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High-performance structural materials (HPSMs) are needed for the successful and safe design of fission and fusion reactors. Their operation is associated with unprecedented fluxes of high-energy neutrons and thermomechanical loadings. In fission reactors, HPSMs are used, e.g., for fuel claddings, core internal structural components and reactor pressure vessels. Even stronger requirements are expected for fourth-generation supercritical water fission reactors, with a particular focus on the HPSM's corrosion resistance. The first wall and blanket structural materials in fusion reactors are subjected not only to high energy neutron irradiation, but also to strong mechanical, heat and electromagnetic loadings. This paper presents a historical and state-of-the-art summary focused on the properties and application potential of irradiation-resistant alloys predominantly strengthened by an oxide dispersion. These alloys are categorized according to their matrix as ferritic, ferritic-martensitic and austenitic. Low void swelling, high-temperature He embrittlement, thermal and irradiation hardening and creep are typical phenomena most usually studied in ferritic and ferritic martensitic oxide dispersion strengthened (ODS) alloys. In contrast, austenitic ODS alloys exhibit an increased corrosion and oxidation resistance and a higher creep resistance at elevated temperatures. This is why the advantages and drawbacks of each matrix-type ODS are discussed in this paper.

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Raman spectroscopy is an emerging technique for rapid and nondestructive analysis of nuclear materials for forensic and nonproliferation applications as it is a powerful tool for distinguishing multiple chemical forms of materials with similar stoichiometries. Recent developments in spectroscopic software have enabled rapid data collection with high-speed Raman spectroscopic mapping capabilities. However, some uranium-rich materials are susceptible to degradation in humid air and/or laser-induced phase transformations. To mitigate environmental or measurement-related sample degradation of potential samples of interest, we have taken a systematic approach to define optimized data collection parameters for high-throughput measurements of uranyl fluoride (UO2F2), which is an important intermediate material in the nuclear fuel cycle. First, we systematically describe the influence of optical magnification (5× to 100×), laser power, and exposure time on obtained signal for identical particles of UO2F2 and find that at low laser power and exposure times, comparable signal is obtained regardless of optical magnification. Second, we ensure sample integrity during data collection, and third, collect spectroscopic maps that employ optimized parameters to reduce the time required to obtain spatially resolved spectroscopic information. Reductions of 90% and 99% in measurement times are discussed as they relate to differences in resolving spectroscopic features of particles in identical mapping areas. During this work, we found that additional data processing options were needed and thus developed a customized Python script for importing, processing, analyzing, and visualizing Raman spectroscopic map data.

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The suitability and applications of Total reflection X-ray Fluorescence (TXRF) for characterization of nuclear materials are numerous. TXRF has been successfully applied for trace, minor and major determinations of constituents in nuclear materials such as fuel, clad, control rod, coolant, etc. The two major advantages of TXRF i.e. requirement of very small sample for analysis and non-requirement of matrix matched standards, make this technique further more attractive and suitable for nuclear industry. The applications of TXRF for trace analysis in nuclear materials such as fuel, clad, coolant and control rods are described in detail along with its applications for determination of major and speciation studies in TXRF mode.

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Nuclear reactions with charged particles have applications in many fields such as radioisotope production, industrial applications, astrophysics, etc. Therefore, examining the excitation functions performed and obtained by the activation technique is also important for understanding the nature of nuclear reactions. Also, it is especially necessary to study these reactions to estimate the effects of radiation damage on the fusion structural materials used in the construction of the first walls and core of the reactor. In this study, cross-section data have been calculated theoretically to 45Sc (d, 3n)44Ti, 63Cu (d, 3n)62Zn, 89Y (d, 3n)88Zr, and 100Mo (d, 3n)99Tc reactions in the range of 1-50 MeV energy via ALICE/ASH, TALYS 1.95 and Empire 3.2.2 nuclear reaction codes. Optical Model Parameters (OMP) calculation for deuteron-induced reaction results has been performed via TALYS 1.95 code and the calculated cross-section values are reproduced well. Also, empirically developed (d, 3n) cross section formula (Kavun, 2020) calculations have been performed at 20 MeV energy. Finally, experimental EXFOR data was compared with all results and were found to be compatible with each other.

