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DOE OSTI2025

Application of a Triple Bubbler Inside Molten Salt for Pyroprocessing Safeguards Purposes

The application of a triple bubbler system within molten salt environments, specifically a eutectic mixture of LiCl-KCl, is explored for nuclear safeguards purposes, focusing on nuclear material accountancy (NMA) and holdup accountancy in pyroprocessing techniques. Traditional holdup accountancy methods, which involve periodic sampling and lengthy lead times, are being supplemented by the development of actinide sensors using electrochemistry. However, these methods alone are insufficient to meet regulatory requirements set by agencies like NRC and IAEA. The triple bubbler device measures salt level, density, and surface tension simultaneously using three dip tubes of varying diameters and heights. This study investigates the accuracy and robustness of the triple bubbler in molten salt conditions at temperatures ranging from 450-550°C. The updated bubbler design, utilizing tantalum metal and larger tube geometry, demonstrated minimal plugging and maintained measurement accuracy within acceptable uncertainties: 0.611% for depth, 1.34% for density, and approximately 40% for surface tension. Results indicate that the triple bubbler system is effective for real-time, accurate measurements in pyroprocessing environments, making it a promising tool for ensuring compliance with nuclear safeguards and supporting nuclear non-proliferation efforts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2019

Laser-Based Defect Reduction in Wide Bandgap Semiconductors Used in Radiation-Voltaics Devices: Radiation Hardening and Annealing

The primary goal of this study was to determine whether laser illumination at sub-bandgap wavelengths of semiconductors (especially those used for radiation voltaics) could anneal defects generated during radiation exposure (Beta and Alpha radiation). Defect annealing was probed on a set of Silicon Carbide (SiC) samples using in situ monitoring of the photoluminescence (PL) emissions from UV- to near infrared spectra under UV excitation (broadband or laser at λ L = 351 nm). No significant effect was found using 1064 nm wavelength light as the annealing source up to the laser damage threshold fluence of the nanosecond pulsed laser (10 Hz rep-rate). Additional research is needed to fully explore effects from laser annealing beyond the scope of this feasibility testing.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Microfluidic devices, systems, and methods for quantifying particles using centrifugal force

Embodiments of the present invention are directed toward microfluidic systems, apparatus, and methods for measuring a quantity of cells in a fluid. Examples include a differential white blood cell measurement using a centrifugal microfluidic system. A method may include introducing a fluid sample containing a quantity of cells into a microfluidic channel defined in part by a substrate. The quantity of cells may be transported toward a detection region defined in part by the substrate, wherein the detection region contains a density media, and wherein the density media has a density lower than a density of the cells and higher than a density of the fluid sample. The substrate may be spun such that at least a portion of the quantity of cells are transported through the density media. Signals may be detected from label moieties affixed to the cells.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2023

A Superconducting Micro-Magnetometer for Quantum Vortex in Superconducting Nanoflakes

Superconducting quantum interferometer device (SQUID) plays a key role in understanding electromagnetic properties and emergent phenomena in quantum materials. The technological appeal of SQUID is that its detection accuracy for the electromagnetic signal can precisely reach the quantum level of a single magnetic flux. However, conventional SQUID techniques normally can only be applied to a bulky sample and do not have the capability to probe the magnetic properties of micro-scale samples with small magnetic signals. Here, in this paper, it is demonstrated that, based on a specially designed superconducting nano-hole array, the contactless detection of magnetic properties and quantized vortices in micro-sized superconducting nanoflakes is realized. An anomalous hysteresis loop and a suppression of Little–Parks oscillation are observed in the detected magnetoresistance signal, which originates from the disordered distribution of the pinned vortices in Bi 2 Sr 2 CaCu 2 O 8+δ . Therefore, the density of pinning centers of the quantized vortices on such micro-sized superconducting samples can be quantitatively evaluated, which is technically inaccessible for conventional SQUID detection. The superconducting micro-magnetometer provides a new approach to exploring mesoscopic electromagnetic phenomena of quantum materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2013

