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Presentation highlight the INL Center for Radiation Chemistry Research's contributions the Material Recovery & Waste Form Development Campaign on sulfur chloride processing technologies.
Reported herein are results from the Eril Research, Inc. (ERI) participation in the JSC-sponsored study characterizing the radiation shielding properties of the two types of space suit that astronauts are wearing during the EVA on-orbit assembly of ISS. Measurements using passive detectors were carried out to assess the shielding properties of the U.S. EMU Suit and the Russian Orlan-M suit during irradiations of the suits and a tissue-equivalent phantom to monoenergetic proton and electron beams at LLUMC. During irradiations of 6 MeV electrons and 60 MeV protons, absorbed dose as a function of depth was measured using TLDs exposed behind swatches of the two suit materials and inside the two EVA helmets. Considerable reduction in electron dose was measured behind all suit materials in exposures to 6 MeV electrons. Slowing of the proton beam in the suit materials led to an increase in dose measured in exposures to 60 MeV protons. During 232 MeV proton irradiations, measurements were made with TLDs and CR-39 PNTDs at five organ locations inside a tissue-equivalent phantom, exposed both with and without the two EVA suits. The EVA helmets produce a 13% to 27% reduction in total dose and a 0% to 25% reduction in dose equivalent when compared to measurements made in the phantom head alone. Differences in dose and dose equivalent between the suit and non-suit irradiations for the lower portions of the two EVA suits tended to be smaller. Proton-induced target fragmentation was found to be a significant source of increased dose equivalent, especially within the two EVA helmets, and average quality factor inside the EMU and Orlan-M helmets was 2% to 14% greater than that measured in the bare phantom head.
We present a study directly measuring the electron-beam-induced plasticity of amorphous Al 2 O 3 coatings. Core–shell nanostructures are employed as small-scale model systems for two-dimensional coatings made by atomic layer deposition (ALD). Copper nanowires (NWs) are used as substrates for ALD deposition, representing a model system for interconnects commonly found in integrated circuits. Experiments are performed in situ in a transmission electron microscope (TEM) and further analyzed with electron energy loss spectroscopy (EELS). Our in situ TEM tensile experiments reveal the highly plastic behavior of the ALD shell, which withstands a maximum strain of 188%. Comparable samples under beam-off conditions show a brittle fracture, which underlines the effect of electron irradiation. The electron-beam-activated bond switching within the amorphous network enables compensation of the applied tensile strain, leading to viscous flow. By incorporating an intermediate nanocrystalline layer within the Al 2 O 3 shell, the plasticity is suppressed and brittle fracture occurs. This work directly demonstrates the tuning of mechanical properties in amorphous ALD structures through electron irradiation.
Niowave Inc. produces medical radioisotopes within the US. Lead-bismuth eutectic (LBE) is irradiated using an electron beam to produce neutrons that are used in the production of Molybdenum-99 (Mo-99). The medical community relies on a steady supply of Mo-99 which is primarily used in medical diagnostic imaging. The irradiation of LBE results in high temperatures within the molten metal, this work focusses on the design of ancillary systems associated with the liquid metal system. The LBE is initially at a temperature of 200°C and flows over a steel plate to create a waterfall. The electron beam is then aimed at the waterfall to generate neutrons. The peak temperatures of the LBE post irradiation depend on the beam energy of the LINAC. For a 15 MeV and 20 kW beam, the temperatures can range between 300°C and 350°C. The LBE is cycled through the system to create a closed loop that requires the post-irradiation LBE to be cooled back to 200°C. This work focuses on the heat exchanger and condenser system responsible for the cooling of the post-irradiation LBE.
Two neutral Mg spectral lines formed in the temperature-minimum region and the low chromosphere, at 4571 and 5173 A, are used to quantify the changes in the atmospheric structure as a function of time during five solar flares. Eight proposed flare heating and ionization mechanisms and predictions of the effects of each on the temperature minimum region are discussed. Two Mg spectral observations made at the National Solar Observatory (Sacramento Peak), along with observations of hard and soft X-rays from the SMM and GOES satellites, are compared to the predictions of the eight proposed mechanisms. The initial effects in all five flares are consistent with backwarming by enhanced Balmer- and Paschen-continuum radiation originating in the upper chromosphere. Extended heating observed in two of the flares is most likely due to UV irradiation. In all cases heating by the dissipation of nonreversed electric currents, collisions with an electron or proton beam, irradiation by soft X-rays, and dissipation of Alfven waves are eliminated.