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Structural materials of the new generation of nuclear reactors, fission as well as fusion, must often cope with high production rates of transmutation helium. Their testing hence requires either a powerful source of fast neutrons or a high-fluence ion-irradiation facility providing sufficient amounts of high-energy helium to investigate its effect on the material. Most ion irradiation studies, however, concentrate on basic effects such as defect evolution or bubble swelling in narrow near-surface regions modified by ion bombardment. Studies on bulk samples with a relatively thick implanted region, which would enable, for instance, micromechanical testing, are underrepresented. This gap might be filled by high-fluence multi-energy ion irradiations modifying several tens of micrometres of the investigated substrate. High-energy ion accelerators providing reasonable currents with energies of tens of MeV are rarely employed in such studies due to their scarcity or considerable beamtime costs. To contribute to this field, this article reports a unique single-beam He implantation experiment aimed at obtaining quasi-uniform displacement damage across >60 µm with the He/dpa ratio roughly one order of magnitude above the typical spallation neutron target irradiation conditions. Some technical aspects of this irradiation experiment, along with recent developments and upgrades at the 6 MV Tandetron accelerator of the Slovak university of technology in Bratislava, are presented.

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In this work, the optical characteristics of uranium (U), lead (Pb), cobalt (Co), and thorium (Th) nanoparticles are fashioned and simulated employing the finite element analysis (FEA) approach concerning multiple particle sizes. Applying finite element analysis, it was found that the simulated absorption peaks of electronic excitations of nuclear nanoparticles are red-shifted from 365 nm to 555 nm for U; from 355 nm to 550 nm for Pb; from 415 nm to 610 nm for Co; and from 350 nm to 540 nm for Th, comparing expanding particle sizes from 60 nm to 100 nm (except for Co, which varied from 70 nm to 100 nm). The FEA-simulated optical band gap energies and far-field radiation patterns were also obtained for nuclear materials. The simulation approach in this research enables the prediction of optical properties and design of nuclear materials before manufacture for nuclear security applications.

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Nanograined nuclear materials are expected to have a better performance as spallation targets and nuclear fuels than conventional materials, but many basic properties of these materials are still unknown. The present work aims to contribute to their better understanding by studying the effect of grain size on the melting and solid-solid transitions of nanograined UC2-y. We laser-heated 4 nm-10 nm grain size samples with UC2-y as the main phase (but containing graphite and UO2 as impurities) under inert gas to temperatures above 3000 K, and their behavior was studied by thermal radiance spectroscopy. The UC2-y solidification point (2713(30) K) and α-UC2 to ß-UC2 solid-solid transition temperature (2038(10) K) were observed to remain unchanged when compared to bulk crystalline materials with micrometer grain sizes. After melting, the composite grain size persisted at the nanoscale, from around 10 nm to 20 nm, pointing to an effective role of carbon in preventing the rapid diffusion of uranium and grain growth.

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Helium is insoluble in most metals and precipitates out to form nanoscale bubbles when the concentration is greater than 1 at.%, which can alter the material properties. Introducing controlled defects such as multilayer interfaces may offer some level of helium bubble management. This study investigates the effects of multilayered composites on helium behavior in ion-implanted, multilayered ErD2/Mo thin film composites. Following in-situ and ex-situ helium implantation, scanning and transmission electron microscopy showed the development of spherical helium bubbles within the matrix, but primarily at the layer interfaces. Bubble linkage and surface blistering is observed after high fluence ex-situ helium implantation. These results show the ability of metallic multilayers to alter helium bubble distributions even in the presence of a hydride layer, increasing the lifetime of materials in helium environments.

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During neutron irradiation of metals, owing to the enhanced number of vacancies and interstitial atoms, the climb motion of dislocations becomes significant at room temperature, leading to a recrystallization of the material. Moreover, the vacancies and interstitial atoms tend to form prismatic dislocation loops that play a crucial role in the plastic properties of the materials. X-ray peak profile analysis is an efficient nondestructive method to determine the properties of dislocation microstructure. In the first half of this article, the foundation of the asymptotic peak broadening theory and the related restricted-moments peak-evaluation method is summarized. After this, the microstructural parameters obtained by X-ray peak profile analysis are reported for irradiated E110 and E110G Zr alloys used as cladding material in the nuclear industry.

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Secondary Ion Mass Spectrometry is an important technique for the study of the composition of a wide range of materials because of the exceptionally high sensitivity that allows the study of trace elements and the ability to distinguish isotopes that can be used as markers for reactions and transport processes. However, when studying nuclear materials, it is often necessary to analyse highly radioactive samples, and only rather few SIMS facilities are available in active environments. In this paper, we present a methodology using focussed ion beam milling to prepare samples from radioactive specimens that are sufficiently large to undertake SIMS mapping experiments over microstructurally significant regions, but with overall activities small enough to be readily transported and analysed by a SIMS instrument in a normal laboratory environment. Radioactive samples prepared using this methodology can also be used for correlative SIMS analysis with other analytical microscopies. SIMS results showing the distributions of deuterium in oxides on in-reactor corroded zirconium alloys are presented to demonstrate the potential of this sample preparation technique.

