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At least 73 records · Page 4

Pushing the limits of high-resolution polymer microscopy using antioxidants

High-resolution transmission electron microscopy (HRTEM) has been transformative to the field of polymer science, enabling the direct imaging of molecular structures. Although some materials have remarkable stability under electron beams, most HRTEM studies are limited by the electron dose the sample can handle. Beam damage of conjugated polymers is not yet fully understood, but it has been suggested that the diffusion of secondary reacting species may play a role. As such, we examine the effect of the addition of antioxidants to a series of solution-processable conjugated polymers as an approach to mitigating beam damage. Characterizing the effects of beam damage by calculating critical dose D c values from the decay of electron diffraction peaks shows that beam damage of conjugated polymers in the TEM can be minimized by using antioxidants at room temperature, even if the antioxidant does not alter or incorporate into polymer crystals. As a consequence, the addition of antioxidants pushes the resolution limit of polymer microscopy, enabling imaging of a 3.6Å lattice spacing in poly[(5,6-difluoro-2,1,3-benzothiadiazol-4,7-diyl)-alt-(3,3"-di(2-octyldodecyl)-2,2';5',2";5",2"-quaterthiophene-5,5"-diyl)] (PffBT4T-2OD).

36 MATERIALS SCIENCE↗

Multidimensional genome-wide screening in yeast provides mechanistic insights into europium toxicity

Abstract Europium is a lanthanide metal that is highly valued in optoelectronics. Even though europium is used in many commercial products, its toxicological profile has only been partially characterized, with most studies focusing on identifying lethal doses in different systems or bioaccumulation in vivo. This paper describes a genome-wide toxicogenomic study of europium in Saccharomyces cerevisiae, which shares many biological functions with humans. By using a multidimensional approach and functional and network analyses, we have identified a group of genes and proteins associated with the yeast responses to ameliorate metal toxicity, which include metal discharge paths through vesicle-mediated transport, paths to regulate biologically relevant cations, and processes to reduce metal-induced stress. Furthermore, the analyses indicated that europium promotes yeast toxicity by disrupting the function of chaperones and cochaperones, which have metal-binding sites. Several of the genes and proteins highlighted in our study have human orthologues, suggesting they may participate in europium-induced toxicity in humans. By identifying the endogenous targets of europium as well as the already existing paths that can decrease its toxicity, we can determine specific genes and proteins that may help to develop future therapeutic strategies.

59 BASIC BIOLOGICAL SCIENCES↗

Rapid Simulation of Irradiation Damage in PWR Internals (NSUF 2019 Milestone Report)

This document summarizes the progress made by Oak Ridge National Laboratory (ORNL) in collaboration with the University of Michigan on “Rapid Simulation of Irradiation Damage in PWR Internals,” a research project led by the University of Michigan and supported by US Department of Energy Office of Nuclear Energy Nuclear Science User Facilities Consolidated Innovative Nuclear Research program. In this reporting period, samples that were exposed to combined neutron and ion irradiation were prepared and shipped to the University of Michigan for further analysis. This report summarizes the specimen preparation performed at ORNL’s Low Activation Materials Development and Analysis facility. The benchmarking work of microstructural characterization on reactor-irradiated samples with different dose levels was completed.

36 MATERIALS SCIENCE↗

NSUF RTE completion report for 23-4780: Microstructural Defect Induced Thermal Conductivity Reduction in Uranium Nitride and Thorium Nitride

