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DOE OSTI2025

Microstructure, stored energy, and stability of H/He-filled nanocavities in low temperature irradiated Inconel 718

The microstructure, trapped transmutation gases, stored energy, and mechanical behavior of samples from an irradiated Inconel 718 proton beam window were characterized using transmission electron microcopy, thermal desorption spectrometry (TDS), differential scanning calorimetry (DSC), and tensile testing. In the as-irradiated condition the microstructure contained a high number density of 1–3 nm gas-filled nanocavities. Emissions of trapped gases, H and He, during TDS correlated with peaks of the energy release curves from DSC examinations, which suggest these gases were likely stored in highly stable defect traps. The stored energy from radiation damage saturated at doses of a few dpa and did not increase with increasing radiation dose, but the amount of stored H and He increased with increasing dose. Effects of post-irradiation annealing were studied as well. After exposure to 700 °C, the nanocavities grew only slightly to 2–4 nm in diameter, but after exposure to 900 °C, the cavities grew to 10–20 nm in diameter and electron energy-loss spectroscopy showed these cavities contained a core of He surrounded by a shell of H. Further, this study demonstrated that the irradiation defect structures containing H and He were remarkably stable during irradiation and after exposure up to 700 °C. The effect of the irradiation temperature, defect mobility, and interaction of H, He, and irradiation defects on mechanical behavior provides insight into the processes responsible for the unusual recovery in ductility with increasing radiation dose observed in Inconel 718 after high energy proton and spallation neutron irradiation.

36 MATERIALS SCIENCE↗

DOE OSTI2022

From ground to excited electronic state dynamics of electron and ion irradiated graphene nanomaterials

Microscopes utilizing convergent electron and ion beams are emerging as powerful tools for both imaging and manipulating two-dimensional materials with atomic resolution, allowing the ultimate limits of nanofabrication to be realized. In this chapter, we detail the use of time-dependent electronic structure theory to determine the excited state properties and reactivity of functionalized graphene nanostructures. A time-dependent density functional theory treatment of electronic excitations of materials is presented, with specific emphasis on predicting the position-dependent electronic response of two-dimensional nanomaterials to electron beams. The method is demonstrated in a study highlighting the important role that electronic excitation can play in opening reaction pathways relevant to atomically precise defect manipulation in graphene. Finally, we provide some perspective on future development directions for methods of simulating nonequilibrium electronic and vibrational dynamics induced by electron/ion beams.

Lingerfelt, David↗

NASA NTRS2006

Effect of Bending Stiffness of the Electroactive Polymer Element on the Performance of a Hybrid Actuator System (HYBAS)

An electroactive polymer (EAP)-ceramic hybrid actuation system (HYBAS) was developed recently at NASA Langley Research Center. This paper focuses on the effect of the bending stiffness of the EAP component on the performance of a HYBAS, in which the actuation of the EAP element can match the theoretical prediction at various length/thickness ratios for a constant elastic modulus of the EAP component. The effects on the bending stiffness of the elastic modulus and length/thickness ratio of the EAP component were studied. A critical bending stiffness to keep the actuation of the EAP element suitable for a rigid beam theory-based modeling was found for electron irradiated P(VDF-TrFE) copolymer. For example, the agreement of experimental data and theoretical modeling for a HYBAS with the length/thickness ratio of EAP element at 375 times is demonstrated. However, the beam based theoretical modeling becomes invalid (i.e., the profile of the HYBAS movement does not follow the prediction of theoretical modeling) when the bending stiffness is lower than a critical value.

Xu, Tian-Bing↗

DOE OSTI2025

Optical Imaging of Laser-Driven Fast Electron Weibel-like Filamentation in Overcritical Density Plasma

We report on the measurement of filamented transport of laser-generated fast electron beams in near-critical density plasma. A relativistic intensity long-wave-infrared laser irradiated a hydrodynamically shaped helium gas flow at an electron density n e ≃ 10 25 m − 3 , generating a large flux of fast electrons that propagated beyond the critical surface. The beam-to-background electron density ratio was sufficiently high to drive growth of Weibel-like filamentation, which was measured by optical probing to extend up to 800 μ m with radii ∼ 10 μ m . Particle-in-cell simulations reproduce the main features of the filamentation generation, suggesting that collisionless processes are dominant in these interactions. Expansion of the filaments after formation infers a fast electron heated plasma temperature ∼ 400 eV in the overcritical density plasma. Published by the American Physical Society 2025

