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DOE OSTI2024

DICER: A new instrument at LANSCE to constrain neutron capture rates on radionuclides

. With very few exceptions, direct measurements of neutron capture rates on radionuclides have not been possible. A number of indirect methods have been pursued such as the surrogate method, the γ-ray strength function method, the Oslo method and the β-Oslo method. Substantial effort has been devoted to quantify the usually large systematic errors that accompany the results from these techniques. A new instrument has been developed at the Los Alamos Neutron Science Center (LANSCE) to provide more accu rate data on several radionuclides relevant to nuclear criticality safety, radiochemical diagnostics, astrophysics, nuclear forensics and nuclear security, by measuring the transmission of neutrons through radioactive samples and studying resonance properties. The Device for Indirect Capture on Radionuclides (DICER) and as sociated radionuclide production at the Isotope Production Facility (IPF), both at LANSCE, as well radioactive sample fabrication, have been under development the last few years. A description of the new apparatus, data on a few mid-weight stable isotopes and efforts on radionuclide measurements will be presented.

Nuclear Criticality Safety Program (NCSP)↗

DOE OSTI2024

Observation of tantalum deposition and growth on TiB2 and ZrB2 from PISCES-RF deuterium and helium plasma exposures

Deuterium and helium plasma exposures on bulk TiB2 and ZrB2 samples were performed using the PISCES-RF linear plasma device. 40 and 90 eV deuterium ion plasma exposures were performed at 240 and 800 °C sample temperatures, and 80 eV helium ion plasma exposures were performed at 800 °C sample temperatures. Following plasma exposures, it was discovered that two plasma conditions (90 eV deuterium and 80 eV helium at 800 °C) resulted in thick (>200 nm) tantalum-rich (>10 at%) surface features on the targets, presumably from tantalum sourced from a tantalum adapter mask or cap used as part of the target holder. This work aims to characterize these tantalum-rich features and examine the mechanisms of impurity deposition.Plasma-induced surface morphology of the tantalum-rich surface layers depends on plasma properties and target temperature and chemistry. Greater titanium sputtering compared to zirconium resulted in more distinct surface features in the TiB2 samples compared to the ZrB2 samples via increased, prompt deposition onto tantalum surface impurities. There is still uncertainty as to why thick tantalum deposition only occurred under some plasma exposure conditions but not others; it is likely due to tantalum sputtering by a combination of boron molecules from the targets and carbon-impurities in the tantalum mask or targets. Impurity driven surface features are a well-documented phenomena in samples exposed to plasma from linear plasma device facilities—this work confirms the occurrence of this and emphasizes the need for chemistry characterization of isolated post-mortem surface features in plasma-exposed samples.

Nuckols, Lauren↗

DOE OSTI2018

Influence of Sm2O3 addition on Judd-Ofelt parameters, thermal and optical properties of the TeO2-Li2O-ZnO-Nb2O5 glass system

