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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

133Xe Noble Gas Mass Spectrometry Measurement for High Purity Germanium Detector Performance Verification

Idaho National Laboratory produces quality control standards for laboratories that operate xenon radionuclide monitoring systems. Activities reported with each quality control standard are quantified using high purity germanium detectors. A collection of measurement capabilities are being set up at Idaho National Laboratory to establish an in-house high purity germanium detector performance verification system, with noble gas mass spectrometry being one of these measurement capabilities. The first noble gas mass spectrometry and high purity germanium measurement comparison is presented here. A Xe-133 gas sample was prepared and the activity was quantified with high purity germanium detectors. The Xe-133 sample was diluted with a known quantity of isotopically enriched Xe-126 gas; the resulting Xe-133 : Xe-126 atom ratio was calculated to be 1.15x10-4 +/- 2% at reference time t. An aliquot of this gas sample containing approximately 10 million Xe-133 atoms was introduced into a ThermoFisher Scientific Helix MC Plus noble gas mass spectrometer for analysis. The measured Xe-133 : Xe-126 atom ratio was determined to be 1.10x10-4 +/- 2% (1-sigma uncertainty) at reference time t, about 4.3% lower than the atom ratio determined with the measured high purity germanium activity.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗
NASA NTRS1978

High-purity silicon for solar cell applications

The article discusses the production of solar cells from high-purity silicon. The process consists of reducing the level of impurities in the raw materials, preventing material contamination before and after entering the furnace, and performing orders-of-magnitude reduction of metal impurity concentrations. The high-purity raw materials are considered with reference to carbon reductants, silica, and graphite electrodes. Attention is also given to smelting experiments used to demonstrate, in an experimental-scale furnace, the production of high-purity SoG-Si. It is found that high-purity silicon may be produced from high-purity quartz and chemically purified charcoal in a 50-kVA arc furnace. The major contamination source is shown to be impurities from the carbon reducing materials.

Dosaj, V. D.↗
DOE OSTI2025

Spatial and temporal evaluations of the liquid argon purity in ProtoDUNE-SP

Liquid argon time projection chambers (LArTPCs) rely on highly pure argon to ensure that ionization electrons produced by charged particles reach readout arrays. ProtoDUNE Single-Phase (ProtoDUNE-SP) was an approximately 700-ton liquid argon detector intended to prototype the Deep Underground Neutrino Experiment (DUNE) Far Detector Horizontal Drift module. It contains two drift volumes bisected by the cathode plane assembly, which is biased to create an almost uniform electric field in both volumes. The DUNE Far Detector modules must have robust cryogenic systems capable of filtering argon and supplying the TPC with clean liquid. This paper will explore comparisons of the argon purity measured by the purity monitors with those measured using muons in the TPC from October 2018 to November 2018. A new method is introduced to measure the liquid argon purity in the TPC using muons crossing both drift volumes of ProtoDUNE-SP. For extended periods on the timescale of weeks, the drift electron lifetime was measured to be above 30 ms using both systems. A particular focus will be placed on the measured purity of argon as a function of position in the detector.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Extraction of high-purity medium-chain-length polyhydroxyalkanoates via combined mechanical treatment and mild oxidation

Polyhydroxyalkanoates (PHAs) are a class of polyester polymers of microbial origin and considered biodegradable alternatives to conventional plastics. To make PHAs cost-competitive with synthetic plastics, their production cost, including extraction cost, should be significantly reduced. Herein, this study aimed to develop an effective extraction method based on combined mechanical disruption and chemical treatment for the recovery of high-purity medium-chain-length PHAs (mcl-PHAs) at a lower cost. mcl-PHAs-accumulating Pseudomonas strains were used for PHA extraction via high-pressure homogenization (HPH) coupled with surfactant treatment and mild alkaline hydrogen peroxide oxidation. The mechanical-chemical method was found to have strong synergy for PHA extraction while minimizing PHA depolymerization. The optimized condition resulted in nearly 90 % mcl-PHA recovery with high purity (>91 %). The extracted high-purity PHAs exhibited thermal and mechanical properties suitable for downstream applications entailing flexible and elastomeric materials.