An atomic force microscopy-based method for line edge roughness measurement

With the constant decrease of semiconductor device dimensions, line edge roughness (LER) becomes one of the most important sources of device variability and needs to be controlled below 2 nm for the future technological nodes of the semiconductor roadmap. LER control at the nanometer scale requires accurate measurements. We introduce a technique for LER measurement based upon the atomic force microscope (AFM). In this technique, the sample is tilted at about 45 Degree-Sign and feature sidewalls are scanned along their length with the AFM tip to obtain three-dimensional images. The small radius of curvature of the tip together with the low noise level of a laboratory AFM result in high resolution images. Half profiles and LER values on all the height of the sidewalls are extracted from the 3D images using a procedure that we developed. The influence of sample angle variations on the measurements is shown to be small. The technique is applied to the study of a full pattern transfer into a simplified gate stack. The images obtained are qualitatively consistent with cross-section scanning electron microscopy images and the average LER values agree with that obtained by critical dimension scanning electron microscopy. In addition to its high resolution, this technique presents several advantages such as the ability to image the foot of photoresist lines, complex multi-layer stacks regardless of the materials, and deep re-entrant profiles.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Direct Fabrication of Vertically Stacked Double Barrier Tunnel Junctions Based on Graphene and h-BN

Direct manufacturing of two-dimensional material-based double barrier (DB) tunnel junctions, based on a lithography-free approach was developed. Graphene/h-BN/Graphene/h-BN/Graphene devices were deposited on Si/SiO2 substrates by employing a plasma enhanced chemical vapor deposition technique in a sequential manner. DB tunneling junctions with varying barrier widths (by varying the thickness of the second graphene layer) were studied. Samples were characterized using Raman, Atomic Force Microscopy and X-ray photoemission spectroscopy. The I–V characteristics of tunneling current showed resonant tunneling behavior at room temperature with a negative differential conductance. The behavior could be explained with quantum mechanical double barrier tunneling model in which analytic solutions to Schrödinger’s equation were obtained in each region of the system. Resonances in transmission probability coefficient for varying barrier widths were evaluated and compared with the experimental results.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Impact of cobalt doping on structural and magnetic properties of zinc oxide nanocomposites synthesized by mechanical ball-milling method

A series of zinc oxide (ZnO) semiconductor nanocomposite samples doped with different concentrations of cobalt (Co) were successfully synthesized via simple and highly effective mechanical ball-milling method using suitable precursors. All doped nanocomposites crystallized in hexagonal wurtzite formation of ZnO. No alteration in the wurtzite structure, with no evidence of any segregated secondary phase(s) was detected with increasing doping concentrations. This result unambiguously verified the substitution of Zn 2+ sites by Co 2+ ions in the ZnO host lattice for different doping concentrations. Moreover, room temperature ferromagnetic behavior was observed in all doped nanocomposite samples in the reported work. Present study clearly shows that mechanical ball-milling is a facile, inexpensive, eco-friendly method to synthesize crystalline and magnetic Co doped ZnO nanocomposites for next generation spin-based devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2013

Growth of single crystalline TaON on yttria-stabilized zirconia (YSZ)

Owing to its high stability in aqueous solution and high quantum efficiency, tantalum based oxyntride (TaON) has attracted increasing attentions for application as visible light photocatalyst. However, despite the recent progress in photocatalytic studies, its bulk charge transport mechanisms are yet to be discovered because of the lack of single crystal sample. In this paper, high quality single crystalline TaON(100) thin film was prepared on cubic YSZ(100) surface by reactive RF magnetron sputtering to avail the understandings of charge transport mechanism so as to improve the device efficiency. The stoichiometry, crystal phase and structure were examined in situ by x-ray photoelectron spectroscopy (XPS) and ex situ by x-ray diffraction (XRD) and transmission electron microscopy (TEM). The TaON film crystallizes in monoclinic β-phase with its [010]/[001] directions aligned to those of the substrate. The small band gap of 2.5 eV as well as the high structure perfection suggests better performance for visible light water splitting. The method can be used to prepare other surface orientations to elucidate fundamental surface structure dependent photoactivities. - Graphical abstract: Structure of single crystalline β-TaON and its diffraction pole figure. Highlights: • High quality single crystal TaON(100) thin film were grown on YSZ(100) surface. • β-phase monoclinic TaON film is formed. • Its [010]/[001] directions are aligned to those of the substrate. • The small band gap and structure perfection suggest visible light photo-activity.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Effect of lattice orientation on compressive properties of selective laser sintered nylon lattice coupons