Uranium nitride (UN) is known to have a higher thermal conductivity than traditional oxide fuels, which could lead to a more efficient energy transport and lower local temperature during its lifetime. But the thermal transport performance of UN in extreme environments has not been systematic studied. This study investigated the irradiation induced microstructural defects in UN and the impacts on thermal conductivity. The samples were produced by spark plasma sintering at University of Texas-San Antonio (UTSA), Los Alamos National Laboratory (LANL), and Idaho National Laboratory (INL). Thermal conductivity of UN before and after 2MeV proton irradiation were measured by using laser metrology at INL in a temperature range of 77-295K. Thermal conductivity measurements in this wide, cryogenic temperature range is critical to understand the phonon scattering mechanisms between the thermal energy carrier, phonons, and different types of irradiation-induced defects. In order to ensure the measurements were conducted in the same grains and minimize the impact of the local heterogeneities, the measurement locations were highlighted by fiducial marks using the focused ion beam (FIB) with grain orientation identified using the electron backscatter diffraction (EBSD) at the Center of Advanced Energy Studies (CAES). Irradiation experiment was conducted at the Ion Beam Laboratory at Texas A&M University (TAMU). A total of 6 samples were irradiated with different irradiation doses and temperatures. After irradiation, the microstructure was characterized by using Transmission Electron Microscope (TEM) at CAES (also in the FIB marks).

36 - MATERIALS SCIENCE↗

Laboratory Infection of Novel Akhmeta Virus in CAST/EiJ Mice

Akhmeta virus is a zoonotic Orthopoxvirus first identified in 2013 in the country of Georgia. Subsequent ecological investigations in Georgia have found evidence that this virus is widespread in its geographic distribution within the country and in its host-range, with rodents likely involved in its circulation in the wild. Yet, little is known about the pathogenicity of this virus in rodents. We conducted the first laboratory infection of Akhmeta virus in CAST/EiJ Mus musculus to further characterize this novel virus. We found a dose-dependent effect on mortality and weight loss (p < 0.05). Anti-orthopoxvirus antibodies were detected in the second- and third-highest dose groups (5 × 104 pfu and 3 × 102 pfu) at euthanasia by day 10, and day 14 post-infection, respectively. Anti-orthopoxvirus antibodies were not detected in the highest dose group (3 × 106 pfu), which were euthanized at day 7 post-infection and had high viral load in tissues, suggesting they succumbed to disease prior to mounting an effective immune response. In order of highest burden, viable virus was detected in the nostril, lung, tail, liver and spleen. All individuals tested in the highest dose groups were DNAemic. Akhmeta virus was highly pathogenic in CAST/EiJ Mus musculus, causing 100% mortality when ≥3 × 102 pfu was administered.

59 BASIC BIOLOGICAL SCIENCES↗

Advanced Microscopy and Spectroscopy for Probing and Optimizing Electrode-Electrolyte Interphases in High Energy Lithium Batteries (Final Scientific/Technical Report)

The earliest developed LiCoO 2 layered oxide cathode material sparked the development of other layered cathode materials, dominating the positive electrode materials for lithium ion batteries. Within the practical operating conditions of today, the current generation layered oxide materials do not meet the future energy storage demands of 350 Wh kg -1 at cell level. Li-rich layered oxide (LRLO) materials have the potential to meet the high energy demands. Unlike the classical layered oxides, LRLO materials exhibit capacities that go beyond conventional topotactic mechanistic theoretical values. Despite its high capacities, this material has several challenges (voltage fading, structural instability, sluggish kinetics, cathode electrolyte interphase instability, etc.) that must be overcome in order to reach commercialization. In the past five years, our research group has made great progress on developing advanced characterization techniques coupled with atomic scale modeling to properly characterize the dynamic phenomena that govern the performance limitations of LRLO materials. Furthermore, our efforts have guided the material synthesis and surface modification to improve capacity retention. By carefully controlling the oxygen activities through the creation of uniform oxygen vacancies, we were able to avoid structural decomposition in LRLO. Our materials deliver a discharge capacity as high as 306 mAh g -1 with an initial coulombic efficiency of 90.6%. Furthermore, they do not exhibit obvious capacity decay with a reversible capacity over 300 mAh g -1 after 100 cycles at 0.1 C-rate. Our approach demonstrates the critical needs for advanced diagnosis and characterization. It is through the in-depth understanding of these high voltage cathode materials at atomistic and molecular level and their dynamic changes during the operation of batteries; we can successfully formulate strategies to further optimize this class of cathode materials, especially for the voltage instabilities. The diagnostic tools developed here can also be leveraged to study anode materials such as Li metal anode. The challenge of probing Li metal is the low dose tolerance (high beam sensitivity) of Li metal. We will have to apply cryogenic method (low-temperature) and low-dose electron microscopy and specialized camera to enable the characterization of the lithium metal.