42 ENGINEERING↗
DOE OSTI2026

Separation and Recovery of High-Purity Dysprosium from Electric Vehicle Scrap Permanent Magnets Using Cyanex 572, a Cationic Extractant in a Membrane Solvent Extraction Process

Rare earth elements (REEs), especially heavy rare earth elements such as dysprosium (Dy), have gained immense attention globally due to their widespread use in many state-of-the-art technologies. Consequently, demand for REEs is increasing rapidly in comparison to their supply. Recycling of REEs from end-of-life (EoL) electronic waste (e-waste) can help to mitigate the increasing gap between the demand and supply of REEs. This study reports the separation and recovery of high-purity Dy from various feedstocks such as scrap permanent magnets (SPMs), electric vehicle (EV) magnets, and mixed rare earth oxides (REOs) using an economically viable and scalable membrane solvent extraction (MSX) process. First, the optimized conditions (organic phase composition and feed solution acid concentration) for the separation of Dy from light REEs such as neodymium (Nd) and praseodymium (Pr) were evaluated using liquid–liquid extraction. Thereafter, a multistage MSX process was developed to separate high purity (>99.5 wt %) Dy from Nd and Pr using Cyanex 572, a cationic extractant. Using feedstocks with varying initial compositions, the MSX process obtained 100% pure Dy with 63–96% Dy recovery in three to six stages with a maximum extraction rate of 2.9 g m–2 h –1 . Purity of the recovered Dy was confirmed via additional characterization such as scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. This novel MSX process holds immense potential for industry deployment for the separation of heavy and light rare REEs from a wide range of e-waste.

electrical vehicle magnets↗
DOE OSTI2026

High Purity and Reduced Defects Hard Carbon Synthesis for Sodium-Ion Batteries

Hard carbon (HC) is the state-of-the-art anode material for sodium-ion batteries; however, the high-temperature carbonization of precursors (>1100 °C) often introduces inorganic impurities, an issue that remains largely underexplored. Here, we report a simple synthesis strategy for producing high purity HC by carbonizing a cellulose-derived precursor at 1400 °C under a slightly reducing Ar–H2 atmosphere on a graphite substrate, thereby eliminating the aluminum contamination observed during conventional carbonization on an alumina substrate under Ar. In addition, the modified synthetic condition reduces surface defects and the concentration of oxygen-containing functional groups, thereby altering the interphase formation on the HC surface. At a current density of 20 mA g−1, the impurity-rich HC exhibited an initial coulombic efficiency (ICE) of 74.1% and a reversible capacity of 248.8 mAh g−1. In sharp contrast, the high purity HC delivered a significantly improved ICE of 90.1% and a reversible capacity of 345.1 mAh g−1. These results underscore the critical importance of impurity and defect control during HC synthesis and highlight the clear electrochemical advantages of high purity HC with reduced defects for sodium-ion battery anodes.

Harshita, Lohanni↗
DOE OSTI2025

Enhanced spectral purity of WSe 2 quantum emitters via conformal organic adlayers

Quantum emitters in solid-state materials are typically embedded in the bulk of their hosts, making their electronic transitions inaccessible to surface modification. In contrast, two-dimensional materials, with their all-surface nature, offer a platform for tuning quantum emitters via chemical functionalization. Because of its semiconducting properties that enable electrical addressability, monolayer WSe 2 is a promising candidate for quantum emission, although the complex interplay between point defects and the localized strain needed to activate quantum emission leads to poor spectral purity. Here, we demonstrate that functionalizing monolayer WSe 2 with conformal adlayers of 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA) improves quantum emission spectral purity. Optical spectroscopy reveals that PTCDA functionalization lowers defect activation energies by 10 meV and induces a 30 nm redshift in quantum emission wavelength, while preserving the bright and dark exciton energies of monolayer WSe 2 . First-principles calculations corroborate these findings, thus providing molecular-level insight into the underlying mechanism of enhanced spectral purity.

