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At least 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Postirradiation Examination of WIRE-21 Experiment Irradiated in the High Flux Isotope Reactor

Westinghouse Electric Company is developing wireless sensors to monitor the centerline temperature and internal pressure of commercial light-water reactor fuel rods during irradiation. Oak Ridge National Laboratory and Westinghouse Electric Company developed the Wireless Instrumented RB Experiment 2021 (WIRE-21) to test wireless temperature and pressure sensor technologies in a removable beryllium position in the High Flux Isotope Reactor. The experiment was irradiated for a total of 75 days, at temperatures ranging from approximately 150°C to 400°C, resulting in a peak fast (energy > 0.1 MeV) neutron fluence of about 3 × 10 21 n/cm 2 . The temperature was intentionally cycled multiple times to compare the response of the wireless temperature sensor to collocated thermocouples. Similarly, the pressure sensor was actuated in multiple steps to compare the response of the wireless measurement to excore pressure transducers (Petrie et al., 2023). After irradiation, the experiment was disassembled in the Irradiated Fuels Examination Laboratory (IFEL) hot cell at Oak Ridge National Laboratory with the intent to recover sensor and dosimetry components, document the as-irradiated condition of the hardware, and investigate possible causes of the sensor behavior observed during irradiation. The postirradiation examination successfully recovered and preserved key WIRE-21 components. After the housing was removed using a milling machine, the internal experiment sections were examined. All eight fiber-optic sensors were recovered, cut, and stored. The silicon carbide thermometry, temperature sensor, pressure sensor, lower spacer, and selected pressure and temperature cable sections were also removed and stored. The metal bellows of the pressure sensor was found to be plastically deformed, indicating that it had been properly pressurized during irradiation and generally behaved as expected. X-ray diffraction analysis of a section of one of the irradiated inductor cores within the pressure sensor was performed and confirmed the presence of phase-pure alpha ferrite (i.e., no unexpected phase transformations). Inductance testing was performed on the irradiated pressure sensor cores using an unirradiated test coil, and DC resistance measurements of the transceiver coils were also performed. The measurements with irradiated inductor cores assembled inside unirradiated coils showed slightly reduced inductance compared to measurements made with unirradiated cores, but the difference was not sufficient to explain the more significant reductions in inductance that were observed in-pile. Therefore, it is suspected that degradation of the inductor coils (specifically the wire wrapping) is responsible for the reduced inductance observed in-pile.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Resolving local structural motifs across the phase evolution of zinc titanates with computational x-ray absorption spectroscopy

Resolving the local structure motifs that characterize phase evolution as a function of composition is a key challenge in structure characterization of complex materials. Here, in this study, we combine first-principles simulations and x-ray absorption near-edge structures (XANES) analysis to gain insights into the structure evolution revealed by measurements across a combinatorial zinc titanate thin film, which was grown with smoothly varying composition over a wide range of the Ti:Zn ratio. Specifically, we propose a cluster blind-signal-separation (cBSS) method for XANES spectral analysis based on a library of the structures and spectra of representative local motifs. In addition to motifs from zinc titanate crystals, two types of Ti-defect models constructed in this study are key to the understanding of the structure characteristics in the Zn-rich region. The cBSS method makes use of both spectral clustering of the simulated site-XANES spectra library and the BSS procedure to construct high-fidelity spectral basis functions from an experimental spectral sequence. The method provides a rigorous measure of the spectral sensitivity and basis completeness. The results of the XANES analysis are corroborated with other experimental modalities, including x-ray diffraction and spectroscopic ellipsometry, to validate the cBSS method. The calculated motif weights resulting from fitting the XANES spectra with the cBSS basis probe the atomic structure characteristics of both crystalline and amorphous phases as a function of the Ti/Zn composition. The insights of the local structure motif evolution are pivotal to the understanding of the nonmonotonic trend in the optical gap, which may lead to potential applications through tuning the optical properties of zinc titanate. The workflow of the XANES spectral analysis developed in this work can be generalized to construct the structure-property relationship in a broad material space.

