The design of radiation-tolerant polycrystalline materials has been mainly based on the control and manipulation of grain boundaries (GBs) that leads to annihilation of point defects at grain-boundary neighborhoods thus resulting in the formation of defect denuded zones. Nanocrystalline materials are potential candidates providing large density defect sinks for individual point defects and small highly mobile defect clusters (DCs). Using the in-situ irradiation transmission electron microscopy (TEM) technique, this study not only experimentally revealed the coalescence of small glissile DCs at/near GB and their subsequent annihilation at grain-boundary, but also provide insight into defect cluster dynamics. The small DCs were found to be transported to grain-boundary neighborhoods where they can annihilate by the onedimensional loop hop or Burgers-vector rotation mechanism to GBs, considered as the main contribution to the long-range flux of interstitials to GB sinks. This process had marked effects on the morphology of the irradiated microstructure in nanocrystalline iron, limiting the length of DC strings and reducing the coalescence of DCs into large clusters (dislocation loops).(c) 2022 Published by Elsevier B.V.

While transformations of dislocation-loop character at high temperatures during heavy ion irradiation has been studied for more than two decades, the role of grain size, or high sink density, has not been considered. To interrogate the effect of defect mobility on irradiated nanocrystalline (nc) microstructures at elevated temperatures, detailed in-situ ion irradiation transmission electron microscopy (TEM) studies were carried out. The transformation temperature for the Burgers vector b = 1/2 <111>-to-<100> transition was found to be 450 °C, representing a lower threshold than that found in micron-grain-sized counterparts. The formation of stable b = 1/2<111> dislocation loops is observed below 400 °C, while at 450∼500 °C, 1/2<111> loops either transformed into 〈100〉 loops or were absorbed at grain boundaries (GBs). Thus, the substantial absorption of point defects and dislocation loops by GBs over a range of temperatures characteristically changes the defect morphology from large finger-shaped observed in micron-sized grains to small circular shape loops in nc grains.

The opportunity to achieve radiation tolerance in crystalline materials hinges on understanding the structure and response of grain boundary sinks to irradiation. A common descriptor of grain boundary efficiency as a defect sink is the denuded zone, which is a defect free zone adjacent to the grain boundary dictated by its ability to absorb radiation induced defects. This descriptor is often used at the mesoscale, which requires an averaging of absorption events. In this paper, we resolve the defect sink efficiency as a function of interfacial strain with respect to grain boundary character, and correlate high levels of grain boundary strain to an enhanced absorption efficiency. We also introduce a key relationship between localized strain in proximity with the grain boundary sink and the variation absorption efficiency associated with these regions, revealing the pitfalls of averaging absorption events along a grain boundary, and presenting a path forward toward improved models for denuded zones and localized grain boundary absorption phenomena.

Grain boundaries (GBs) are considered sinks where mobile defects are attracted and annihilated thereby hampering irradiation damage accumulation. Nanocrystalline (NC) metals characteristically have greater densities of GBs relative to their coarse-grained counterparts hence they are postulated to provide enhanced resistance to irradiation damage.The use of alloying as a means to impart synergistic properties such as corrosion resistance, increased toughness, or improved conductivity is well studied, yet the cooperative effects of solute addition and grain size in the nano-regime is not well understood. In this study, a combination of in situ ion irradiation, transmission electron microscopy (TEM), and automated crystal orientation mapping (ACOM) on model Ni, NiCr, Fe, and FeCr NC thin-films are used to provide experimental evidence that grain size and irradiation induced defect morphology (defect density and size) are not directly correlated due to defect agglomeration, annihilation at sinks, and saturation, while the addition of solute impedes defect mobility, altering the final damage state.

To evaluate the potential of high entropy alloys (HEAs) for nuclear applications, two HEAs, Al0.3CoCrFeNi and CoCrFeMnNi, and a conventional Type 316H stainless steel (SS) were irradiated with 1 MeV krypton ions at 500 degrees C up to 1 dpa, and examined in-situ with a transmission electron microscope (TEM). After irradiation, a high density of ordered L1(2) nanoparticles was observed in Al0.3CoCrFeNi. In contrast, no phase transformation was observed in CoCrFeMnNi and 316H SS. In the thin foil regions of TEM samples, stacking-fault tetrahedra were observed in the HEAs. In the thick foil regions, interstitial dislocation loops were observed for all alloys, and the areal loop density increased linearly with foil thickness. The Al0.3CoCrFeNi had the largest loop size (the lowest density), followed by the CoCrFeMnNi and then the 316H SS. The higher loop nucleation rate in the 316H SS was attributed to carbon content. The degree of irradiation hardening was slightly lower for the HEAs than for the 316H SS, which is a promising sign for the nuclear application of HEAs at high temperatures. Published by Elsevier B.V.