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Mass attenuation coefficients (MACs) of Th, U, Np, and Pu for oxygen X-rays have been experimentally determined using an electron microprobe. The MACs were obtained by measuring relative X-ray intensities emitted from ThO2, UO2, NpO2, and PuO2 targets, for incident electron energies from 5 to 30 keV, and processing them with the help of the computer program XMAC. The accuracy of the measured MACs is estimated to be better than 5%. Results are compared with MAC tabulations commonly used in electron probe microanalysis as well as with theoretical photoionization calculations. It is concluded that the MACs implemented in the Monte Carlo simulation program PENELOPE which are based on the photoionization cross-section calculations of Sabbatucci & Salvat [(2016). Theory and calculation of the atomic photoeffect. Rad Phys Chem121, 122-140], provide the best agreement with our measurements. The use of different MAC schemes for the analysis of mixed actinide oxide materials is discussed.

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Porous uranium oxide hollow sphere nanoparticles were synthesized in ionic liquids under hydrothermal conditions. Various precipitating agents and ionic liquids were investigated to determine their respective impact on the resultant uranium oxide morphologies. Using hydrazine hydrate as precipitating agent and N-butyl pyridinium bromide as templating agent, a porous-hollow structure was created with a surface area of 1958 m2.g-1 and an average pore diameter of 30 nm. The nanoparticles revealed high peroxidase-mimicking activity. This was evaluated by using the peroxidase substrate 3,3',5,5'-tetramethylbenzidine (TMB) that is catalytically oxidized by H2O2 to give oxidized TMB (oxTMB) which is blue (with an absorption peak at 652 nm). The material was used as a nanozyme for colorimetric detection of Sn2+. Meanwhile, it is found that BSA strongly improves the catalytic activity of the nanozyme, while Sn(II) inhibits its activity. Thus, a colorimetric method for Sn2+ detection was designed. The method works in the 0.5-100 µM Sn(II) concentration range and has a lower detection limit of 0.36 µM (at S/N = 3). Graphical abstract The catalytic activity of porous-hollow nano-UO2 toward the oxidation of 3,3',5,5'-tetramethylbenzidine by H2O2 is remarkably improved in the presence of bovine serum albumin, while tin(II) inhibits its activity. This finding has been applied to design a method for colorimetric quantification of tin(II) in water samples.

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Analysis and understanding of the role of hydrogen in metals is a significant challenge for the future of materials science, and this is a clear objective of recent work in the atom probe tomography (APT) community. Isotopic marking by deuteration has often been proposed as the preferred route to enable quantification of hydrogen by APT. Zircaloy-4 was charged electrochemically with hydrogen and deuterium under the same conditions to form large hydrides and deuterides. Our results from a Zr hydride and a Zr deuteride highlight the challenges associated with accurate quantification of hydrogen and deuterium, in particular associated with the overlap of peaks at a low mass-to-charge ratio and of hydrogen/deuterium containing molecular ions. We discuss possible ways to ensure that appropriate information is extracted from APT analysis of hydrogen in zirconium alloy systems that are important for nuclear power applications.

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An automated separation-direct analysis scheme has been developed to determine both the concentration and isotopic composition of a suite of elements down to the low picogram level in a complex silicon-based matrix. With the ultimate goal of performing rapid analysis of materials with non-natural isotopic compositions, RAPID (Rapid Analysis of Post-Irradiation Debris) consists of a high-pressure ion chromatography system directly coupled to an inductively coupled plasma mass spectrometer. The RAPID method achieves matrix exclusion and direct online analysis of the elementally separated components, yielding precise isotopic compositions for up to 40 elements in less than one hour per sample. When combined with isotope dilution, this approach shows the potential to yield elemental concentrations with low uncertainties, providing a rapid analytical method that encompasses group I and II metals, transition metals, refractory metals, platinum group metals, lanthanides, and actinides. The method development, robustness, sensitivity, uncertainties, and potential applications in nuclear and environmental measurements will be discussed in this paper.