36 MATERIALS SCIENCE↗
DOE OSTI2022

X-ray free-electron laser based dark-field X-ray microscopy: a simulation-based study

Dark-field X-ray microscopy (DFXM) is a nondestructive full-field imaging technique providing three-dimensional mapping of microstructure and local strain fields in deeply embedded crystalline elements. This is achieved by placing an objective lens in the diffracted beam, giving a magnified projection image. So far, the method has been applied with a time resolution of milliseconds to hours. In this work, the feasibility of DFXM at the picosecond time scale using an X-ray free-electron laser source and a pump–probe scheme is considered. Thermomechanical strain-wave simulations are combined with geometrical optics and wavefront propagation optics to simulate DFXM images of phonon dynamics in a diamond single crystal. Using the specifications of the XCS instrument at the Linac Coherent Light Source as an example results in simulated DFXM images clearly showing the propagation of a strain wave.

47 OTHER INSTRUMENTATION↗
DOE OSTI2026

Quaternary i-MAX Phases (Mo 2/3 RE 1/3 ) 2 AlC (RE: Dy, Tb, Er): Experimental Characterization and First-Principles Insights into their Fundamental Properties

Rare earth (RE)-based materials have unique electronic, magnetic, and optical properties, leading to the recent discovery of atomically layered solids with the chemical formula (M' 2/3 RE 1/3 ) 2 AlC, which have since garnered significant attention in the scientific community. This study aims to synthesize, characterize, and investigate the structural and thermal stability of the RE i-MAX phases. We prepared i-MAX phases using molybdenum (Mo) as M′ and RE elements as Dy, Tb, and Er, namely (Mo 2/3 Dy 1/3 ) 2 AlC, (Mo 2/3 Tb 1/3 ) 2 AlC, and (Mo 2/3 Er 1/3 ) 2 AlC. Structural characterization through x-ray diffraction (XRD) and Raman spectroscopy confirms the formation of the RE-based i-MAX phase, along with the presence of minor impurity phases in the alloys. Thermogravimetric analysis (TGA) conducted up to 1000°C under ambient conditions reveals that the i-MAX phases remain thermally stable up to approximately 450°C, beyond which oxidation leads to a noticeable weight gain in all samples. Differential scanning calorimetry (DSC) measurements during heating and cooling cycles show endothermic and exothermic peaks for (Mo 2/3 Dy 1/3 ) 2 AlC i-MAX in the 410–420°C range, indicating a temperature-induced minor atomic arrangement. In contrast, these peaks are absent in the Tb- and Er-based i-MAX phases. These findings offer valuable insights into the thermal behavior and stability of these i-MAX phases under thermal stress, contributing to a deeper understanding of their unique properties. Furthermore, first-principles density functional theory (DFT) calculations were performed to investigate the electronic and optical properties of the i-MAX phases. The results reveal their metallic nature, with pronounced contributions from Mo and RE elements near the Fermi level and within the conduction band.

Rare earth↗
DOE OSTI2021

Nonequilibrium charge-density-wave order beyond the thermal limit

The interaction of many-body systems with intense light pulses may lead to novel emergent phenomena far from equilibrium. Recent discoveries, such as the optical enhancement of the critical temperature in certain superconductors and the photo-stabilization of hidden phases, have turned this field into an important research frontier. Here, we demonstrate nonthermal charge-density-wave (CDW) order at electronic temperatures far greater than the thermodynamic transition temperature. Using time- and angle-resolved photoemission spectroscopy and time-resolved X-ray diffraction, we investigate the electronic and structural order parameters of an ultrafast photoinduced CDW-to-metal transition. Tracking the dynamical CDW recovery as a function of electronic temperature reveals a behaviour markedly different from equilibrium, which we attribute to the suppression of lattice fluctuations in the transient nonthermal phonon distribution. A complete description of the system’s coherent and incoherent order-parameter dynamics is given by a time-dependent Ginzburg-Landau framework, providing access to the transient potential energy surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Elimination of remnant phases in low-temperature growth of wurtzite ScAlN by molecular-beam epitaxy