The Ni–Fe–Cr based superalloy with percentage additions of Nb, Al and Ti, called "Inconel X750 superalloy", is studied with its importance in nuclear application. Under reactor neutron irradiation, the strengthening phase Ni3(Al, Ti) in the form of gamma prime precipitates were somehow disordered, and dissolved eventually, by which the mechanical properties of materials were degraded. It is of high interests to investigate the effects of transmutation production helium on radiation-induced instability of gamma prime in the materials. The transmission electron microscope in situ heavy ion irradiations with and without pre-injected helium are performed purposely. The precipitates were disordered by heavy ion irradiation after 0.06 displacement per atom (dpa). The presence of 2×10−4 atoms helium delayed the disordering of Ni3(Al, Ti) precipitates to 0.68 dpa. With 4×10−4 atoms helium, the precipitates required doses of > 2.7 dpa to become disordered. In addition, the precipitation of M23C6 particles were observed at 600 °C irradiation to 5.4 dpa with 4×10−4 atoms helium pre-injected.

We report for the first time the observation of irradiation-induced amorphization of the zirconium suboxide formed during aqueous corrosion of Zr-0.5Nb alloys. High-resolution transmission electron microscopy results reveal amorphization of the hexagonal-ZrO suboxide under heavy ion irradiation at cryogenic temperatures. This irradiation-induced amorphization behaviour is discussed in relation to the arrangement of oxygen interstitials and the formation of stable superlattices. The sensitivity of the suboxide to irradiation damage can lead to phase changes and the accumulation of defects near the oxide/metal interface, which needs to be taken into account in the development of mechanistic models addressing radiation-assisted acceleration of corrosion rates in zirconium alloys.

Nanocrystalline and nanolaminated materials show enhanced radiation tolerance compared with their coarse-grained counterparts, since grain boundaries and layer interfaces act as effective defect sinks. Although the effects of layer interface and layer thickness on radiation tolerance of crystalline nanolaminates have been systematically studied, radiation response of crystalline/amorphous nanolaminates is rarely investigated. In this study, we show that irradiation can lead to formation of nanocrystals and nanotwins in amorphous CuNb layers in Cu/amorphous-CuNb nanolaminates. Substantial element segregation is observed in amorphous CuNb layers after irradiation. In Cu layers, both stationary and migrating grain boundaries effectively interact with defects. Furthermore, there is a clear size effect on irradiation-induced crystallization and grain coarsening. In situ studies also show that crystalline/amorphous interfaces can effectively absorb defects without drastic microstructural change, and defect absorption by grain boundary and crystalline/amorphous interface is compared and discussed. Our results show that tailoring layer thickness can enhance radiation tolerance of crystalline/amorphous nanolaminates and can provide insights for constructing crystalline/amorphous nanolaminates under radiation environment.

A detailed study has been carried out on recrystallised Zr-1.0Nb alloys corroded and irradiated under different conditions, including ex-autoclave and ex-reactor samples. After 540 days in reactor and damage around 5 dpa, the neutron irradiated sample shows no serious evidence for radiation enhanced corrosion and is still in pre-transition stage. The good corrosion resistance of the neutron irradiated Zr-1.0Nb can be related to the higher volume fraction of tetragonal phase and fewer interconnected nano porosity/cracks in the oxide. This indicates less tetragonal to monoclinic transition, leads to more protective oxide in the neutron irradiated sample, containing little evidence for short circuit paths for the penetration of oxygen or water towards the metal-oxide interface. These observations on a sample with a slow overall oxidation rate are consistent with the hypothesis that interconnected porosity can lead to early transitions and rapid oxidation. Tetragonal oxide can be either stabilised by irradiation, or stabilised by local release of impurity species from SPPs such as dissolution of Fe from Zr-Nb-Fe precipitates or radiation introduced precipitates (RIPs) which is likely to be small β-Nb clusters. The oxide consists of well-aligned columnar-equiaxed microstructure in the autoclave sample while a more complex oxide grain structure was observed in the neutron-irradiated sample. As oxide continues to grow, there are more and loops, dissolved Fe and RIPs in the metal matrix, however, the corrosion rate is low enough for the tetragonal oxide to stabilise and suboxide + Zr(Osat) phases exist for protectiveness, so there is no enhanced corrosion after radiation. In situ ion irradiation in the TEM revealed no visible defect clusters or voids in the oxide, suggesting that radiation damage to the metal matrix rather than oxide may have a stronger effect on corrosion mechanisms after neutron irradiation, however, cascade damages are not visible in this case. Neutron irradiation also seems to have little effect on promoting fast oxidation or dissolution of β-Nb precipitates into the surrounding oxide or metal during irradiation. These results are discussed in the light of the current mechanisms for corrosion of nuclear fuel cladding alloys.