25 ENERGY STORAGE↗

HFIR SiC-SiC Composite Clad Tube Bowing Test: Pre-Irradiation Characterization

This report describes the pre-irradiation characterization of the SiC-SiC composite clad tube bowing experiment that will be irradiated in the High Flux Isotope Reactor (HFIR). There are concerns that SiCSiC fuel cladding in light water reactors could undergo bowing because of the non-uniform fast neutron flux profiles. This experiment is combined with the SiC-SiC channel box experiment, which has similar concerns regarding control blade movements in boiling water reactors. The HFIR experiment aims to validate the predicted deformation and stresses in the composite clad specimen after the exposure of fast neutron flux gradients. Significant radial fast neutron flux gradients that exist in the permanent reflector of HFIR were thoroughly characterized by using detailed 3D neutronic calculations. The 3D displacement damage dose rate profile and the resulting volumetric swelling in SiC were used as inputs to structural analyses to determine the predicted deformation that will affect the specimens. The tube specimens were characterized by using traditional dimensional inspection and surface profilometry to provide detailed information regarding the pre-irradiation condition as the first step to evaluate the radiation-induced deformation. Furthermore, fine engraving markers were inscribed along all outer surfaces of the specimen and mapped by using a digital microscope and a multidimensional stage. This allows marker spacings to be accurately measured and compared with similar measurements that will be made post-irradiation to provide local radiation-induced strain mapping. The experiment successfully completed two HFIR cycle irradiations, cycles 492 and 493, which finished on July 25, 2021.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Energy Characterization of the UMD Electron Accelerator

Multiple different groups at Los Alamos National Laboratory have a cited interest in understanding the effects of ionizing radiation in materials. Of especial interest to the ISR division is understanding the effects in materials that are used in the space environment, where radiation is omnipresent and impossible to fully shield from. Development is under way to simulate the effects of radiation damage in detectors and electronics, primarily with particle transport codes such as Geant4 and RAMPART, a code that provides a user friendly interface to Geant4. However, these simulations need benchmarking to experimental tests, some of which have been performed at a variety of small electron accelerator facilities. One of these facilities is the Linear Electron Accelerator at the University of Maryland Radiation Facilities. This facility can provide electron beams on the order of 100 mA delivered in tight macropulse bunches, which allows for experiments where the behavior of electronics is monitored as a function of pulse number. While the beam rates per macropulse of this accelerator is monitored during an experiment via a current pick-off connected to a large graphite beamstop, the energy distribution of this electron beam is not measured during the experiment and has not been well characterized. The energy distribution of the beam is pertinent for these types of experiments, since dose is directly related to energy deposited in a medium. Further, these experiments are performed in open air and sample placement in the room can dictate what dose rate they receive per macropulse. We have created simulated dosemaps for the UMD vault room, but these simulations assume a given energy of the beam, both for calculating the dose and to simulate how much the beam diverges in the air. There have been two attempts now to characterize this accelerator beam energy with a plate type spectrometer, including the most recent experiment earlier this year to quantify the beam energy distribution. These results will also be compared to a dosimetry experiment performed by collaborators at the UMD facility, the details of which are described in Reference. Understanding the electron beam energy is important for future experiments, because the energy directly impacts the dose and radiation damage given to a sample and is important for properly simulating the electron beam when comparing simulation to experiment.