We report growth of wurtzite Sc x Al 1-x N (x < 0.23) by plasma-assisted molecular-beam epitaxy on c-plane GaN at high temperatures significantly alters the extracted lattice constants of the material due to defects likely associated with remnant phases. In contrast, ScAlN grown below a composition-dependent threshold temperature exhibits uniform alloy distribution, reduced defect density, and atomic-step surface morphology. The c-plane lattice constant of this low-temperature ScAlN varies with composition as expected from previous theoretical calculations and can be used to reliably estimate alloy composition. Moreover, lattice-matched Sc 0.18 Al0 .82 N/GaN multi-quantum wells grown under these conditions display strong and narrow near-infrared intersubband absorption lines that confirm advantageous optical and electronic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Reconfigurable Grating Diffraction Structural Color in Self-Assembled Colloidal Crystals

Self-assembled colloidal crystals display structural colors due to light diffracted from their microscale, ordered structure. This color arises due to Bragg reflection (BR) or grating diffraction (GD); the latter mechanism is much less explored than the former. Here the design space for generating GD structural color is identified and its relative advantages are demonstrated. Electrophoretic deposition is used to self-assemble crystals with fine crystal grains from colloids of diameter 1.0 µm. The structural color in transmission is tunable across the full visible spectrum. The optimum optical response—represented by both color intensity and saturation—is observed at low layer number (≤5 layers). The spectral response is well predicted by Mie scattering of the crystals. Taken together, the experimental and theoretical results demonstrate that vivid grating colors with high color saturation can be produced from thin layers of micron-sized colloids. These colloidal crystals extend the potential of artificial structural color materials.

42 ENGINEERING↗
DOE OSTI2024

Parameter development and characterization of laser powder directed energy deposition of Nb – Alloy C103 for thin wall geometries

This work focuses on the parameter development and microstructural characterization of Nb-based alloy C103 for thin wall structures produced via laser powder – directed energy deposition (LP – DED). Laser power and scanning speeds were varied as part of a design of experiments to identify adequate print parameters. Combinations were evaluated for relative density, porosity, and geometrical accuracy. A combination of a laser power of 1420 W and scanning speed of 14 mm/s resulted in a relative density >99%, exhibited a consistent weld bead profile and was used for further microstructural evaluation. A mix of optical and scanning electron microscopy (SEM) revealed small, slightly elongated grains along the edges and large epitaxial grains in the central region along the Build – Transverse view. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis revealed Hf rich columnar cells in the center that transition into an evenly spaced cellular structure towards the edges of the built sample. Electron backscatter diffraction (EBSD) scans show a sharp [001] texture when looking at the cross section of the sample along the build direction. The Build – Scan view revealed a zig – zag pattern that follows the back – and – forth deposition strategy that was used. Finally, microhardness measurements were taken in the as – built (AB) and stress relieved (SR) conditions to baseline preliminary mechanical properties. The AB condition exhibited a large amount of scatter in the data and averages up to 11% larger than the SR condition. The reduction in scatter upon applying the SR cycle are indicative of a large concertation of dislocations present in the AB condition.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Transient Mesoscopic Immiscibility, Viscosity Anomaly, and High Internal Pressure at the Semiconductor–Metal Transition in Liquid Ga 2 Te 3

Gallium tellurides appear to be promising phase-change materials (PCMs) of the next generation for brain-inspired computing and reconfigurable optical metasurfaces. They are different from the benchmark PCMs because of sp 3 gallium hybridization in both cubic Ga 2 Te 3 and amorphous pulsed laser deposition (PLD) films. Liquid Ga 2 Te 3 also shows a viscosity η(T) anomaly just above melting when η(T) first increases and only then starts decreasing. We used high-energy X-ray diffraction to observe a transient mesoscopic immiscibility that suggested dense metallic liquid droplets in a semiconducting melt. The η(T) shape was consistent with this finding. A vanishing first sharp diffraction peak that also shifts to a higher Q indicates a high internal pressure in the metallic melt, which produces a remarkable asymmetry of the Ga–Te nearest neighbor distances and is reminiscent of high-pressure rhombohedral Ga 2 Te 3 . Finally, the observed phenomena provide a realistic scenario for a fast, multilevel SET–RESET response, which also unravels similar trends in the purported density-driven liquid polyamorphism of water, phosphorus, sulfur, and other materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