Highlights: • Synthesis of Sm{sub 2}O{sub 3} doped TeO{sub 2}-Li{sub 2}O-ZnO-Nb{sub 2}O{sub 5} glass to be used in optical devices. • Area under the peak calculations of FTIR and Raman display higher presence of BOs. • DSC plots indicate high stability and high rigidity of prepared glass samples. • Judd-Ofelt analysis shows the ionic nature of Sm{sup 3+} ions with neighboring atoms. • Higher branching ratio values obtained from {sup 6}H{sub 5/2} → {sup 6}F{sub 5/2} emission transition. - Abstract: A series of transparent and light yellow color samples composed of Sm{sub 2}O{sub 3} doped tellurium oxide glasses with chemical composition 75TeO{sub 2}-5Li{sub 2}O-10ZnO-(10-X) Nb{sub 2}O{sub 5}-XSm{sub 2}O{sub 3} was prepared by conventional melt-quenching technique. Rare earth (Sm{sub 2}O{sub 3}) was added to improve all glass properties. From obtained radiative properties, the samples which prepared with above composition can be considered as a prospect application for laser design due to higher branching ratio. The physical properties including sample density, molar volume, and OPD were measured. The glassy nature is approved by XRD analysis. The structural modification of glass forming units with introducing Sm{sub 2}O{sub 3} was studied by FTIR and Raman spectra. The intensity ratio of TeO{sub 4}/TeO{sub 3} was measured to determine the ratio of bridging/non-bridging oxygen exists in glass network. Glass thermal stability, glass transition temperature, and melting temperature were obtained from DSC plots. The UV–vis-NIR absorption spectra display 9 peaks. Optical parameters including optical band gap E{sub Opt}, Urbach energy ΔE and refractive index n were determined. From absorption spectra, Judd-Ofelt intensity parameters (Ω{sub λ} and λ = 2, 4, 6) have been derived to study bonding nature. A spectroscopic quality factor was calculated. Branching ratio (β{sub r}) and lifetime (τ) have been calculated using JO parameters. Absorption and emission cross-sections were determined to measure the probability of an absorption or emission process. Finally, we propose that these prepared samples can be used in optical devices and other applications.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Transmission electron microscope cells for use with liquid samples

This disclosure provides systems, methods, and devices related to transmission electron microscopy cells for use with liquids. In one aspect a device includes a substrate, a first graphene layer, and a second graphene layer. The substrate has a first surface and a second surface. The first surface defines a first channel, a second channel, and an outlet channel. The first channel and the second channel are joined to the outlet channel. The outlet channel defines a viewport region forming a though hole in the substrate. The first graphene layer overlays the first surface of the substrate, including an interior area of the first channel, the second channel, and the outlet channel. The second graphene layer overlays the first surface of the substrate, including open regions defined by the first channel, the second channel, and the outlet channel.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Development of a Multi-Press Assembly Device for Planar Dynamic Material Property Targets

A class of dynamic material property (DMP) experiments on the Sandia National Laboratories (SNL) pulse power Z-Machine requires planar samples to be held in a panel assembly. A custom press device to fabricate the assemblies has the ability to assemble one sample, window, or stack at a time, resulting in a one week lead time for a typical three-pocket panel assembly. Fabrication of targets with more than three pockets can take longer. In late 2015, General Atomics (GA) conceptualized a new multi-press device to enable several samples, windows, or stacks to be assembled simultaneously, and a prototype was designed, procured, and outfitted in six months. Since June 2016, this multi-press design has successfully assembled 60 planar DMP targets. Furthermore, the development considerations for this new device and the resulting benefits for the fabrication of targets are discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Wireless Frequency‐Multiplexed Acoustic Array‐Based Acoustofluidics

Abstract Acoustofluidics has shown great potential in enabling on‐chip technologies for driving liquid flows and manipulating particles and cells for engineering, chemical, and biomedical applications. To introduce on‐demand liquid sample processing and micro/nano‐object manipulation functions to wearable and embeddable electronics, wireless acoustofluidic chips are highly desired. This paper presents wireless acoustofluidic chips to generate acoustic waves carrying sufficient energy and achieve key acoustofluidic functions, including arranging particles and cells, generating fluid streaming, and enriching in‐droplet particles. To enable these functions, the wireless acoustofluidic chips leverage mechanisms, including inductive coupling‐based wireless power transfer (WPT), frequency multiplexing‐based control of multiple acoustic waves, and the resultant acoustic radiation and drag forces. For validation, the wirelessly generated acoustic waves are measured using laser vibrometry when different materials (e.g., bone, tissue, and hand) are inserted between the WPT transmitter and receiver. Moreover, the wireless acoustofluidic chips successfully arrange nanoparticles into different patterns, align cells into parallel pearl chains, generate streaming, and enrich in‐droplet microparticles. This research is anticipated to facilitate the development of embeddable wireless on‐chip flow generators, wearable sensors with liquid sample processing functions, and implantable devices with flow generation and acoustic stimulation abilities for engineering, veterinary, and biomedical applications.

