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At least 595 records · Page 33

Retractable Sensor for Reactor Experiments

This presentation is to orient a mechanical or nuclear engineering senior design team so that they can help solve an instrumentation problem found in high power test reactors. Test reactors such as the Advanced Test Reactor (ATR) at the Idaho National Laboratory are used to irradiate nuclear fuels and materials to evaluate performance after high levels of exposure to a reactor in-pile environment. The purpose of the experiments is to determine property changes as the materials or fuels are bombarded with fast neutrons (and thermal (slow) neutrons as well). Typically, the irradiation must take place at a very specific temperature. Sometimes other parameters are monitored as well as properties such as creep, or gas composition, etc. However, the fast neutrons cause changes in not only the materials, but also in the transducers that are placed in the neutron flux, e.g., thermocouples or optical fibers. This task will be limited to considering temperature measurements. Thermocouples experience decalibration from not only the neutron flux, but also from the very high temperatures that are sometimes measured. Optical fibers darken in a neutron or gamma flux. However, it takes quite a few hours, or days for these changes to manifest. High power test reactors typically run at a constant power and so the temperature in an experiment is fairly stable over time. Because the changes are typically very slow, even a single temperature measurement per day, would provide 95% of a perfect data set. The basic concept of this effort is to push a very small diameter thermocouple or optical fiber into the location to be measured, leave it for 30 seconds or so for it to come to equilibrium, and transmit the signal, and then pull it up and away from the high neutron flux and high temperature region. The distance the thermocouple or fiber would need to move is on the order of 50 – 100 cm. By doing this, the thermocouple junction or optical fiber would spend only a few hours in the high flux/high temperature environment over the life of the irradiation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Evidence of lithium mobility under neutron irradiation

Understanding the evolution of intermetallic materials in high-radiation environments is of great importance for fusion science and national security. Tritium ( 3 H) and lithium ( 6 Li, 7 Li) transport within neutron irradiated claddings coated with aluminide (FeAl3) has been investigated using state-of-the-art multimodal imaging. Specifically, scanning electron microscopy – focused ion beam (SEM-FIB) was used to prepare irradiated coating lift-out samples for follow-on microanalysis. Here, scanning transmission electron microscopy (STEM) was used to acquire atomic-scale information on the carbonaceous structure and elemental mapping. Atomic force microscopy (AFM) was used to determine lift-out dimensions nondestructively. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) spectral and depth profiling show unexpected lithium isotopic distributions in the irradiated cladding, raising an important evidence of possible light isotope mobility within the cladding under elevated temperature and irradiation. ToF-SIMS three-dimensional chemical mappings of mid- and bottom-cladding coatings show light isotopic (e.g., 3 H, 6 Li, 7 Li) distributions in the irradiated coating and give new insights into the fundamental mechanism related to transport mechanisms within the cladding. Multimodal imaging is power to link microstructure, chemistry, and nanoscale defects that impact reliability of these materials. Furthermore, chemical mapping offers observations of the microstructural evolution due to irradiation and provides insights into unexpected material transport under extreme conditions.

36 MATERIALS SCIENCE↗

RaDIATE Collaboration for Material Studies

In the recent past, major accelerator facilities have been limited in beam power not by their accelerators, but by the beam intercepting device survivability. As next-generation accelerator target facilities (High Energy Physics, Spallation Sources, …) become increasingly more powerful and intense, high power target systems face key technical challenges. Beam-intercepting devices such as beam windows and secondary particle-production targets are continuously bombarded by high-energy high-intensity pulsed proton beams to produce secondary particles. Energy deposition from the primary beam induces near instantaneous heating (thermal shock) and microstructural changes (radiation damage) in the beam-intercepting materials. Both thermal shock and radiation damage ultimately degrade the performance and lifetime of targets and have been identified as the leading cross-cutting challenges of high-power target facilities. In order to operate reliable beam-intercepting devices in the framework of energy and intensity increase for next generation accelerators, the RaDIATE collaboration (Radiation Damage In Accelerator Target Environment) managed by Fermilab, brings together existing expertise in nuclear material and accelerator targets from 20 international institutions to execute a coordinated strategy for high power targetry R&D. This collaboration is generating new and useful materials data for application within the accelerator and the fission/fusion communities. I will give an overview of the RaDIATE R&D program and the achievement in the last few years on material studies in support of High Power Targetry development, including results obtained from irradiation test, development of novel materials and the prospective towards future irradiation campaign. A highlight will be given to the results in collaboration with our colleagues from J-PARC.