2022 AI Testbed Expeditions Report

By exploiting the coherent properties of a light source, coherent diffraction imaging (CDI) is able to obtain the sample image at a nanoscale resolution using the measured diffraction pattern. Bragg Coherent Diffraction Imaging (BCDI) has become valuable for recovering the displacement and strain field of crystals, providing a valuable tool in material science and solid-state physics. X-ray ptychography is another emerging CDI technique that can produce a high-resolution image of the extended sample and has become popular in many research areas (e.g., materials science, biology, electronics, and optics characterization). CDI including BCDI and ptychography has become an established technique in Synchrotron Facilities including the Advanced Photon Source (APS) and will greatly benefit from the 100x coherent flux increase of the upcoming APS Upgrade (APSU). The current image formation process in CDI employs iterative phase retrieval algorithms, which is a time-consuming and computationally expensive process. Especially after APSU, the traditional iterative methods will not be able to match the experimental data acquisition speed. We employ deep learning (DL) approach to replace the iterative approaches, therefore allowing hundreds of times faster recovery of the object. We developed AutoPhaseNN, a DL-based approach which learns to solve the inverse problem without labeled data. Taking 3D BCDI as a representative technique, AutoPhaseNN has been demonstrated to be one hundred times faster than traditional iterative phase retrieval methods while providing comparable image quality. The current network is trained with 64 x 64 x 64 data size, to achieve higher resolution imaging, we will need to scale the network to input and train/infer 3D arrays of size 256 x 256 x 256 (today) and of size 2560x2560x2560 (APSU). However, the scalability of the network is restricted due to the memory-intensive training process. To perform the training for a 256 x 256 x 256 data size, the required memory exceeds the capacity of the current machine. In this project, we explore using Sambanova system to train the network for the direct data inversion for CDI.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Development of green-colour-emitting pyrotechnics as a core for 3D temperature imaging sensors inside coal boilers

Efficiency in the control operation of the boilers for coal and coal with biomass can be further improved if the flue gas temperature distribution can be better characterized. This is very difficult in these harsh environmental systems, where spatially resolved measurements are nearly impossible with solid-state sensors. Here, in this work, we evaluate the development of pyrotechnic compounds that would serve as the basis for a novel optical mapping of the temperature inside coal boilers. For this purpose, various green-colour-emitting pyrotechnics using BaCl 2 · 2H 2 O and Ba(NO 3 ) 2 as the green light source were prepared, as this colour offers a distinct signal from the combustion-based background in the boiler. These pyrotechnics were characterized using thermogravimetric analysis (TGA) and X-ray diffraction (XRD) and tested using a flat-flame burner. Furthermore, the composition was varied to evaluate the effect of different metal fuels such as Sn, Co, and Mg, as well as various binders such as ethylcellulose, shellac, parlon, and PVC on green light emission. The emission intensity and the apparent ignition temperature were strongly dependent on the metal type, with Mg showing higher intensities. On the other hand, the effect of the binder showed that the ignition behaviour, emission intensity, and spectral purity were influenced by the nature and exothermicity of the binder. The addition of other potential green light-producing materials, such as boric acid, increased the intensity of emission by 17% for a BaCl 2 · 2H 2 O-based composition. This study identified prospective compositions with intense and bright green-colour emissions that have high spectral purities.

42 ENGINEERING↗
DOE OSTI2025

Scalable freeform optimization of wide-aperture 3D metalenses by zoned discrete axisymmetry

We introduce a novel framework for design and optimization of 3D freeform metalenses that attains nearly linear scaling of computational cost with diameter, by breaking the lens into a sequence of radial “zones” with 𝑛-fold discrete axisymmetry, where 𝑛 increases with radius. This allows vastly more design freedom than imposing continuous axisymmetry, while avoiding the compromises of the locally periodic approximation (LPA) or scalar diffraction theory. Using a GPU-accelerated finite-difference time-domain (FDTD) solver in cylindrical coordinates, we perform full-wave simulation and topology optimization within each supra-wavelength zone. We validate our approach by designing millimeter and centimeter-scale, poly-achromatic, 3D freeform metalenses which outperform the state of the art. By demonstrating the scalability and resulting optical performance enabled by our “zoned discrete axisymmetry” (ZDA) and supra-wavelength domain decomposition, we highlight the potential of our framework to advance large-scale meta-optics and next-generation photonic technologies.