Li, Jiali↗

DOE OSTI2026

Development of a Flow-through Cell for Ultrasonic Extraction (UE)─Single Particle (SP)─ICP-MS─an Approach for Nano/Microparticle Elemental and Isotopic Analysis

Nanotechnology is a salient part of the scientific landscape, and analytical approaches are rapidly evolving to enable small-scale characterization of nano- and microparticle compositions and impurities. Here, a flow-through sonicating cell was developed for direct particle extraction from a silicon wafer and integrated with an inductively coupled plasma–mass spectrometer (ICP-MS) for subsequent elemental and isotopic characterization of the released particles. Ultrasonic extraction (UE)─single particle (SP)─ICP-MS offers controlled particle mobilization from solid substrates and allows for increased sample throughput by eliminating the need for pre-extraction of particles and decreasing sample preparation steps. Coupling this device to an ICP-MS with a time-of-flight (TOF) mass analyzer, it is possible to distinguish unique isotopic compositions of the particles. Both tungsten and nickel isotopically tagged particles, which were deposited on Si wafers, are presented here with analysis via UE─SP─ICP-MS. This approach could support efforts in the fields of particle synthesis, nuclear safeguards and forensics, environmental monitoring, and semiconductor industries in which the detection of particles from substrates and wafers is critical.

Paul, Molly [ORNL] (ORCID:0009000009672055)↗

DOE OSTI2023

Production of zirconium-88 via proton irradiation of metallic yttrium and preparation of target for neutron transmission measurements at DICER

Abstract A process for the production of tens to hundreds of GBq amounts of zirconium-88 ( 88 Zr) using proton beams on yttrium was developed. For this purpose, yttrium metal targets (≈20 g) were irradiated in a ~16 to 34 MeV proton beam at a beam current of 100–200 µA at the Los Alamos Isotope Production Facility (IPF). The 88 Zr radionuclide was produced and separated from the yttrium targets using hydroxamate resin with an elution yield of 94(5)% (1σ). Liquid DCl solution in D 2 O was selected as a suitable 88 Zr sample matrix due to the high neutron transmission of deuterium compared to hydrogen and an even distribution of 88 Zr in the sample matrix. The separated 88 Zr was dissolved in DCl and 8 µL of the obtained solution was transferred to a tungsten sample can with a 1.2 mm diameter hole using a syringe and automated filling station inside a hot cell. Neutron transmission of the obtained 88 Zr sample was measured at the Device for Indirect Capture Experiments on Radionuclides (DICER).

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2018

Strain-Induced Spin-Resonance Shifts in Silicon Devices

In spin-based quantum-information-processing devices, the presence of control and detection circuitry can change the local environment of a spin by introducing strain and electric fields, altering its resonant frequencies. These resonance shifts can be large compared to intrinsic spin linewidths, and it is therefore important to study, understand, and model such effects in order to better predict device performance. We investigate a sample of bismuth donor spins implanted in a silicon chip, on top of which a superconducting aluminum microresonator is fabricated. The on-chip resonator provides two functions: it produces local strain in the silicon due to the larger thermal contraction of the aluminum, and it enables sensitive electron spin-resonance spectroscopy of donors close to the surface that experience this strain. Through finite-element strain simulations, we are able to reconstruct key features of our experiments, including the electron spin-resonance spectra. Our results are consistent with a recently observed mechanism for producing shifts of the hyperfine interaction for donors in silicon, which is linear with the hydrostatic component of an applied strain.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2016

Electron microscopy study of the microstructure of Ni–W substrate surface

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni{sub 95}W{sub 5} tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO{sub 4} precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°C is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing in a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

An Experimental Cell for a Radio Light Receiver

The problem of creating a receiver for incoherent microwave radiation from sources realized on the basis of ultra-wideband oscillators of chaotic oscillations and objects and surfaces “illuminated” by these sources has been considered. The structure of the device is proposed, the experimental sample is described, and its ability to register sources of incoherent microwave radiation with an integrated output power of ~2 mW at a distance of more than 100 m is shown.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2023

Autosampler software

control software for an automated liquid chromatography sample injection and separation system. It is related to a PNNL invention report 31630-E, Method for direct delivering trace samples from smallsize wells to liquid chromatography and mass spectrometry. The main purpose of the control software is to enable automated sample injection from a nanowell device.