Austenitic 21Cr32Ni model alloy thin foils, previously irradiated with 5 MeV Fe ++ ions in bulk to create voids, were re-irradiated in-situ in the Intermediate Voltage Electron Microscope Facility (IVEM). The voids which had been formed under bulk-ion irradiation shrank and disappeared after in-situ Kr ion irradiation in the temperature range 50 K-713 K to an additional dose of 1 dpa. The voids were unaffected by eithersuccessive thermal annealing to 673 K and by prolonged exposure to the 200 keV electron beam at the irradiation temperature. The high void shrinkage rate observed did not change significantly for irradiation temperatures between 50 K and 713 K, suggesting that the void shrinkage process in thin foils during in-situ heavy-ion irradiation results from the interactions of displacement cascades with the voids. Finally, possible void shrinkage mechanisms under thin foil irradiation are discussed in this study.
The Universal Neutron Irradiator (UNI) was designed to irradiate a small volume of uranium solution and to achieve high fission power without creating a large radionuclide (RN) inventory. The UNI system is equipped with a fully enclosed off-gas system with online hydrogen gas monitoring to prevent the production of an explosive atmosphere, as well as storage cylinders for capturing fission gases. It also includes a catalytic recombiner in the target capsule (to immediately recombine radiolytic hydrogen and oxygen gas in the system) and access ports for sampling the target solution and capsule headspace. In UNI Phase I experiments, 50 mL of uranyl sulfate solution was irradiated at 0.3–0.5 W/mL fission power using a tantalum target assembly to produce photoneutrons via irradiation with an electron beam. The purposes of the Phase I experiments were to test the efficacy of adding 200 ppm Fe 2+ to the target solution to prevent uranyl peroxide precipitation under representative irradiation conditions, and to monitor iodine speciation in the irradiated uranyl sulfate solution. The focus of the UNI Phase II experiments was to use an irradiated uranyl sulfate solution containing a mixture of fission products and monitor their distribution in various streams during the primary recovery column (titania-based column) that separates Mo-99 from uranium. Irradiations were designed to create sufficient activity for tracking their distribution in various processing streams using a combination of gamma counting and inductively coupled plasma mass spectrometry (ICP-MS) analyses. Obtained data will be used to better understand the composition of waste streams, accumulation of RN on the titania column, and identify what RNs accumulate in the uranyl sulfate solution. Furthermore, this knowledge will allow us to determine waste classifications for various streams produced during the Mo-99 purification process and develop an appropriate waste clean-up strategy.
Here, a study of 316L type stainless steel in its base metal and electron-beam (e-beam) welded conditions was performed to observe the effects of low-temperature (60 °C to 100 °C) neutron irradiation on the tensile behavior of the samples. Fractography was used in understanding the tensile-tested fracture surfaces of the 316L samples in these different forms with the characterization of the both base metal and welded samples using electron microscopy. Irradiation of the tensile specimens made free of defects of cutting and mechanical polishing showed a reduction in their tensile ductility with increased radiation-induced hardening up to 1.40 × 10 19 n/cm 2 (E > 0.1 MeV) fluence that corresponds to 1.1x 10 -2 dpa, even at the low irradiation temperatures. These low-temperature neutron irradiated base metal and e-beam welded 316L specimens also consisted of closely similar fracture surfaces characteristic of ductile rupture.
On demand switchable additive/subtractive patterning of 2D nanomaterials is an essential capability for developing new concepts of functional nanomaterials and their device realizations. Traditionally, this is performed via a multi-step process using photoresist coating and patterning by conventional photo or electron beam lithography, which is followed by bulk dry/wet etch or deposition. This limits the range of functionalities and structural topologies that can be achieved, as well as increases the complexity, cost, and possibility of contamination which are significant barriers to device fabrication from highly sensitive 2D materials. Focused electron beam induced processing (FEBIP) enables a material chemistry/site-specific, high-resolution multi-mode atomic scale processing and provides unprecedented opportunities for direct-write, single-step surface patterning of 2D nanomaterials with an in-situ imaging capability. It allows for realizing a rapid multi-scale/multi-mode approach, ranging from an atomic scale manipulation (e.g., via targeted defect introduction as an active site) to a large-area surface modification on nano and micro scales, including patterned doping and material removal/deposition with 2D (in-plane)/3D (out-of-plane) control. In this work, we report on a new capability of FEBIP for nanoscale patterning of graphene oxide via removal of oxygenated carbon moieties with no use of reactive gas required for etching complemented by carbon atom deposition using focused electron beam. The mechanism of experimentally observed phenomena is explored using the density functional theory (DFT) calculations, revealing that interactions of e-beam liberated reactive oxygen radicals with carbon atoms on graphene basal plane lead to creation of atomic vacancies in the material. The reaction by-products are volatile carbon di-oxides, which are dissociated and volatilized from the graphene oxide surface functional groups by interactions with an energetic focused electron beam. Along with selective “subtractive” patterning of graphene oxide, the same electron beam with increased irradiation doses can deposit out-of-plane 3D carbon nanostructures on top of or around the 2D etched pattern, thus forming a hybrid 2D/3D nanocomposite with feature control down to a few nanometers. Furthermore, this in-operando dual nanofabrication capability of FEBIP is unmatched by any other nanopatterning techniques and opens a new design window for forming 2D/3D complex nanostructures and functional nanodevices.