Sun, Mengdi [Wesleyan University]↗
DOE OSTI2021

Interface and optical properties of Zn 1-x Mg x O films with Mg content of more than 70% grown on the (1$\bar{2}$10)-ZnO substrates

Fabricating Zn 1-x MgxO films with a high Mg content is key to their applications in deep-ultraviolet optoelectronic devices. In this work, we report the preparation of Zn1-xMgxO films on ($1\bar{2}10$)-ZnO substrates by molecular beam epitaxy. The Zn 1-x Mg x O/($1\bar{2}10$)-ZnO structure is revealed by x-ray diffraction and high-resolution transmission electron microscopy. Remarkably, no cubic MgO is observed for films with 74.6% Mg content; the film shows mainly the wurtzite structure with some intermediate phases at the interface. Photoluminescence spectra show that the film exhibits good optoelectronic properties with a bandgap of 4.6 eV. This work provides a new avenue for the fabrication of deep-ultraviolet Zn 1-x Mg x O films.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2026

Design of a broadband, high-power, off-axis spiral polarization reflector

Spirally polarized beams are known to produce a strong longitudinal field under high numerical aperture focusing. Here, we report on the design of a reflective optical element with an off-axis geometry that is capable of transforming a uniformly polarized beam into a predominantly spirally polarized beam. By utilizing the retardance present in Fresnel reflection, our device can operate over a broad range of wavelengths. The output polarization and intensity structure of a beam passing through the reflector are calculated using polarization and scalar ray tracing. Vector diffraction is used to calculate the polarization and intensity structure under $f/0.656$ focusing. The off-axis reflective design is well-suited for high-power laser applications and could enable current and future laser-based particle accelerators to achieve strong longitudinal fields at focus.

Black, A. Nicholas [Univ. of Rochester, NY (United↗
DOE OSTI2021

Ferroelectrics everywhere: Ferroelectricity in magnesium substituted zinc oxide thin films

We demonstrate ferroelectricity in Mg-substituted ZnO thin films with the wurtzite structure. Zn 1–x Mg x O films are grown by dual-cathode reactive magnetron sputtering on (111)-Pt // (0001)-Al 2 O 3 substrates at temperatures ranging from 26 to 200 °C for compositions spanning from x = 0 to x = 0.37. X-ray diffraction indicates a decrease in the c-lattice parameter and an increase in the a-lattice parameter with increasing Mg content, resulting in a nearly constant c/a axial ratio of 1.595 over this composition range. Transmission electron microscopy studies show abrupt interfaces between Zn 1–x Mg x O films and the Pt electrode. When prepared at pO 2 = 0.025, film surfaces are populated by abnormally oriented grains as measured by atomic force microscopy for Mg concentrations >29%. Raising pO 2 to 0.25 eliminates the misoriented grains. Optical measurements show increasing bandgap values with increasing Mg content. When prepared on a 200 °C substrate, films display ferroelectric switching with remanent polarizations exceeding 100 μC cm –2 and coercive fields below 3 MVcm –1 when the Mg content is between ~30% and ~7%. Substrate temperature can be lowered to ambient conditions, and when doing so, capacitor stacks show only minor sacrifices to crystal orientation and nearly identical remanent polarization values; however, coercive fields drop below 2 MV/cm. Using ambient temperature deposition, we demonstrate ferroelectric capacitor stacks integrated directly with polymer substrate surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Fast and bright scintillators for ultrafast materials dynamics using 4th generation synchrotron