43 PARTICLE ACCELERATORS↗

NASA NTRS1987

Spacecraft dielectric surface charging property determination

The charging properties of 127 micron thick polyimide, (a commonly used spacecraft dielectric material) was measured under conditions of irradiation by a low-current-density electron beam with energy between 2 and 14 keV. The observed charging characteristics were consistent with predictions of the NASCAP computer model. The use of low electron current density results in a nonlinearity in the sample-potential versus beam-energy characteristic which is attributed to conduction leakage through the sample. Microdischarges were present at relatively low beam energies.

Williamson, W. S.↗

NASA NTRS1987

The production of low-energy neutral oxygen beams by grazing-incidence neutralization

The Vanderbilt University neutral oxygen facility produces beams of low-energy neutral oxygen atoms by means of grazing-incidence collisions between ion beams and metal surfaces. Residual ions are reflected by applied electric fields. This method can utilize initial ion beams of either O(+) or O2(+) since a very large percentage of molecular oxygen ions are dissociated when they undergo grazing-incidence neutralization. The method of neutralization is applicable to low-energy beams and to all ions. Particular emphasis is on O and N2 beams for simulation of the low Earth orbit space environment. Since the beam is a pure O-neutral beam and since measurements of the interaction of the beam with solid surfaces are made spectroscopically, absolute reaction rates can be determined. The technique permits the beams to be used in conjunction with electron and photon irradiation for studies of synergistic effects. Comparisons of optical spectra of Kapton excited by 2.5-keV O, O(+), and O2(+) show significant differences. Optical spectra of Kapton excited by neutral oxygen beams of less than 1 keV have been recorded.

Albridge, R. G.↗

DOE OSTI2023

E-beam-enhanced solid-state mechanical amorphization of α-quartz: Reduced deformation barrier via localized excess electrons as network modifiers

Under hydrostatic pressure, α-quartz (α-SiO 2 ) undergoes solid-state mechanical amorphization wherein the interpenetration of [SiO 4 ] 2- tetrahedra occurs and the material loses crystallinity. This phase transformation requires a high hydrostatic pressure of 14GPa because the repulsive forces resulting from the ionic nature of the Si–O bonds prevent the severe distortion of the atomic configuration. Herein, we experimentally and computationally demonstrate that e-beam irradiation changes the nature of the interatomic bonds in α-quartz and enhances the solid-state mechanical amorphization at nanoscale. Specifically, during in situ uniaxial compression, a larger permanent deformation occurs in α-quartz submicron pillars compressed during e-beam irradiation than in those without e-beam irradiation. Microstructural analysis reveals that the large permanent deformation under e-beam irradiation originates from the enhanced mechanical amorphization of α-quartz and the subsequent viscoplastic deformation of the amorphized region. Further, atomic-scale simulations suggest that the delocalized excess electrons introduced by e-beam irradiation move to highly distorted atomic configurations and alleviate the repulsive force, thus reducing the barrier to the solid-state mechanical amorphization. In conclusion, these findings deepen our understanding of electron–matter interactions and can be extended to new glass forming and processing technologies at nano- and microscale.

36 MATERIALS SCIENCE↗

NASA NTRS1981

Processing of silicon solar cells by ion implantation and laser annealing

Methods to improve the radiation tolerance of silicon cells for spacecraft use are described. The major emphasis of the program was to reduce the process-induced carbon and oxygen impurities in the junction and base regions of the solar cell, and to measure the effect of reduced impurity levels on the radiation tolerance of cells. Substrates of 0.1, 1.0 and 10.0 ohm-cm float-zone material were used as starting material in the process sequence. High-dose, low-energy ion implantation was used to form the junction in n+p structures. Implant annealing was performed by conventional furnace techniques and by pulsed laser and pulsed electron beam annealing. Cells were tested for radiation tolerance at Spire and NASA-LeRC. After irradiation by 1 MeV electrons to a fluence of 10 to the 16th power per sq cm, the cells tested at Spire showed no significant process induced variations in radiation tolerance. However, for cells tested at Lewis to a fluence of 10 to the 15th power per sq cm, ion-implanted cells annealed in vacuum by pulsed electron beam consistently showed the best radiation tolerance for all cell resistivities.