As AM lattices become more popular in medical devices, it is important to consider how lattice design parameters affect the mechanical integrity and performance of a device. This research investigated the effect of lattice orientation on the compressive mechanical response of five common lattice geometries: Hexagonal Honeycomb (Hex), Diamond, Voronoi Tessellation Method (VTM), sheet-based Gyroid, and Face-Centered-Cubic (FCC). Samples were tested at two relative densities and eight orientations, printed in Nylon 12 (PA2200) on an EOS P396. The mechanical response was compared to simulated finite element analysis (FEA) response for Hex and FCC lattices. Hex lattices displayed significant orientation dependance. Diamond lattices demonstrated some orientation dependance when at a lower relative density. Gyroid, FCC, and VTM all displayed minimal orientation dependance. Increasing lattice relative density appeared to reduce anisotropy among tested orientations of all lattice geometries except Hex. FEA simulations were able to produce a trend response that matched the mechanical response trends based on the investigated orientations. Furthermore, these results support the need for multi axial lattice mechanical test considerations. It also bolsters the need for lattice FEA models to have a sufficient comparator when identifying “worst-case” lattice test scenarios.

36 MATERIALS SCIENCE↗

DOE OSTI2018

4D nano-tomography of electrochemical energy devices using lab-based X-ray imaging

Electrochemical energy devices offer a variety of alternate means for low-carbon, multi-scale energy conversion and storage. Reactions in these devices are supported by electrodes with characteristically complex microstructures. To meet the increasing capacity and lifetime demands across a range of applications, it is essential to understand microstructural evolutions at a cell and electrode level which are thought to be critical aspects influencing material and device lifetime and performance. X-ray computed tomography (CT) has become a highly employed method for non-destructive characterisation of such microstructures with high spatial resolution. However, sub-micron resolutions present significant challenges for sample preparation and handling particularly in 4D studies, (three spatial dimensions plus time). Here, microstructural information is collected from the same region of interest within two electrode materials: a solid oxide fuel cell and the positive electrode from a lithium-ion battery. Using a lab-based X-ray instrument, tomograms with sub-micron resolutions were obtained between thermal cycling. The intricate microstructural evolutions captured within these two materials provide model examples of 4D X-ray nano-CT capabilities in tracking challenging degradation mechanisms. Furthermore, this technique is valuable in the advancement of electrochemical research as well as broader applications for materials characterisation.

25 ENERGY STORAGE↗

DOE OSTI2012

Enhanced microwave dielectric properties of Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics doping by metal Fe powders

Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics by adding mental Fe powders have been fabricated via the solid-state reaction method. The microstructures and optical properties of samples are systematically studied in order to establish the effects of Fe powder additives on microwave dielectric properties of Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics by x-ray diffraction, x-ray photoelectron spectroscopy, and optical reflective spectrum. The results show the coexistence of Fe{sup 2+} and Fe{sup 3+} in Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics, the decrease of O vacancy concentrations, and their incorporation into the B-site (Ti) of the Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} host lattice give rise to excellent microwave dielectric properties. All samples have a higher Q value above 290 while maintaining relatively high tunability above 16.6%. In particular, the sample with the composition of x = 0.035 mol has the dielectric constant of 889, Q Multiplication-Sign f value of 826 (at 1.370 GHz), and tunability of 24%, which are very promising for high power tunable devices. In comparison, Fe{sub 2}O{sub 3} oxide doped Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics with the same molar ratios of Fe exhibit inferior microwave properties. It indicates that additives of the metal Fe powders can more effectively improve dielectric properties of Ba{sub x}Sr{sub 1-x}TiO{sub 3} system than Fe{sub 2}O{sub 3} oxide.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Screening materials with the XIA UltraLo alpha particle counter at Southern Methodist University