We present recent advances in fast and bright scintillators for ultrafast X-ray phase contrast imaging of dynamic materials experiments at the upgraded Advanced Photon Source (APS-U), a fourth generation synchrotron. APS-U enables hard X-ray imaging at frame rates of at least 13 MHz (corresponding to 77 ns or shorter interframe intervals), creating a new need for scintillators with faster response and higher light output than lutetium yttrium oxyorthosilicate (LYSO). For indirect imaging and diffraction with ultrafast cameras, commercial lanthanum bromide (LaBr3) and cerium bromide (CeBr3) are promising candidates. These materials exhibit decay times approximately a factor of two shorter than LYSO (around 40 ns) and lutetium oxyorthosilicate (LSO), while maintaining comparable light yield per incident X-ray photon. However, their implementation at APS-U requires addressing several challenges, including material limitations due to hygroscopicity, efficient optical coupling to imaging systems, and high quantum efficiency for conversion of scintillation light, predominantly at wavelengths below 400 nm, into detectable electronic signals. We report results from material characterization, detector integration and packaging, and beamline experiments of materials with impact. In addition, emerging scintillator classes, including perovskites and high-entropy materials, are discussed as potential alternatives for next-generation ultrafast X-ray diagnostics.

Wang, Zhehui [Los Alamos] (ORCID:0000000178264063)↗
DOE OSTI2020

Point and extended defects in heteroepitaxial 𝛽−G⁡a 2 ⁢O 3 films

G⁡a 2 ⁢O 3 is emerging as an excellent potential semiconductor for high power and optoelectronic devices. However, the successful development of G⁡a 2⁢ O 3 in a wide range of applications requires a full understanding of the role and nature of its point and extended defects. Here, in this work, high quality epitaxial G⁡a 2 ⁢O 3 films were grown on sapphire substrates by metal-organic chemical vapor deposition and fully characterized in terms of structural, optical, and electrical properties. Then defects in the films were investigated by a combination of depth-resolved Doppler broadening and lifetime of positron annihilation spectroscopies and thermally stimulated emission (TSE). Positron annihilation techniques can provide information about the nature and concentration of defects in the films, while TSE reveals the energy level of defects in the bandgap. Despite very good structural properties, the films exhibit short positron diffusion length, which is an indication of high defect density and long positron lifetime, a sign for the formation of Ga vacancy related defects and large vacancy clusters. These defects act as deep and shallow traps for charge carriers as revealed from TSE, which explains the reason behind the difficulty of developing conductive G⁡a 2 ⁢O 3 films on non-native substrates. Positron lifetime measurements also show nonuniform distribution of vacancy clusters throughout the film depth. Further, the work investigates the modification of defect nature and properties through thermal treatment in various environments. It demonstrates the sensitivity of G⁡a 2 ⁢O 3 microstructures to the growth and thermal treatment environments and the significant effect of modifying defect structure on the bandgap and optical and electrical properties of G⁡a 2 ⁢O 3 .

defects↗
DOE OSTI2024

Directing Charge Carriers and Ferroelectric Domains at Lateral Interfaces in van der Waals Heterostructures

Emergent phenomena in traditional ferroelectrics are frequently observed at heterointerfaces. Accessing such functionalities in van der Waals ferroelectrics requires the formation of layered heterostructures, either vertically stacked (similar to oxide ferroelectrics) or laterally stitched (without equivalent in 3D-crystals). Here, we investigate lateral heterostructures of the ferroelectric van der Waals semiconductors SnSe and SnS. A two-step process produces ultrathin crystals comprising an SnSe core laterally joined to an SnS edge-band, as confirmed by Raman spectroscopy, transmission electron microscopy (TEM) imaging, and electron diffraction. TEM shows a moiré pattern across the SnSe core due to coverage by an ultrathin SnS layer. The ability of the lateral interface (IF) to direct excited carriers, probed by cathodoluminescence, shows electron transfer over 560 nm diffusion length from the SnS edge-band. Large, thin flakes supporting ferroelectricity allow investigating domains and domain wall interactions in uniform crystals and lateral heterostructures. Polarized optical microscopy of sub-20 nm flakes consistently shows ⟨110⟩ oriented stripe domains with mirror-twin domain walls. Heterostructures adopt two domain configurations, with domains either constrained to the SnSe core or propagating across the entire SnSe–SnS flakes. Furthermore, the combined results demonstrate multifunctional van der Waals heterostructures with high-quality IFs presenting extraordinary opportunities for manipulating carrier flows and ferroelectric domain patterns.

2D ferroelectrics↗