Minnucci, J. A.↗

DOE OSTI2022

Comparative Effects of Radiation Sterilization Modality on Medical PVC Tubing

As the production volume of single-use, polymer-based medical devices increases each year, so does the need for throughput capacity to sterilize the devices. Around 80% of radiation-sterilized devices are processed using gamma-ray radiation from industrial cobalt-60 sources. Supply chain, security, and disposal concerns are prompting manufacturers and contract sterilizers to explore alternatives to irradiation using cobalt-60 gamma-rays, such as electron beam (E-beam) and X-ray radiation. Advantages of these ‘machine’ sources over radioisotope-based sources are that they do not decay, a characteristic that requires cobalt-60 to be replaced over time, they can be turned off when not in use, and they do not represent the same level of concern regarding misuse. One of the barriers to direct transition from gamma-ray sterilization to E-beam or X-ray sterilization is concern over the relatively unknown effects of sterilization dose of these alternative modalities on the performance of medical device polymers. Commercially available medical devices sterilized with gamma-ray irradiation exhibit acceptable device function, acceptable mechanical performance, and acceptable discoloration. To be viable, alternate sterilization methods must not only achieve acceptable sterilization, but the process must also result in a product with functional, mechanical, and visual effects acceptable to customers and the regulator. Flexible polyvinyl chloride (PVC) is a plastic material that is commonly found in single-use medical devices and is known for its sensitivity to radiation processing. For instance, transparent PVC is known to yellow upon irradiation. To encouraging sterilization alternatives to cobalt-60 gamma-ray, we directly compared the effects of gamma-ray, E-beam, and X-ray radiation exposure at similar sterilization-relevant doses on key properties of medical grade PVC tubing.

cobalt-60↗

NASA NTRS1985

Kapton charging characteristics: Effects of material thickness and electron-energy distribution

Charging characteristics of polyimide (Kapton) of varying thicknesses under irradiation by a very-low-curent-density electron beam, with the back surface of the sample grounded are reported. These charging characteristics are in good agreement with a simple analytical model which predicts that in thin samples at low current density, sample surface potential is limited by conduction leakage through the bulk material. The charging of Kapton in a low-current-density electron beam in which the beam energy was modulated to simulate Maxwellian and biMaxwellian distribution functions is measured.

Williamson, W. S.↗

DOE OSTI2022

Exploring Functional Materials by Understanding Beam‐Sample Interactions

Abstract Ultra‐low‐dose electron diffraction is performed with a double metal cyanide catalyst (DMC) to understand how electron irradiation stimulates structural alterations in functional materials. The commonly fading diffraction patterns with dose accumulation depend on the irradiated area and the beam current even when below 50 femto Amperes. Heat generation is observed and modeled by statistical, inelastic scattering events to describe how phonon excitations modulate radiation hardness. Specifically, the characteristic 1/e‐decay of Bragg intensities from DMC is delayed from 6 to 30 eÅ −2 at room temperature, which is comparable to the effect of embedding radiation soft matter in ice. DMC's radiation hardness is enhanced by a latency dose that forms during a phase transformation. This unifying model predicts that a critical dose rate exists for any material that varies between 0.1 and 10 4 eÅ −2 s −1 because of a material dependent competition of heat generation and spread. It shows that Brillouin scattering causes time dependent perturbations in electron irradiated solids that trigger time‐temperature‐transformations on a time scale of nanoseconds to microseconds at room temperature, which is not included in traditional models describing the decay of Bragg intensities by radiolysis.

Kisielowski, Christian↗

DOE OSTI2023

3-D reconstruction and microstructural characterization of neutron-irradiated U-10Zr fuel using FIB-SEM serial sectioning

Herein, focused ion beam-scanning electron microscopy serial sectioning was applied to characterize the three-dimensional (3-D) porosity and phase regions of a neutron-irradiated U-10 wt% Zr fuel. The specimen was removed from an intermediate radial region of a fuel pin irradiated to 5.7 at.% burn-up. Backscattered electron imaging and energy-dispersive spectroscopy were performed on each serial section, allowing for the characterization of microstructural morphology and composition. Porosity size followed a lognormal distribution, ranging from 1.46 × 10 –4 to 25.58 µm 3 with a total porosity volume fraction of 13.02%. Distinctive microstructural regions were identified by composition and porosity: (1) a Zr-rich region with an average composition of 28.4 wt% Zr and a local porosity fraction of 6.88%, and (2) a U-rich region with an average composition of 97.0 wt% U and a local porosity fraction of 14.11%; subdivided into U-rich—high porosity (16.68%) and U-rich—low porosity (8.04%) regions. The detailed 3-D compositional and porosity regions can improve nuclear fuel performance codes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Hierarchical, Self-Assembled Metasurfaces via Exposure-Controlled Reflow of Block Copolymer-Derived Nanopatterns