43 PARTICLE ACCELERATORS↗

Uncovering the three-dimensional structure of upconverting core–shell nanoparticles with multislice electron ptychography

In photon upconverting core–shell nanoparticles, structure strongly dictates performance. Typical imaging in scanning transmission electron microscopy has sufficient resolution to probe the atomic structure of these nanoparticles, but contrast, dose, and projection limitations make conventional methods insufficient for fully characterizing these structures. Phase retrieval techniques provide a promising alternative imaging mode, and, in particular, multislice electron ptychography can recover depth-dependent information. Here, we study beam-sensitive photon upconverting core–shell nanoparticles with a multislice ptychography approach using a low electron dose to avoid damage. Large strain fields arise in these heterostructures due to the mismatch in lattice parameter between the core and the shell. We reconstruct both a nanoparticle that appears defect-free and one that has a large break in the side and map the distribution of strain in 3D by computing distortion fields from high-resolution potential images of each slice. In the defect-free nanoparticle, we observe twisting of the shell, while in the broken nanoparticle, we measure the 3D position of the crack, the core, and dislocations. These results highlight the advantage of multislice electron ptychography to recover 3D information from a single scan, even under strict electron dose requirements from beam-sensitive samples.

74 ATOMIC AND MOLECULAR PHYSICS↗

Deciphering decomposition pathways of high explosives with cryogenic X-ray Raman spectroscopy

We employed cryogenic X-ray Raman spectroscopy to investigate the early-stage decomposition of the high explosive molecule hexanitrohexaazaisowurtzitane (CL-20). By systematically varying the radiation dose under cryogenic conditions, we induced the decomposition of the molecule using ionizing radiation and observed the evolution of spectral features at the carbon, nitrogen, and oxygen K edges. Through extensive first-principles calculations, we identified key intermediates in the early stages of the decomposition process, resulting from C–C and C–N bond cleavage which leads to the opening of the internal cage structure. A detailed analysis of spectral trends and fingerprints provided evidence supporting N–NO 2 homolytic cleavage as the primary initial decomposition pathway. The combination of advanced core-level spectroscopy methods and state-of-the-art theoretical calculations enabled a comprehensive characterization of the molecular changes induced by controlled radiation dose exposures. In conclusion, our findings establish a benchmark for understanding the decomposition chemistry of high-explosive materials, offering important insights into their stability and reactivity under extreme conditions.

X-ray Raman spectroscopy↗

Microstructure Experiments-Enabled MARMOT Simulations of SiC/SiC-based Accident Tolerant Nuclear Fuel System

We have undertaken an experimental-computational project that addresses a few key technology gaps associated with the use of SiC/SiC composites for light water reactor fuel cladding. Two principal endeavors in this project are to assess the irradiation-induced microstructural changes and swelling in SiC/SiC composites, and to characterize and model the porous oxide surface layer (when exposed to steam) along SiC recession that is detrimental to the clad integrity under accident conditions. The project tasks are: (i) ion irradiation and characterization (University of Tennessee, Knoxville), (ii) mechanical tests and analysis (University of South Carolina), (iii) steam exposure tests (Oak Ridge National Laboratory), (iv) electron microscopy and spectroscopic characterization (NC State University), (v) x-ray microscopy and reconstruction (University of South Carolina and NC State University), (vi) phase field modeling and simulations (NC State University and Idaho National Laboratory). The effects of 10 MeV Au ion irradiation at 350°C on the microstructure evolution in SiC/SiC composites are investigated at doses up to 400 displacements per atom (dpa) at the University of Tennessee, Knoxville. Atomic force microscopy and optical profilometry reveal irradiation induced axial and radial shrinkage of the fibers for doses greater than 10 dpa. Based on detailed electron microscopy characterization, the primary cause of the fiber shrinkage is attributed to irradiation-induced loss of carbon packets. Additionally, the multilayer PyC interface is observed to portray high resistance to irradiation damage. The mechanical response and failure mechanisms of un-irradiated samples is also assessed through loading tests and X-ray imaging at the University of South Carolina. Steam exposure tests are performed at the Oak Ridge National Laboratory in a facility that represents a reactor pressure vessel under a loss-of-coolant-accident scenario. The samples that are analyzed methodically in this report are tested for 32/31 hours at 1200°C with a velocity of 0.25 cm/s for the pressures: 0.1 MPa, 0.45 MPa, 0.92 MPa and 1.38 MPa. Scanning/transmission electron microscopy analysis conducted at the NC State University (NCSU) shows that the oxide layer thickness increases with the steam pressure. While the oxide layer is crystalline (α- cristobalite) for the pressures 0.45 MPa, 0.92 MPa and 1.38 MPa, the layer is amorphous at 0.1 MPa. Results from Raman spectroscopy have also confirmed the formation of α-cristobalite phase of SiO₂. The abrupt increase in the integrated Raman intensity ratio between steam pressures 0.1 and 0.45 MPa suggests the onset of accelerated crystallization. Non-destructive three dimensional X-ray microscopy/tomography (XCT) and computational image processing techniques are employed by the University of South Carolina to probe the porous oxidation features on SiC samples at varying pressures. Interestingly, most pores are observed to be located away from the surface as well as the oxide-SiC interface. The average oxide layer thickness assessed from the XCT analysis is seen to be in excellent agreement with the values determined through scanning electron microscopy analysis for the highest pressures where the oxide layer is relatively more uniform. A phase-field model developed by the NC State University and Idaho National Laboratory for simulating oxidation of SiC by steam captures the paralinear kinetics of SiC oxidation with a high degree of fidelity. Results from quasi-one-dimensional and two dimensional simulations show that the pores with oxidizing species lead to a higher volatilization rate. These simulations indicate that the enhanced apparent volatilization rates at higher pressures observed in experiments can be rationalized by the increased volatilization from the pores. The project team has also successfully developed the capability to import images from experiments for realistic evolution of the oxidizing microstructure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Lithium indium diselenide — An advanced material for neutron detection