Pellemoine, Frederique↗

Atom probe tomography characterization of ion and neutron irradiated Alloy 800H

Alloy 800H is a high temperature and creep resistant alloy, and is considered as a candidate alloy for use in Generation IV nuclear reactor systems. To clarify the alloy's behavior under irradiation, samples were subjected to single ion irradiations up to 20 dpa at 440°C, a dual ion/He irradiation to 17 dpa at 460°C, and a neutron irradiation to 17 dpa at 385°C. The irradiated microstructures were characterized using atom probe tomography to complement previously published transmission electron microscopy studies. Additionally, after single ion irradiation, sparse fine Al and Ti clusters were observed after 1dpa, while high number densities of nanoscale Ni-Al-Ti clusters, Cr-Ti rich carbides, and Si-decorated dislocation loops developed after 10 and 20 dpa. The microstructure formed during single ion irradiation exhibited a strong depth dependence. No significant differences were observed between the single and dual ion irradiations. While Ni-Al-Ti clusters, Cr-Ti rich carbides, and Si-decorated dislocation loops were also observed after neutron irradiation, the neutron-irradiated microstructure differed from those found in the ion-irradiated samples.

36 MATERIALS SCIENCE↗

Microstructural and compositional evolutions in $γ$-LiAlO 2 pellets during ion irradiation at an elevated temperature

This study reports on the microstructural, phasic and compositional evolutions of γ-LiAlO 2 during ion irradiation. Polycrystalline γ-LiAlO 2 pellets were irradiated sequentially with He + and D 2 + ions to the same combined fluences of up to 3 × 10 17 (He + +D + )/cm 2 at 773 K. The irradiated pellets were characterized using scanning transmission electron microscopy and atom probe tomography. Surface amorphization likely due to radiolysis and planar defects as a possible precursor for formation of precipitates are created at 5 × 10 16 (He + +D + )/cm 2 , followed by the formation of nano-sized precipitates and fractures at higher doses. Spinel-like precipitates of non-stoichiometric LiAl 5 O 8 and gas-filled cavities are observed to grow with increasing dose. Faceted precipitates and rounded cavities appear at 2 × 10 17 (He + +D + )/cm 2 . With further increasing ion fluence to 3 × 10 17 (He + +D + )/cm 2 , amorphization of the precipitates takes place and micron-sized fractures appear. Surface exfoliation could occur at an extremely high ion fluence. There are compositional changes in the γ-LiAlO 2 pellets during the microstructural evolution. In the precipitate and amorphized regions, Li concentrations decrease to ~7 and 3.7 at.% from 25 at.% in γ-LiAlO 2 , respectively. This study reveals a full-cycle microstructural evolution with corresponding compositional changes in γ-LiAlO 2 pellets during ion irradiation at 773 K. In conclusion, the data could help model, assess, and predict the material performance during neutron irradiation in reactors.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Irradiation effects in tungsten—From surface effects to bulk mechanical properties

Advanced materials such as tungsten fibre-reinforced composites allow to overcome severe weaknesses of the baseline materials for plasma-facing components — copper and tungsten. The effect of the fusion environment on the mechanical properties of these materials, e.g. the embrittlement by neutron irradiation, plays a key role for the development of future fusion reactors. To simulate this effect, high-energy ions are used as a substitute for the displacement damage by neutrons. We propose the use of very fine tungsten wire as a possibility of studying the influence of irradiation damage on the mechanical properties. This is possible as they allow full-depth irradiation of almost the entire volume despite the limited penetration depth of ions. Geometrical size effects are mitigated due to the nanoscale microstructure of the wire. In addition, similar wire is used in tungsten fibre-reinforced composites. Thus, the investigation of irradiated wire can directly be used for the prediction of the bulk composite properties. For the proof of this concept tungsten wire with a diameter of 16 μm was electrochemically thinned to 5 μm and irradiated with 20.5 MeV W 6+ ions. The mechanical properties were subsequently determined by macroscopic tensile testing. Irradiation to 0.3, 1 and 9 dpa did not lead to a change of the mechanical behaviour. Both strength and ductility, the latter indicated by the reduction of area, were similar to the as-fabricated state.