Here, nanopatterning for the fabrication of optical metasurfaces entails a need for high-resolution approaches like electron beam lithography that cannot be readily scaled beyond prototyping demonstrations. Block copolymer thin film self-assembly offers an attractive alternative for producing periodic nanopatterns across large areas, yet the pattern feature sizes are fixed by the polymer molecular weight and composition. Here, a general strategy is reported that overcomes the limitation of fixed feature size by treating the copolymer thin film as a hierarchical resist, in which the nanoscale pattern motif is defined by self-assembly. Feature sizes can then be tuned by thermal reflow controlled locally by irradiative crosslinking or chemical alteration using lithographic ultraviolet light or electron beam exposure. Using blends of polystyrene-block-poly(methylmethacrylate) (PS-b-PMMA) with PS and PMMA homopolymer, we demonstrate both self-assembled PS grating and hexagonal hole patterns; exposure-controlled reflow is then used to reduce hole diameter by as much as 50% or increase PS grating linewidth by more than 180%. Transferring these nanopatterns, or their inverse obtained by a lift-off approach, into silicon yields structural colors that may be prescriptively controlled based on nanoscale feature size. Furthermore, patterned exposure enables area-selective feature size control, yielding uniform structural color patterns across centimeter square areas. Electron beam lithography is also used to show that the lithographic resolution of this selective-area control can be extended to the nanoscale dimensions of the self-assembled features. The exposure-controlled reflow approach demonstrated here takes a pivotal step towards fabricating complex, hierarchical optical metasurfaces using scalable self-assembly methods.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2024

Application of Weak-Beam Dark-Field STEM for Dislocation Loop Analysis

Nanoscale dislocation loops formed by irradiation can significantly contribute to both irradiation hardening and embrittlement of materials when subjected to extreme nuclear reactor environments. Here, this study explores the application of weak-beam dark-field (WBDF) scanning transmission electron microscopy (STEM) methods for quantitative irradiation-induced defect analysis in crystalline materials, with a specific focus on dislocation loop imaging and analysis. A high-purity Fe-5 wt% Cr model alloy was irradiated with 8 MeV Fe 2+ ions at 450°C to a fluence of 8.8 × 10 19 m -2 , inducing dislocation loops for analysis. While transmission electron microscopy (TEM) has traditionally been the primary tool for dislocation imaging, recent advancements in STEM technology have reignited interest in using STEM for defect imaging. This study introduces and compares three WBDF STEM methods, demonstrating their effectiveness in suppressing background contrasts, isolating defect information for dislocation loop type classification, providing finer dislocation line images for small loop analysis, and presenting inside–outside contrast for identifying loop nature. Experimental findings indicate that WBDF STEM methods surpass traditional TEM approaches, yielding clearer and more detailed images of dislocation loops. The study concludes by discussing the potential applications of WBDF STEM techniques in defect analysis, emphasizing their adaptability across various material systems beyond nuclear materials.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Design of target irradiation and diagnostic chamber to study ps-laser generated plasma as a source of singly charged ions for external injection into an electron beam ion source

High repetition-rate (~10 kHz) ps-lasers are becoming available on the market with reasonable cost and may offer several advantages compared to ns-lasers by generating nearly continuous beams of singly charged ions appropriate for the “slow” injection mode into the Electron Beam Ion Source (EBIS). To evaluate these advantages, we will perform studies of a ps-laser generated plasma using a laser with a pulse duration of 8 ps and energy up to 5 mJ per pulse. A vacuum chamber equipped with a 3D target positioner, a focusing lens, and a Faraday Cup has been designed and built for this study. Lens-to-target distance variations have been measured using a laser tracker over the whole range of horizontal and vertical translation for all five targets we will use. The variations were found to be within ±150 µm. This level of “target flatness” should be acceptable for our experimental conditions. Ion currents and ion pulse durations of various elements (from Al to Ta) will be measured for different target irradiation conditions (focal spot size and laser pulse energy). The results obtained will allow us to specify all parameters and geometry of a laser ion source based on a ps-laser to provide external ion injection into the relativistic heavy ion collider EBIS

