinement of these alloys for improved superplastic properties will be discussed.

Radiation-induced segregation (RIS) to grain boundaries in Fe-Ni-Cr-Si stainless alloys has been measured as a function of irradiation temperature and dose. Heavyion irradiation was used to produce damage levels from 1 to 20 displacements per atom (dpa) at temperatures from 175 to 550°C. Measured Fe, Ni, and Cr segregation increased sharply with irradiation dose (from 0 to 5 dpa) and temperature (from 175 to about 350°C). However, grain boundary concentrations did not change significantly as dose or temperatures were further increased. Although interfacial compositions were similar, the width of radiation-induced enrichment or depletion profiles increased consistently with increasing dose or temperature. Impurity segregation (Si and P) was also measured, but only Si enrichment appeared to be radiation-induced. Grain boundary Si peaked at levels approaching 8 at% after irradiation doses to 10 dpa at an intermediate temperature of 325°C. No evidence of grain boundary silicide precipitation was detected after irradiation at any temperature. Equilibrium segregation of P was measured in the high-P alloys, but interfacial concentration did not increase with irradiation exposure. Comparisons to reported RIS in neutronirradiated stainless steels revealed similar grain boundary compositional changes for both major alloying and impurity elements.

Analysis of the deformation microstructures in ion-irradiated stainless steel shows twinning to be the predominant deformation mode at room temperature. Dislocation channelling also occurs under slow strain rate conditions. Stresses required for twinning were calculated by the model of Venables and are compatible with observed yield stresses in neutron-irradiated material if loops are the principal twin source. Computation of the expected radiation hardening from the defect structure, based on a simple model, is consistent with yield strengths measured on neutron-irradiated steels. Lower yield stresses and greater thermal energy at 288°C lessen the probability of twinning and dislocation channeling becomes the primary deformation mode at the higher temperature. However, preliminary results show that some twinning does occur in the irradiated stainless steel even at the higher temperature when higher strain rates are used.

Defect kinetic parameters for radiation-induced grain boundary segregation in austenitic stainless alloys are evaluated by comparing model predictions to measured responses. Heavy-ions, neutrons, and proton irradiations having substantial statistical bases are examined. The combined modeling and measurement approach is useful for quantifying fundamental defect parameters. The mechanism evaluation indicates that vacancy migration energies were 1.15 eV or less and the vacancy formation energy at grain boundaries was 1.5 eV. Damage efficiencies of heavy ions and light-water reactor neutrons were about 0.03. Inferred proton damage efficiencies were about 0.15. Segregation measured in an advanced gas-cooled reactor component was much greater than predicted from those parameters alone.

Defect-solute interactions control radiation-induced segregation (RIS) to interfacial sinks, such as grain boundaries, in metallic materials. The best studied system in this regard has been austenitic stainless steels. Measurements of grain boundary composition indicate that RIS of major alloying elements is in reasonable agreement with inverse-Kirkendall predictions. The steep and narrow composition profiles are shown to result from limited back diffusion near the boundary. Subsequently, defect-solute interactions that affect the near-boundary defect concentrations strongly affect RIS. The variability in measured RIS may in part be caused by grain boundary characteristics.

Recent research on the low- and high-temperature properties of two beryllium-niobium intermetallic compounds, Be12Nb and Be17Nb2, is reviewed and discussed. Strength (bend and compression), hardness and fracture toughness has been mapped as a function of test temperature up to 1200°C. Results for hot-isostatically-pressed Be12Nb and Be17Nb2 are highlighted illustrating the potential for reasonable strength at both low and high temperatures. Chemical compatibility between Be12Nb and several high-temperature materials such as SiC, Al2O3, MoSi 2and various refractory metals is evaluated. Limitations for the structural use of the beryllides are identified and discussed including low-temperature toughness, intermediate-temperature embrittlement, high-temperature creep strength and composite compatibility.