Here, this paper describes the synthesis, crystal growth, detector fabrication, radiation hardening studies, MCNP modeling, and characterization of lithium indium diselenide or LiInSe 2 . This newly-developed room temperature thermal neutron detector has semiconducting and scintillating properties and it is suitable for neutron detection application. LiInSe 2 was synthesized starting from elemental Li, In, Se in two steps due to high reactivity of Li. A single crystal of LiInSe 2 was grown using the Vertical Bridgman method. The room temperature band gap was found to be 2.8 eV using optical absorption measurements. Bulk resistivity was measured at ∼5 × 10 11 Ωcm. Photoconductivity measurements of LiInSe 2 wafers identified a peak in the photocurrent around 445 nm. Nuclear radiation detectors were fabricated from single crystal wafer and the responses to alpha particles at various biases were measured. The mobility-lifetime product was estimated. Gamma irradiation studies were performed with calculated absorbed doses ranging from 0.2126 to 21,262 Gy. The characterization of the two wafers for their scintillator performance was conducted after each irradiation. The gamma irradiation produced a reduction of the light yield that translated to a lower channel number for the centroid of alpha detection spectra. It also showed a considerable reduction of the decay time after the first irradiation. These are the first studies on gamma radiation hardening with this material.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Demonstration of the On-the-Fly Shielding Analysis Method: Spent Fuel and Waste Disposition