36 MATERIALS SCIENCE↗

Implementing Automation of Foreign Obligations Tracking at SRS

Obligated Nuclear Material Principles • Stay with the originating item if at all practical. • Additional principles apply to bulk processes for pool accounting. • Fungibility: Individual units are indistinguishable therefore equal units are interchangeable. • Equivalence: Material of the same quality and same quantity • Isotopic composition • Physical and chemical form • State: fresh, irradiated, waste • Proportionality: If material is mixed and is processed, a proportion of the resultant material will be obligated in the same proportion as the originating material.

Ramsey, Catherine M. [Savannah River National Labo↗

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

We discuss the need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I 3 TEM) is designed to explore these principles. To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I 3 TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind. Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I 3 TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

47 OTHER INSTRUMENTATION↗

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗

Characterization of boundary precipitation in a heavy ion irradiated tungsten heavy alloy under the simulated fusion environment

In the concerted effort to identify materials capable of surviving the adverse environment of a fusion reactor interior, tungsten heavy alloys have been put forth as leading candidates. Experimental trials and behavioral studies have yielded positive results for their adoption by taking advantage of the alloy’s unique balance of inherently high fracture toughness and low sputter yields; yet due to their relative novelty in the fusion community, there remains a lack of understanding on the response of these materials to the extended high temperature irradiation environment of the reactor interior. Further, to alleviate this issue and provide the necessary data on the behavior of tungsten heavy alloys to the simulated fusion environment, a 90W-7Ni-3Fe alloy has been subjected to elevated temperature sequential Ni + and He + ion irradiations to mimic the expected displacement damage and gas production expected after five years of service as a plasma facing material component. Atomic-scale structural analyses and nanoscale chemical mapping have identified the formation of two distinct precipitation structures, a surface localized η-carbide and an a-W 2 C type tungsten carbide, both of which appear to originate at the bi-phase interface between W and the ductile phase. This irradiation assisted and induced precipitate formation respectively is anticipated to adversely affect these materials by selective embrittlement at bi-phase interfaces leading to a reduction in the material’s overall fracture toughness during prolonged high temperature irradiation. It is asserted that any potential exposure to C during fusion reactor operational service should be minimized as to prevent the formation of these phases.

36 MATERIALS SCIENCE↗

Effects of electron irradiation on large insulating surfaces used for European Communications Satellites

Samples of aluminized Kapton used for passive thermal control on the VHF shield and the antenna dish of ESA's OTS satellite and its derivatives were subjected to an incident electron beam of 25 keV and irradiated for 8 hours at room temperature and at -173 C under a vacuum of the 10 to the minus 6 th power torr. Visual observations during electron irradiation, measurements of leakage current and discharge characteristics, and material degradation following completion of irradiation are discussed.

Reddy, J.↗

Radial radio frequency (RF) electron guns

Radial radio frequency (RF) electron guns and radial RF electron gun systems are provided that are capable of generating an electron beam that can propagate either radially inward, towards the axis of a cylinder, or radially outward from the axis. A beam source capable of generating a radially inwardly propagating electron beam, while perhaps not particularly useful as a source for a higher-energy accelerator, offers potential advantages for materials processing, as the geometry allows irradiation from all sides of an enclosed material flow with a single structure. Other potential applications include, but are not limited to, atmospheric plasma generation, radiation damage testing, and possibly, novel electron lens-type devices for hadron accelerators.