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The effect of the strain rate, experimental temperature, Zn content in the test solution, and prefilming time on the mechanical properties was investigated by a tensile test with a slow strain rate, at a chemical solution of 2.2 ppm Li and 1200 ppm B in a static autoclave with 8.2 MPa. The experimental parameters clearly affected the tensile properties. The surface morphology, fractograph, and cross-sectional microstructure were analyzed by scanning electron microscopy and transmission electron microscopy. The δ (elongation) and UTS (ultimate tensile strength) of the samples tested in chemical solution were obviously lower than those of the samples tested under a nitrogen atmosphere. However, in general, all samples showed a ductile fracture characteristic and an excellent tensile property in all experimental conditions. The δ and UTS were first increased with increasing Zn content, and then decreased at both conditions of 9.26 × 10-7/s and 4.63 × 10-7/s strain rates. The difference values of tensile properties at different strain rates showed fluctuations with increasing Zn content. The δ increased with both increasing experimental temperature and prefilming time. The UTS first decreased with increasing prefilming time and then increased. The Iscc (stress corrosion cracking susceptibility) decreased with an increasing strain rate, experiment temperature, and prefilming time. Many particles with polyhedrons were formed on the sample surfaces, which was attributed to corrosion in a periodical location at the sample surface. The average length of the particles decreased with increasing Zn content, but increased with both increasing experimental temperatures and prefilming time. The corresponding mechanism is also discussed in this work.

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A portable handheld laser-induced breakdown spectroscopy (HH LIBS) instrument was evaluated as a rapid method to qualitatively analyze rare earth elements in a uranium oxide matrix. This research is motivated by the need for development of a method to perform rapid, at-line chemical analysis in a nuclear facility, particularly to provide a rapid first pass analysis to determine if additional actions or measurements are warranted. This will result in the minimization of handling and transport of radiological and nuclear material and subsequent exposure to their associated hazards. In this work, rare earth elements (Eu, Nd, and Yb) were quantitatively spiked into a uranium oxide powder and analyzed by the HH LIBS instrumentation. This method demonstrates the ability to rapidly identify elemental constituents in sub-percent levels in a uranium matrix. Preliminary limits of detection (LODs) were determined with values on the order of hundredths of a percent. Validity of this methodology was explored by employing a National Institute of Standards and Technology (NIST) standard reference materials (SRM) 610 and 612 (Trace Elements in Glass). It was determined that the HH LIBS method was able to clearly discern the rare earths elements of interest in the glass or uranium matrices.

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The formation of radiation-induced dislocation loops and voids in tantalum at 180(2), 345(3) and 590(5)°C was assessed by 3MeV proton irradiation experiments and subsequent damage characterisation using transmission electron microscopy. Voids formed at 345(3)°C and were arranged into a body centred cubic lattice at a damage level of 0.55 dpa. The low vacancy mobility at 180(2)°C impedes enough vacancy clustering and therefore the formation of voids visible by TEM. At 590(5)°C the Burgers vector of the interstitial-type dislocation loops is a<100>, instead of the a/2 <111> Burgers vector characteristic of the loops at 180(2) and 345(3)°C. The lower mobility of a<100> loops hinders the formation of voids at 590(5)°C up to a damage level of 0.55 dpa.

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Some illustrations of the use of deuterium or tritium for isotopic tracing of hydrogen absorption, transport and trapping in nuclear materials are presented. Isotopic tracing of hydrogen has been shown to be successful for the determination of the boundaries conditions for hydrogen desorption or absorption in a material exposed to a hydrogen source. Also, the unique capabilities of isotopic tracing and related techniques to characterize H interactions with point defects and dislocations acting as moving traps has been demonstrated. Such transport mechanisms are considered to play a major role in some stress corrosion cracking and hydrogen embrittlement mechanisms.This article is part of the themed issue 'The challenges of hydrogen and metals'.

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Nuclear forensics techniques, including micro-XRF, gamma spectrometry, trace elemental analysis and isotopic/chronometric characterization were used to interrogate two, potentially related plutonium metal foils. These samples were submitted for analysis with only limited production information, and a comprehensive suite of forensic analyses were performed. Resulting analytical data was paired with available reactor model and historical information to provide insight into the materials' properties, origins, and likely intended uses. Both were super-grade plutonium, containing less than 3% 240Pu, and age-dating suggested that most recent chemical purification occurred in 1948 and 1955 for the respective metals. Additional consideration of reactor modeling feedback and trace elemental observables indicate plausible U.S. reactor origin associated with the Hanford site production efforts. Based on this investigation, the most likely intended use for these plutonium foils was 239Pu fission foil targets for physics experiments, such as cross-section measurements, etc.