Transmission electron microscopy (TEM) is an established tool used for the investigation of defects in materials. Traditionally, diffraction contrast techniques—two-beam bright-field and weak-beam dark-field—have been used to image defects due to contrast sensitivity from weak lattice strains. Use of these methods entail an intricate tilt series of imaging using different diffracting vectors, g, to verify the g•b invisibility criterion relative to the different defect types and habit planes inherent to the material. Recently, the addition of down-zone imaging and STEM imaging has also proven to be effective imaging techniques for defect density analysis. Interest in nanocrystalline (NC) materials, spurred by their conjectured superior properties compared to their coarse-grain counterparts, has been thriving and the investigation of their defect morphologies is essential. Maneuvering within NC samples in the TEM adds another layer of difficulty making the aforementioned techniques not practical for application to specimens with complex microstructures. For this reason, we have devised a protocol for identifying NC grains optimally oriented for quantitative analysis using NanoMegas ASTAR automated crystal orientation mapping (ACOM) in the TEM. In this work, we conduct a series of experiments assessing the effectiveness of conventional two-beam bright-field, weak-beam dark-field, and down-zone STEM imaging. We also evaluate an ACOM-assisted multibeam imaging method and compare defect density results obtained using each technique in an irradiated nanocrystalline Au sample.

The evolution of irradiation defects in Ti2AlC under Kr ion irradiation at room and elevated temperatures has been investigated. The dependence of defect size and density on the irradiation dose and temperature was characterized by in-situ transmission electron microscopy (TEM) irradiation experiments. At 25-800 degrees C, interstitial-type dislocation loops with several nanometers in diameter form on the basal plane of Ti2AlC mostly with a Burgers vector of 1/2[0 0 0 1], and no voids have been observed. The number density of dislocation loops approaches saturation at a level of about 2 dpa at 800 degrees C. Ti2AlC samples remain crystalline in structure without amorphization or phase transformation. However, the localized disorder of atomic positions on the basal plane of the irradiated Ti2AlC was revealed by high-resolution transmission electron microscopy (HRTEM) studies, which increases with irradiation dose while decreases with elevated temperatures.

The mechanism of radiation-induced detwinning is different from that of deformation detwinning as the former is dominated by supersaturated radiation-induced defects while the latter is usually triggered by global stress. In situ Kr ion irradiation was performed to study the detwinning mechanism of nanotwinned Cu films with various twin thicknesses. Two types of incoherent twin boundaries (ITBs), so-called fixed ITBs and free ITBs, are characterized based on their structural features, and the difference in their migration behavior is investigated. It is observed that detwinning during radiation is attributed to the frequent migration of free ITBs, while the migration of fixed ITBs is absent. Statistics shows that the migration distance of free ITBs is thickness and dose dependent. Potential migration mechanisms are discussed.

The development of materials that can better withstand the operating environment within nuclear reactors is of critical importance for the longevity of existing and the robustness of future nuclear energy systems [1]. It is imperative to explore progressive structural materials and microstructural designs that can be used in new and advanced reactors planned to undergo more extreme environments and longer material lifetime [1]. Of particular interest are nanostructured materials, which contain an extremely high density of interfaces, i.e. grain boundaries [2]. Grain boundaries (GBs) can act as effective sinks for irradiation-induced defects. Individual GB response and the effect of GB density on irradiation-induced defect accumulation are dependent on a number of factors including the GB density and character [3]. Hence, it is important to have a comprehensive knowledge of how specific types of grain boundaries respond to irradiation to develop enhanced radiation resistant materials.

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Oxide‐dispersion‐strengthened (ODS) austenitic steels are promising materials for next‐generation fossil and nuclear energy systems. In this study, laser shock peening (LSP) has been applied to ODS 304 austenitic steels, during which a high density of dislocations, stacking faults, and deformation twins are generated in the near surface of the material due to the interaction of laser‐driven shock waves and the austenitic steel matrix. The dispersion particles impede the propagation of dislocations. The compressive residual stress generated by LSP increases with successive LSP scans and decreases along the depth, with a maximum value of −369 MPa. The hardness on the surface can be improved by 12% using LSP. In situ transmission electron microscopy (TEM) irradiation studies reveal that dislocations and incoherent twin boundaries induced by LSP serve as effective sinks to annihilate irradiation defects. These findings suggest that LSP can improve the mechanical properties and irradiation resistance of ODS austenitic steels in nuclear reactor environments.