Laser damage of optical components can be a limiting factor in scaling the energetics of high-peak and average power laser systems. Specifically for optical coatings, damage under nanosecond pulsed irradiation is initiated by pre-existing defects in the coating layers, including those that cause discontinuities in the structure, like craze lines. Crazing or cracking in a multilayer dielectric optical coating is induced when the overall coating stress is sufficiently tensile, and is an occasionally observed issue when employing more porous deposition techniques like electron-beam evaporation. Here, in this study, electron-beam high-reflectors were fabricated utilizing process parameters that are known to induce crazing based on prior processing history to systematically evaluate the impact of crazing on reflector damage performance for 1064 and 355 nm lasers. The crazing that was observed was apparently nucleated at nodular defects. When the cross-section of these nodules was investigated, it was observed that there were cracks into the fused silica substrate of approximately 5 µm in depth. The craze lines were irradiated with 1064 and 355 nm light at fluences slightly above the onset of damage initiation fluence of the coating. The 1064 nm irradiated sub-apertures exhibit laser damage but with no spatial correlation with the craze line, whereas the 355 nm irradiated area exhibited many damage sites along the craze line. Finite-difference time-domain electric-field simulations were conducted, and ∼2× field amplification in hafnia was observed for the 355 nm wavelength case. The laser damage can be attributed to a slight electric-field intensification coincidental with an area where UV damage-prone precursors are known to occur. The 355 nm laser damage in uncoated fused silica substrates has been previously correlated to initiate through localized UV absorption at the broken silica bonds in the tips of fractures.
This paper presents measurements of the electromagnetic radiation pulses and the replacement current pulses which result from the breakdown of Mylar and Kapton samples. The observed dependence of the characteristics of the replacement current pulse as a function of electron beam energy is discussed. The characteristics of the electromagnetic radiation pulses are also analyzed in the text of this paper. The source of the irradiating electrons is a monoenergetic electron beam whose energy was varied from 12.5 KeV to 25 KeV.
A branched nanostructure is synthesized. A porous material, with pores having a diameter of approximately 1 .mu.m or less, is placed in a vacuum. It is irradiated with an electron beam. This causes a trunk to grow from the porous material and further causes branches to grow from the trunk.
Los Alamos National Laboratory (LANL) is working with NorthStar Medical Radioisotopes (NMR) on their efforts to produce Mo-99 from the irradiation of Mo-100 targets. The NMR target consists of an Inconel window that allows the electron beam to penetrate and irradiate a stack of Mo-100 disks. The irradiation process generates large amounts of heat and is cooled using pressurized helium gas flowing at 400 g/s. LANL provides both numerical analysis support and experimental support. Computational fluid dynamics (CFD) and conjugate heat transfer (CHT) analysis are performed on the NMR target to analyze the helium flow and volumetric heating through the NMR system. In this iteration of numerical analysis, we update the Mo-100 disk thickness to 0.74 mm and the gap between the Inconel window and the first disk to 0.69 mm. Estimates of the heat flux from the electron beams from Monte Carlo N-Particle code (MCNP) analysis were combined with CFD to perform the CHT analysis. The pressure drop through the targets, force applied on the first disk, beam window and target disk temperatures are some of the quantities estimated using the simulations. The pressure drop through the target was estimated as 0.198 MPa, while the force due to venturi effects across the first disk was estimated to be 100 N. The results show maximum window temperatures over 600 °C and peak disk temperatures over 1600 °C. Past work has shown that beyond 650-700 °C, the Inconel window becomes susceptible to yield and rupture. The increased temperature in these results reduces the margin of error possible on beam spot size. The disk temperatures showed a sinusoidal distribution with the 6 th – 8 th disk from each window exhibiting highest disk temperatures. The peak temperature of the stainless steel housing was close to 316 °C and that of the laminations and spacers was approximately 582 °C.