Lewellen, John↗

Impacts of irradiation-induced nanostructure on phonon linewidths and thermal conductivity in U-Zr alloy

Ion irradiation can significantly change material properties. Thermal conductivity degradation of reactor fuel is detrimental to safety and efficiency—driving research on how irradiation impacts heat-carrying phonons. Here, we report the measurements of phonon dispersion and lifetimes (inverse linewidths) in freestanding irradiated crystals and reveal the relationship between thermal conductivity and proton irradiation induced nanostructures in UZr 2.6 using inelastic x-ray scattering, electron microscopy, modulated thermoreflectance, and first-principles calculations. Irradiation results in more significant increases in phonon linewidths and decreased thermal conductivity in the basal plane than that along the c axis, decreasing thermal conductivity anisotropy. Furthermore, microscopy reveals that this results from irradiation induced nanoprecipitates and metastable phase separation. Surprisingly, irradiation leads to smaller phonon linewidths near some zone boundaries, which we attribute to irradiation induced short-range order.

36 MATERIALS SCIENCE↗

Krypton-85 chronometry of spent nuclear fuel

We describe the use of the radionuclide 85 Kr, which is produced by nuclear fission and has a half-life of 10.76 years, to determine the age of spent nuclear fuel. The method is based on mass-spectrometric measurement of the relative abundance of fissiogenic Kr isotopes extracted from a fuel sample, and we show that it can be applied to micron-scale particles of spent fuel that are analogous to particles that have been released into the environment from various nuclear facilities in the past. 85 Kr chronometry is potentially valuable for identifying and attributing nuclear materials, grouping samples into collections of common origin that can be used to reconstruct the origin and irradiation history of the material, and verifying declared nuclear activities in the context of international monitoring programs.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Radiation-Induced Modifications in Copper Oxide Growth

Radiation-induced effects and their influence on oxidation processes were evaluated for their use as a forensic tool for special nuclear material (SNM). A beam of 10 MeV Au³⁺ ions was used to mimic the accumulation of microstructural damage from self-irradiation through the decay of radionuclides. Several copper samples were irradiated as suitable surrogate materials at 200 °C with a flux of 1x10¹² ions/cm·s to damage levels of 5, 10, and 15 displacements per atom (dpa). This corresponds to about 50, 100, and 150 years, respectively, of accumulated α-decay damage in a PuGa alloy assuming a damage rate of 0.1 dpa/year. After irradiation, all samples were exposed to an accelerated aging process induced by thermal treatment at 350 °C for 1 hour in air. This resulted in the growth of a mixed oxide layer (Cu₂O and CuO) which was characterized in detail using several complementary analytical techniques: Scanning Electron Microscopy, Raman spectroscopy, Synchrotron X-ray diffraction (transmission mode), and Grazing Incidence X-ray diffraction. The oxide layer growth of irradiated Cu at 350°C is distinctly modified as a result of the ion irradiation. Most notably, the growth of the CuO phase is suppressed with increasing radiation damage on the Cu substrate, and structural changes occurred in the Cu₂O phase. These results indicate that damage from self-irradiation over time can cause quantifiable modifications in the oxidation process of metals that could be harnessed for their use as a novel forensic tool.

36 MATERIALS SCIENCE↗

Latent Tracks in Ion-Irradiated LiTaO 3 Crystals: Damage Morphology Characterization and Thermal Spike Analysis

Systematic research on the response of crystal materials to the deposition of irradiation energy to electrons and atomic nuclei has attracted considerable attention since it is fundamental to understanding the behavior of various materials in natural and manmade radiation environments. This work examines and compares track formation in LiTaO3 induced by separate and combined effects of electronic excitation and nuclear collision. Under 0.71–6.17 MeV/u ion irradiation with electronic energy loss ranging from 6.0 to 13.8 keV/nm, the track damage morphologies evolve from discontinuous to continuous cylindrical zone. Based on the irradiation energy deposited via electronic energy loss, the subsequently induced energy exchange and temperature evolution processes in electron and lattice subsystems are calculated through the inelastic thermal spike model, demonstrating the formation of track damage and relevant thresholds of lattice energy and temperature. Combined with a disorder accumulation model, the damage accumulation in LiTaO3 produced by nuclear energy loss is also experimentally determined. The damage characterizations and inelastic thermal spike calculations further demonstrate that compared to damage-free LiTaO3, nuclear-collision-damaged LiTaO3 presents a more intense thermal spike response to electronic energy loss owing to the decrease in thermal conductivity and increase in electron–phonon coupling, which further enhance track damage.

36 MATERIALS SCIENCE↗