This report documents work performed supporting the US Department of Energy (DOE) Office of Nuclear Energy (NE) Spent Fuel and Waste Disposition (SFWD) Integrated Waste Management activities under work breakdown structure element 1.08.02.04.01, “Data and Tools Development, Validation, and Maintenance.” In particular, this report fulfills milestone M3SF-21OR020401016, “Implement on-the-fly dose analysis methodology in UNF-ST&DARDS” within work package SF-21OR02040101, “Commercial SNF Characterization - ORNL.” The Used Nuclear Fuel - Storage, Transportation & Disposal Analysis Resource and Data System (UNFST& DARDS) enables automated dose rate calculations for spent nuclear fuel (SNF) transportation packages and storage casks using a Monte Carlo radiation transport code. The explicit method uses a detailed model of the SNF system and its contents. Therefore, a dose rate calculation is required for each as-loaded transportation package or storage cask because the SNF assemblies within a canister typically have unique irradiation characteristics. An alternate method, referred to as the “on-the-fly” shielding analysis method, has been proposed that requires only a set of Monte Carlo dose rate calculations for each transportation packaging/storage cask design. The results of the Monte Carlo dose rate calculations are independent of the SNF assembly irradiation and decay characteristics. The dose rate values may then be combined with the radiation source strength of the SNF assemblies associated with a particular transportation packaging/storage cask design to determine actual dose rates. This report presents on-the-fly dose rate calculations for a representative SNF storage cask and verification of the on-the-fly dose rate calculation results by comparison with reference dose rate calculations using the explicit Monte Carlo dose rate calculation. The on-the-fly shielding analysis method was implemented in UNF-ST&DARDS. A Python program was developed to process the MAVRIC dose rate results obtained by source particle type, energy group, and fuel geometry region. A Python processor created binary files, which were saved as a special UNF-ST&DARDS library for on-the- fly shielding analyses. UNF-ST&DARDS uses the precalculated on-the-fly binary libraries generated by the Python data processor and directly executes the Python code for on-the-fly dose analysis. This Python code unzips the pre-generated binary files mentioned above, reads the data, and combines them with user-specified sources for dose and uncertainty calculations. The Python programs were verified using Excel calculations and by comparison with the values obtained with the MAVRIC post-processing utilities applied to the 3dmap files. This method can currently be used to determine dose rates for as-loaded HI-STORM FW storage casks. The UNF-ST&DARDS analysis wizard for on-the-fly shielding analysis is described in this report.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Calculations versus measurements for residual dose rates from SNS spent structures

Here, residual dose rate measurements were conducted on target vessel #13 and proton beam window #5 after extraction from their service locations. These measurements are used to verify calculation methods of radionuclide inventory assessment that are typically performed for nuclear waste characterization and transportation of these structures. Neutronics analyses for predicting residual dose rates are carried out using the transport code MCNPX and the transmutation code CINDER90. For transport analyses a complex and rigorous geometry model of the structures and their surroundings are applied. The neutronics analyses are carried out using the Bertini and CEM high energy physics models for simulating particles interactions above the table-based cross section range. Finally, obtained calculational results are analyzed and compared to the measured dose rates and overall show good agreement within 25%, which shows applicability of the methods used in analyses.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Cavity Swelling in Irradiated Materials

Cavity swelling, due to three-dimensional clustering of vacancies, is an undesirable isotropic volume expansion of materials under irradiation. This phenomenon occurs above stage-III recovery temperature where vacancies are mobile, between ~0.3–0.6 Tm where Tm is the absolute melting temperature. The primary mechanism for cavity swelling is “dislocation bias”, i.e., preferential absorption of interstitials by network dislocations, causing a vacancy supersaturation. Cavity swelling is highly temperature dependent and typically follows a bell-shaped curve with peak swelling occurring at an intermediate temperature. With increasing temperature, cavity size increases, and number density decreases logarithmically. With increasing dose, cavity swelling increases, but follows a hockey-stick type pattern, characterized by a low-swelling transient incubation period and then a steady-state regime. The incubation period, dominant in cavity nucleation, is dependent upon material’s chemistry and irradiation conditions such as dose rate/temperature. Cavity swelling increases linearly with dose in the steady-state regime, that is independent of chemistry and dose rate. This regime is dominated by cavity growth. Transmutation gases like He enhance cavity nucleation such that an early onset of cavity formation occurs. However, swelling magnitudes can be either increased or suppressed when He is present. Results in austenitic steels and Cu indicate that cavity swelling peaks at intermediate He/dpa ratios of ~10 appm He/dpa. The most effective method to mitigate cavity swelling is by increasing the fixed point-defect sink density, by promoting precipitation or dispersion strengthening.