Southern Methodist University houses one of five existing commercially available UltraLo 1800 production model alpha counters made by XIA LLC. The instrument has an electron drift chamber with a 707 cm{sup 2} or 1800 cm{sup 2} counting region which is determined by selecting the inner electrode size. The SMU team operating this device is part of the SuperCDMS screening working group, and uses the alpha counter to study the background rates from the decay of radon in materials used to construct the SuperCDMS experiment. We have studied four acrylic samples obtained from the MiniCLEAN direct dark matter search with the XIA instrument demonstrating its utility in low background experiments by investigating the plate-out of {sup 210}Pb and comparing the effectiveness of cleaning procedures in removing {sup 222}Rn progenies from the samples.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2014

Bi{sub 2}Sr{sub 2}CaCu{sub 2}O{sub 8} intrinsic Josephson junction stacks with improved cooling: Coherent emission above 1 THz

We report on Bi{sub 2}Sr{sub 2}CaCu{sub 2}O{sub 8} (BSCCO) intrinsic Josephson junction stacks with improved cooling, allowing for a remarkable increase in emission frequency compared to the previous designs. We started with a BSCCO stack embedded between two gold layers. When mounted in the standard way to a single substrate, the stack emits in the range of 0.43–0.82 THz. We then glued a second, thermally anchored substrate onto the sample surface. The maximum voltage of this better cooled and dimension-unchanged sample was increased and, accordingly, both the emission frequencies and the tunable frequency range were significantly increased up to 1.05 THz and to 0.71 THz, respectively. This double sided cooling may also be useful for other “hot” devices, e.g., quantum cascade lasers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Design of a telemetry system based on wireless power transmission for physiological parameter monitoring

An implanted telemetry system for experimental animals with or without anaesthesia can be used to continuously monitor physiological parameters. This system is significant not only in the study of organisms but also in the evaluation of drug efficacy, artificial organs, and auxiliary devices. The system is composed of a miniature electronic capsule, a wireless power transmission module, a data-recording device, and a processing module. An electrocardiograph, a temperature sensor, and a pressure sensor are integrated in the miniature electronic capsule, in which the signals are transmitted in vitro by wireless communication after filtering, amplification, and A/D sampling. To overcome the power shortage of batteries, a wireless power transmission module based on electromagnetic induction was designed. The transmitting coil of a rectangular-section solenoid and a 3D receiving coil are proposed according to stability and safety constraints. Experiments show that at least 150 mW of power could pick up on the load in a volume of Φ10.5 mm × 11 mm, with a transmission efficiency of 2.56%. Vivisection experiments verified the feasibility of the integrated radio-telemetry system.

36 MATERIALS SCIENCE↗

DOE OSTI2016

A generalization of the Drude-Smith formula for magneto-optical conductivities in Faraday geometry

In this study, we generalize the impulse response approach and Poisson statistics proposed by Smith [Phys. Rev. B 64, 155106 (2001)] to evaluate the longitudinal and transverse magneto-optical conductivities in an electron gas system in Faraday geometry. Comparing with the standard Drude model, the coefficients a{sub n} are introduced in the Drude-Smith formula to describe the backscattering or localization effect for the nth electronic scattering event. Such a formula can also be applied to study the elements of the dielectric function matrix in the presence of magnetic and radiation fields in electron gas systems. This theoretical work is primely motivated by recent experimental activities in measuring the real and imaginary parts of longitudinal and transverse magneto-optical conductivities in condensed matter materials and electronic devices using terahertz time-domain spectroscopy. We believe that the results obtained from this study can provide an appropriate theoretical tool in reproducing the experimental findings and in fitting with experimental data to determine the important sample and material parameters.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2017