Atomic mixing by replacement collision sequences and other cascade effects is well known to create chemical disorder in irradiated alloys. Most studies of irradiation-induced disordering have focused on ex situ analysis of irradiated samples; however, fast in situ techniques are necessary to measure disordering at elevated temperatures without significant interference from concurrent re-ordering processes. In the present work, we use in situ electron diffraction with high speed data collection to measure the initial change in the long-range order parameter S with ion dose ϕ during 500 keV Ne+ irradiation of Cu3Au foils. The data reveal an unexpected and dramatic increase in the disordering rate as the critical order–disorder transition temperature TC is approached. Molecular dynamics simulations show that this increase is not due to temperature-dependent cascade mixing. We attribute the enhanced disordering, instead, to coupling between point defect fluxes and the chemical state of order.

Here, in situ ion irradiation and rate theory calculations were employed to directly compare the radiation resistance of an oxide dispersion strengthened alloy with that of a conventional ferritic/martensitic alloy. Compared to the rapid buildup of dislocation loops, loop growth, and formation of network dislocations in the conventional ferritic/martensitic alloy, the superior radiation resistance of the oxide dispersion strengthened alloy is manifested by its stable dislocation structure under the same irradiation conditions. The results are consistent with rate theory calculations, which show that high-density nanoparticles can significantly reduce freely migrating defects and suppress the buildup of clustered defects.

Many methods used to produce nanocrystalline (NC) materials leave behind non-equilibrium grain boundaries (GBs) containing excess free volume and higher energy than their equilibrium counterparts with identical 5 degrees of freedom. Since non-equilibrium GBs have increased amounts of both strain and free volume, these boundaries may act as more efficient sinks for the excess interstitials and vacancies produced in a material under irradiation as compared to equilibrium GBs. The relative sink strengths of equilibrium and non-equilibrium GBs were explored by comparing the behavior of annealed (equilibrium) and as-deposited (non-equilibrium) NC iron films on irradiation. These results were coupled with atomistic simulations to better reveal the underlying processes occurring on timescales too short to capture using in situ TEM. After irradiation, NC iron with non-equilibrium GBs contains both a smaller number density of defect clusters and a smaller average defect cluster size. Simulations showed that excess free volume contribute to a decreased survival rate of point defects in cascades occurring adjacent to the GB and that these boundaries undergo less dramatic changes in structure upon irradiation. These results suggest that non-equilibrium GBs act as more efficient sinks for defects and could be utilized to create more radiation tolerant materials in future.

We have constructed a computer model of irradiation defect production closely coordinated with TEM and in situ ion irradiation of Molybdenum at 80 degrees C over a range of dose, dose rate and foil thickness. We have reexamined our previous ion irradiation data to assign appropriate error and uncertainty based on more recent work. The spatially dependent cascade cluster dynamics model is updated with recent Molecular Dynamics results for cascades in Mo. After a careful assignment of both ion and neutron irradiation dose values in dpa, TEM data are compared for both ion and neutron irradiated Mo from the same source material. Using the computer model of defect formation and evolution based on the in situ ion irradiation of thin foils, the defect microstructure, consisting of densities and sizes of dislocation loops, is predicted for neutron irradiation of bulk material at 80 degrees C and compared with experiment. Reasonable agreement between model prediction and experimental data demonstrates a promising direction in understanding and predicting neutron damage using a closely coordinated program of in situ ion irradiation experiment and computer simulation. Published by Elsevier B.V.

In this study, smaller-grained (hundred nano-meter size grain) and larger-grained ( micro-meter size grain) U-10Mo specimens have been irradiated (implanted) with 250 keV Xe_ beam and were in situ characterized by TEM. Xe bubbles were not seen in the specimen after an implantation fluence of 2 x 10(20) ions/m(2) at room temperature. Nucleation of Xe bubbles happened during heating of the specimen to a final temperature of 300 degrees C. By comparing measured Xe bubble statistics, the nucleation and growth behaviors of Xe bubbles were investigated in smaller-grained and larger-grained U-10Mo specimens. A multi-atom kind of nucleation mechanism has been observed in both specimens. X-ray Absorption spectroscopy showed the edge position in the bubbles to be the same as that of Xe gas. The size of Xe bubbles has been shown to be bigger in larger-grained specimens than in smaller-grained specimens at the same implantation conditions. (C) 2017 Elsevier B.V. All rights reserved.