Bhattacharya, Arunodaya↗

Small, solubilized platinum nanocrystals consist of an ordered core surrounded by mobile surface atoms

In situ structures of Platinum (Pt) nanoparticles (NPs) can be determined with graphene liquid cell transmission electron microscopy. Atomic-scale three-dimensional structural information about their physiochemical properties in solution is critical for understanding their chemical function. We here analyze eight atomic-resolution maps of small (<3 nm) colloidal Pt NPs. Their structures are composed of an ordered crystalline core surrounded by surface atoms with comparatively high mobility. 3D reconstructions calculated from cumulative doses of 8500 and 17,000 electrons/pixel, respectively, are characterized in terms of loss of atomic densities and atomic displacements. Less than 5% of the total number of atoms are lost due to dissolution or knock-on damage in five of the structures analyzed, whereas 10–16% are lost in the remaining three. Less than 5% of the atomic positions are displaced due to the increased electron irradiation in all structures. The surface dynamics will play a critical role in the diverse catalytic function of Pt NPs and must be considered in efforts to model Pt NP function computationally.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effects of dose rate on the microstructure and deuterium retention in γ-LiAlO 2 pellets

This report presents experimental findings obtained from November 2024 to September 2025. Defect accumulation and microstructural evolution during ion irradiation at elevated temperatures are governed by two competing processes: defect production, driven by dose rate, and defect recovery, controlled by defect diffusion, interaction, and annihilation. At a given dose, the resulting microstructural evolution depends on both the dose rate and irradiation temperature. As a continuation of our FY24 tritium science project, which investigated temperature effects at a fixed dose rate, this study focuses on dose-rate effects at a fixed temperature to provide deeper insights into the irradiated microstructure and compositional changes in γ-LiAlO 2 pellets. The study aims to elucidate the impact of dose rate on microstructure, precipitate morphology, deuterium retention, and lithium volatility in γ-LiAlO 2 pellets under sequential 120 keV He + and 80 keV D 2 + ion irradiation. Three dose rates of 7.3×10 4 , 2.9×10 4 and 6.8×10 5 dpa/s were applied to achieve the same total ion fluence of 2×10 17 (He + +D + )/cm 2 at 500 °C, corresponding to a maximum combined dose of 7.55 dpa at ~255 nm. The irradiated pellets were subsequently characterized using scanning transmission electron microscopy (STEM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The microstructural response of γ-LiAlO 2 to ion irradiation was found to be strongly dose-rate dependent. At medium and high dose rates, irradiation produced a surface amorphized layer and an underlying crystalline layer containing LiAl 5 O 8 precipitates, with implanted gases accumulating and forming blisters at the crystalline-amorphous interface. It remains to be investigated whether the amorphized layer was produced by He + ion irradiation prior to D 2 + ion irradiation. In contrast, at low dose rates, the material remained crystalline, with cavities, likely gas-filled, distributed around precipitates, within the γ-LiAlO 2 matrix, and along grain boundaries. While precipitate morphology exhibited anisotropy, their size showed little sensitivity to dose rate in the applied range of this study. This result, however, does not rule out the possibility that further reductions in dose rate could influence precipitate size. High dose-rate irradiation enhanced protonium–deuterium isotopic exchange and lithium depletion in the amorphized region. Collectively, the results show that dose rate governs amorphization, gas redistribution, isotopic exchange, and lithium depletion, providing important insights into the mechanisms underlying structural evolution in γ-LiAlO 2 pellets under reactor-relevant irradiation conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

IER-484 CED4a Report: AFRRI ER1 Dosimetry Characterization

This report presents an analytical function as the reference neutron and photon dose (normalized to an ion chamber integral) for future nuclear accident dosimeter (NAD) exercise at the Armed Forces Radiobiology Research Institute (AFRRI). Various dosimeters and equipment were positioned within exposure room 1 (ER1) and irradiated using a 1.1 MW Training, Research, Isotope, General Atomics (TRIGA) Mark-F nuclear reactor. An ion chamber located in ER1 was used as a normalization factor in Equation 2. This allows for a quick calculation of neutron and photon dose based on the ion chamber data. Currently, AFRRI is in preparation to host a NAD exercise this summer.

61 RADIATION PROTECTION AND DOSIMETRY↗