Liyu, Andrey↗

DOE OSTI2021

Thin-film chemical expansion of ceria based solid solutions: laser vibrometry study

The chemical expansion of Pr 0.1 Ce 0.9 O 2-δ (PCO) and CeO 2-δ thin films is investigated in the temperature range between 600 °C and 800 °C by laser Doppler vibrometry (LDV). It enables non-contact determination of nanometer scale changes in film thickness at high temperatures. The present study is the first systematic and detailed investigation of chemical expansion of doped and undoped ceria thin films at temperatures above 650 °C. The thin films were deposited on yttria stabilized zirconia substrates (YSZ), operated as an electrochemical oxygen pump, to periodically adjust the oxygen activity in the films, leading to reversible expansion and contraction of the film. This further leads to stresses in the underlying YSZ substrates, accompanied by bending of the overall devices. Film thickness changes and sample bending are found to reach up to 10 and several hundred nanometers, respectively, at excitation frequencies from 0.1 to 10 Hz and applied voltages from 0–0.75 V for PCO and 0–1 V for ceria. At low frequencies, equilibrium conditions are approached. As a consequence maximum thin-film expansion of PCO is expected due to full reduction of the Pr ions. The lower detection limit for displacements is found to be in the subnanometer range. At 800 °C and an excitation frequency of 1 Hz, the LDV shows a remarkable resolution of 0.3 nm which allows, for example, the characterization of materials with small levels of expansion, such as undoped ceria at high oxygen partial pressure. As the correlation between film expansion and sample bending is obtained through this study, a dimensional change of a free body consisting of the same material can be calculated using the high resolution characteristics of this system. A minimum detectable dimensional change of 5 pm is estimated even under challenging high-temperature conditions at 800 °C opening up opportunities to investigate electro-chemo-mechanical phenomena heretofore impossible to investigate. The expansion data are correlated with previous results on the oxygen nonstoichiometry of PCO thin films, and a defect model for bulk ceria solid solutions is adopted to calculate the cation and anion radii changes in the constrained films during chemical expansion. The constrained films exhibit anisotropic volume expansion with displacements perpendicular to the substrate plane nearly double that of bulk samples. The PCO films used here generate high total displacements of several 100 nm’s with high reproducibility. Consequently, PCO films are identified to be a potential core component of high-temperature actuators. They benefit not only from high displacements at temperatures where most piezoelectric materials no longer operate while exhibiting, low voltage operation and low energy consumption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Two and three-dimensional near infrared subcutaneous structure imager using realtime nonlinear video processing

A method includes placing an imaging device in contact with a sample, irradiating the sample via an illuminator such that radiation scatters off of the structure, and providing the scattered radiation to a detector to generate a digital video signal. A processor then performs various operations including subtracting a sum of a black state value and a user-defined black level clamping value from the digital video signal to create subtracted image data, substituting negative values in the subtracted image data with a reference value to create modified image data, and amplifying the modified image data by a user-defined gain to create contrast enhanced image data.