Nonlinear terahertz metamaterials with active electrical control

Here, we present a study of an electrically modulated nonlinear metamaterial consisting of an array of split-ring resonators fabricated on n-type gallium arsenide. The resonant metamaterial nonlinearity appears as an intensity-dependent transmission minimum at terahertz frequencies and arises from the interaction between local electric fields in the split-ring resonator (SRR) capacitive gaps and charge carriers in the n-type substrate. We investigate the active tuning range of the metamaterial device as the incident terahertz field intensity is increased and conversely the effect of an applied DC bias on the terahertz field-induced nonlinear modulation of the metamaterial response. Applying a DC bias to the metamaterial sample alters the nonlinear response and reduces the net nonlinear modulation. Similarly, increasing the incident terahertz field intensity decreases the net modulation induced by an applied DC bias. Finally, we interpret these results in terms of DC and terahertz-field-assisted carrier acceleration, scattering, and multiplication processes, highlighting the unique nature of this DC-field modulated terahertz nonlinearity.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Magnetic structure determination of multiple phases in the multiferroic candidate GdCrO 3

Due to their potential applications in low-power consumption and/or multistate memory devices, multiferroic materials have attracted a lot of attention in the condensed matter community. As part of the effort to identify new multiferroic compounds, perovskite-based GdCrO 3 was studied in both bulk and thin film samples. A strong enhancement of the capacitance in a field suggested ferroelectric behaviour but significant leakage and no well developed P–E hysteresis loops were observed. Measurements clearly indicate the existence of a polar phase but only below 2 K (likely connected to Gd ordering). Here the determination of the magnetic structure through neutron diffraction collected on an isotopic 160 GdCrO 3 sample at the WISH diffractometer at ISIS is reported. The presence of three successive magnetic phases as a function of temperature (commensurate, spin re-orientation and incommensurate phases once the Gd order), previously only seen by magnetization, is confirmed. Using the most recent guidelines for reporting the determined structures, we highlight the benefits of using such nomenclature for discussing physical properties and consider possible mechanisms and couplings that led this seemingly rather isotropic system to display the complex structures observed.

incommensurate magnetic structure↗

DOE OSTI2024

Composition Quantification of SiGeSn Alloys Through Time-of-Flight Secondary Ion Mass Spectrometry: Calibration Methodologies and Validation With Atom Probe Tomography

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is a powerful technique for elemental compositional analysis and depth profiling of materials. However, it encounters the problem of matrix effects that hinder its application. In this work, we introduce a pioneering ToF-SIMS calibration method tailored for SixGeySnz ternary alloys. SixGe1-x and Ge1-zSnz binary alloys with known compositions are used as calibration reference samples. Through a systematic SIMS quantification study of SiGe and GeSn binary alloys, we unveil a linear correlation between secondary ion intensity ratio and composition ratio for both SiGe and GeSn binary alloys, effectively mitigating the matrix effects. Extracted relative sensitivity factor (RSF) value from SixGe1-x (0.07 < x < 0.83) and Ge1-zSnz (0.066 < z < 0.183) binary alloys are subsequently applied to those of SixGeySnz (0.011 < x < 0.113, 0.863 < y < 0.935 and 0.023 < z < 0.103) ternary alloys for elemental compositions quantification. These values are cross-checked by Atom Probe Tomography (APT) analysis, an indication of the great accuracy and reliability of as-developed ToF-SIMS calibration process. Furthermore, the proposed method and its reference sample selection strategy in this work provide a low-cost as well as simple-to-follow calibration route for SiGeSn composition analysis, thus driving the development of next-generation multifunctional SiGeSn-related semiconductor devices.

36 MATERIALS SCIENCE↗