Los Alamos National Laboratory (LANL) is working with NorthStar Medical Radioisotopes (NMR) on their efforts to produce Mo-99 from the irradiation of Mo-100 targets. The NMR target consists of an Inconel window that allows the electron beam to penetrate and irradiate a stack of Mo-100 discs. The irradiation process generates large amounts of heat and is cooled using pressurized helium gas flowing at 400 g/s. LANL provides both numerical analysis support and experimental support. Computational fluid dynamics (CFD) simulations for both 300 g/s and 400 g/s are performed on the NMR target to analyze the helium flow through the NMR system. The pressure drop, the mass flow rate through each of the disc and window channels and the force applied on the first disc are some of the quantities estimated using CFD. These results will be combined with Monte Carlo N-Particle (MCNP) estimates of heat flux into the system from the electron beam to perform conjugate heat transfer analysis (CHT). The experiments presented in this report focus on the effect of the flow induced vibrations from helium flowing through the coolant gaps between the discs. There is concern that the flow induced vibrations may lead to excessive mass loss of the enriched Mo-100 discs, and the goal would be to mitigate the mass loss. This work presents benchtop tests of flow through a subset of the target stack which involves high speed imaging and displacement measurements used to estimate disc vibration, as well as mass loss.
Focused ion beam scanning electron microscopy (FIB-SEM) tomography has increasingly been utilized for acquiring three-dimensional (3D) microstructure features at the sub-micron scale in irradiated nuclear materials. This technique involves sequential ion beam slicing followed by electron beam imaging and compositional mapping using energy dispersive spectroscopy (EDS). Despite its growing use, several challenges persist. These include the time-intensive nature of data collection of EDS data, difficulties in distinguishing between various microstructures, and issues with image alignment. These challenges currently limit the broader application of FIB-SEM tomography in the field. To overcome these limitations, we propose using convolutional neural networks (CNNs) to automate microstructure identification in SEM images. Our study introduces a new framework for identifying microstructures in irradiated U-10Zr (wt. %) metallic fuel with limited annotated data. The framework includes the creation of a reliable annotated dataset with paired SEM and ground truth data from EDS maps, the applications of CNNs for microstructure identification, and the validation of model performance. Specifically, we employed the Segment Anything Model (SAM) to align SEM images with corresponding EDS maps and focused ion beam (FIB) tomography SEM data. We evaluate several models, including Patch-based U-Net, Attention U-Net, and Residual U-Net, finding that patch-based U-Net exhibits superior segmentation performance and consistency. This approach reduces reliance on EDS detectors and aids in accelerating nuclear material analysis process, highlighting the potential of advanced deep learning techniques to improve microstructural understanding in nuclear material. This is the first framework to integrate SAM and Patch-based CNN models for semantic segmentation of irradiated nuclear materials, with potential applicability to other tomography datasets.
Photoneutron cross sections were extracted for isotopes of ruthenium and molybdenum on natural abundance targets via a reduced chi-squared analysis on excitation functions, or activation yields, as function of electron beam energy. Bremsstrahlung photons were produced via an electron linear accelerator and a tungsten radiator at the Idaho Accelerator Center. A total of 16 irradiations were performed with electron beam energies ranging from approximately 8 MeV to 23 MeV. Induced radioactivity was measured using a high purity germanium detector. The cross sections were extracted assuming a three parameter Lorentzian fit with a smooth truncated rise at reaction threshold.
Amorphous boron carbide (a-BxC) networks consist of light elements, and their low atomic scattering factors makes structural analysis by x-ray diffraction difficult. Electron diffraction has an advantage of detecting the light elements, because of the strong interaction between the matter and electrons. In this work, we prepared a-BxC by ion beam technologies and plasma-enhanced chemical vapor deposition, and characterized their structures via atomic pair-distribution functions derived from electron diffraction intensity profiles. It was found that a pentagonal pyramid is the most favorable cluster in a-B4C generated by ion irradiation, while C—C homonuclear bonds were formed in the deposited a-B x C thin film. X-ray photoemission spectroscopy revealed that the a-BxC thin film possesses more carbon than B 4 C, which is responsible for the formation of the homonuclear bonds.
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi 3 + primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.