Krasowski, Michael J.↗

DOE OSTI2018

Pyrite shrink-film laminate as a hydroxyl radical generator

Disclosed are hydroxyl radial generating devices, comprising: a substrate layer; and a pyrite layer configured to produce hydroxyl radicals. Another aspect relates to a method for producing a hydroxyl radical generating device, comprising: providing a polymeric substrate layer; placing a layer of pyrite on a surface of the polymeric substrate layer to form a multi-layer structure; and applying heat to the multi-layer structure such that at least the surface of the polymeric substrate layer contracts; wherein the layer of pyrite contracts to a lesser extent than the surface of the polymeric substrate layer providing a textured surface comprising the pyrite layer. Also disclosed is a method of analysis, comprising: placing a solution comprising a biological substance on a sample site of a hydroxyl generating device comprising a surface of pyrite; incubating the solution; and analyzing a sample including proteolytic fragments of the biological substance.

Brenowitz, Michael David↗

DOE OSTI2021

Growth, characterization, and Chern insulator state in MnBi 2⁢ Te 4 via the chemical vapor transport method

As the first intrinsic antiferromagnetic topological insulator, MnBi 2 Te 4 has provided a platform to investigate the interplay of band topology and magnetism as well as the emergent phenomena arising from such an interplay. Here we report the chemical-vapor-transport (CVT) growth and characterization of MnBi 2 Te 4 , as well as the observation of the field-induced quantized Hall conductance in 6-layer devices. Through comparative studies between our CVT-grown and flux-grown MnBi 2 Te 4 via magnetic, transport, scanning tunneling microscopy, and angle-resolved photoemission spectroscopy measurements, we find that CVT-grown MnBi 2 Te 4 is marked with higher Mn occupancy on the Mn site, slightly higher Mn Bi antisites, smaller carrier concentration, and a Fermi level closer to the Dirac point. Furthermore, a 6-layer device made from the CVT-grown sample shows by far the highest mobility of 2500 cm 2 V s in MnBi 2 Te 4 devices with the quantized Hall conductance appearing at 1.8 K and 8 T. Furthermore, our study provides a route to obtain high-quality single crystals of MnBi 2 Te 4 that are promising to make superior devices and realize emergent phenomena, such as the layer Hall effect and quantized anomalous Hall effect, etc.

36 MATERIALS SCIENCE↗

DOE OSTI2017

High current table-top setup for femtosecond gas electron diffraction

Here, we have constructed an experimental setup for gas phase electron diffraction with femtosecond resolution and a high average beam current. While gas electron diffraction has been successful at determining molecular structures, it has been a challenge to reach femtosecond resolution while maintaining sufficient beam current to retrieve structures with high spatial resolution. The main challenges are the Coulomb force that leads to broadening of the electron pulses and the temporal blurring that results from the velocity mismatch between the laser and electron pulses as they traverse the sample. We also present here a device that uses pulse compression to overcome the Coulomb broadening and deliver femtosecond electron pulses on a gas target. The velocity mismatch can be compensated using laser pulses with a tilted intensity front to excite the sample. The temporal resolution of the setup was determined with a streak camera to be better than 400 fs for pulses with up to half a million electrons and a kinetic energy of 90 keV. Finally, the high charge per pulse, combined with a repetition rate of 5 kHz, results in an average beam current that is between one and two orders of magnitude higher than previously demonstrated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Performance Assessment of Several Low-Cost Consumer-Grade Analog-to-Digital Conversion Devices

The Oak Ridge National Laboratory (ORNL) has pioneered an approach where low-cost consumer-grade electronics can be used as the basis of a highly reliable data acquisition architecture. One twenty-channel system based on this approach has been operating almost 4 years at ORNL. The architecture allows a mix-and-match level of configurability so the designer can select devices that best match the desired performance trade-offs. The most important device to be selected is the analog-to-digital converter. This paper explores the performance of several candidate audio recording devices that can be used as high-speed analog-to-digital converters for such measurement systems. Various performance metrics are explored including frequency response, noise floor, and synchronous sampling. Sample rates as high as 192 KHz are supported with 16 and 24-bit resolution. While most of the devices are dual-channel, there are multi-channel devices now available that will allow modal type of synchronous sampling. One such device was tested and is discussed is this paper.

Wetherington Jr, G↗