43 PARTICLE ACCELERATORS↗

DOE OSTI2023

Comparison of unirradiated and irradiated AGR-2 TRISO fuel particle oxidation response

The silicon carbide (SiC) coating in a tristructural isotropic (TRISO) particle acts as a barrier to fission product release during reactor operation and accident scenarios. Oxidation and subsequent failure of the SiC layer during a rare air ingress event is a proposed mechanism for fission product release in a high-temperature gas-cooled reactor (HTGR). Although previous oxidation studies have analyzed unirradiated TRISO particle response, this study compared the oxidation behavior of irradiated and unirradiated TRISO particles from the second Advanced Gas Reactor Fuel Development and Qualification Program irradiation experiment (AGR-2). Particles with exposed SiC were subjected to six varying oxidizing tests in the Furnace for Irradiated TRISO Testing (FITT), examined for failure fraction with the Irradiated Microsphere Gamma Analyzer (IMGA) and characterized with focused ion beam and scanning/transmission electron microscopy techniques to analyze the oxide layer. Uncorrelated unirradiated particle failures throughout the series of exposures suggests that external factors inherent to the experiment increased particle failure sensitivity. However, irradiated particle observations indicated an increased failure response at 400 h 1400 °C in both 2% and 21% O 2 atmospheres above failure associated with external factors. Oxide thickness measurements after 400 h at 1400 °C revealed a greater oxidation rate than predicted by parabolic growth, which was attributed to the increased complexity of the oxide structure at longer exposure times. Altering the atmosphere from 21% to 2% O 2 reduced the average oxide thickness by approximately 12%–14% in both irradiated and unirradiated particles at 400 h 1400 °C. Altogether, the minor variations observed between irradiated and unirradiated particles in this study led to the conclusion that unirradiated TRISO particles can be used to approximate irradiated TRISO oxidation kinetics.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Quantitative Electron Beam‐Single Atom Interactions Enabled by Sub‐20‐pm Precision Targeting

The ability to probe and control matter at the picometer scale is essential for advancing quantum and energy technologies. Scanning transmission electron microscopy offers powerful capabilities for materials analysis and modification, but sample damage, drift, and scan distortions hinder single atom analysis and deterministic manipulation. Materials analysis and modification via electron–solid interactions can be transformed by precise delivery of electrons to a specified atomic location, maintaining the beam position despite drift, and minimizing collateral dose. Here a fast, low-dose, sub-20-pm precision electron beam positioning technique is developed, “atomic lock-on,” (ALO), which offers the ability to position the beam on a specific atomic column without previously irradiating that column. This technique is used to lock onto a single selected atomic location to repeatedly measure its weak electron energy loss signal despite sample drift. Moreover, electron beam-matter interactions in single atomic events are measured with μ s time resolution. This enables observation of single-atom dynamics, such as atomic bistability, revealing partially bonded atomic configurations and recapture phenomena. This opens prospects for using electron microscopy for high-precision measurements and deterministic control of matter for quantum technologies.

2D materials↗

DOE OSTI2022

AGR-2 irradiated TRISO particle IPyC/SiC interface analysis using FIB-SEM tomography

In this work, the morphology in the interface region between the inner pyrolytic carbon layer (IPyC) and silicon carbide (SiC) layers in tristructural-isotropic (TRISO) particle fuel from the AGR-2 irradiation experiment were studied using focused ion beam-scanning electron microscopy tomography. This work quantitatively described the interface and corresponding relevant metrics to understand how the microstructural features at the IPyC/SiC interface may influence actinide and fission product interactions with the SiC layer. Particles were selected with varied 110m Ag retention rates, and their volumes were reconstructed and analyzed for distributions of pores, fission product/actinide features, SiC, and IPyC. It was found that porosity accommodates fission products in the interface and SiC layers. The largest fission product/actinide precipitates were found in the interface region. This was also where the largest number fraction of fission products/actinides was found, consistent with SEM showing fission product/actinide pileup along selected areas of the interface region.

36 MATERIALS SCIENCE↗