Ananth, Riddhi [Northwestern Univ., Evanston, IL (↗
DOE OSTI2025

Blinking compromises the single-photon purity of individual CsPbBr 3 perovskite nanocrystals

Individual lead halide perovskite nanocrystals (PNCs) are promising single photon emitters but often suffer from photoluminescence blinking. Here, we correlate the photoluminescence blinking behavior of CsPbBr 3 NCs with their second-order correlation functions. We find that even moderate band-edge carrier blinking (BC-blinking) can significantly decrease the PNC’s single photon purity, while the impact from Auger blinking is much smaller. Additionally, the degree of BC-blinking can introduce significant uncertainties in single photon purity compared to PNCs with suppressed blinking. Furthermore, we quantitatively correlate the decrease in single photon purity with BC-blinking severity.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Ensuring High-Purity Liquid Argon for the LBNF FDC: Collaborative Cryogenics Research Between UNICAMP and Fermilab

Ensuring High-Purity Liquid Argon for the LBNF FDC: Collaborative Cryogenics Research Between UNICAMP and Fermilab R. Doubnik1, M. Adamowski1, F. de M. Blaszczyk1, A. Hahn1, D. Montanari1, R. Mrowca1, Z. West1, C. Adriano2, T. P.M. Alegre2, D. Correia2, A. A. B. Machado2, E. Segreto2, R. G. Gonçalves3, E. M. Assaf6, J. M. Assaf3, D. Cardoso3, M. B. Fontes4, H. Da Motta4, D. Noriler5, P. J. G. Pagliuso2. 1 Fermi National Accelerator Laboratory, PO Box 500, Batavia IL 60510, United States. 2 “Gleb Wataghin” Institute of Physics, UNICAMP, Campinas-SP, 13083-859, Brazil. 3 CPqMAE - Research Center on Advanced Materials and Energy, Federal University of São Carlos (UFSCar), São Carlos, 13565-905, Brazil. 4 The Brazilian Center for Research in Physics (CBPF), Rio de Janeiro-RJ, 22290-180, Brazil. 5 School of Chemical Engineering, UNICAMP, Campinas-SP, 13083-859, Brazil. 6 São Carlos Institute of Chemistry, University of São Paulo, São Carlos-SP, 13566-590, Brazil. Email: rdoubnik@fnal.gov Abstract. The Long-Baseline Neutrino Facility (LBNF) located at the Sanford Underground Research Facility (SURF) in Lead, South Dakota, hosts the Deep Underground Neutrino Experiment (DUNE). This experiment employs cryostats containing nearly 70,000 metric tons of high-purity liquid argon (LAr). Ensuring LAr purity is critical for achieving the required electron lifetime, which directly impacts the experiment’s signal-to-noise ratio. The Horizontal Drift (HD) detector demands an electron lifetime exceeding 3 ms within its 3.5 m drift, equivalent to less than 100 parts-per-trillion (ppt) Oxygen contamination, while the Vertical Drift (VD) detector requires over 6 ms electron lifetime within its 6.0 m drift, corresponding to less than 50 ppt Oxygen contamination. To mitigate Nitrogen (N2) quenching of scintillation light, N2 contamination must remain below 1 ppm, as higher levels can result in up to a 20 % loss of light. The Brazil State University of Campinas (UNICAMP) significantly contributes to LBNF FDC through the development of argon purification and regeneration systems for HD and VD cryostats. UNICAMP designed and constructed the Purification Liquid Argon Cryostat (PuLArC), a small-scale test facility holding approximately 90 liters of LAr. Tests using PuLArC demonstrated that 1.2 kg of Li-FAU zeolite could reduce N₂ contamination from 20-50 ppm to 0.1-1.0 ppm within 1-2 hours. Tests at Fermilab’s Iceberg cryostat (2,596 liters) confirmed scalability, with 3 kg of Li-FAU reducing N₂ contamination from ~5 ppm to <1 ppm over 96 hours cycles without active circulation. This presentation will detail the research methods, test setups, and results, showcasing the potential of Li-FAU as an alternative to Molecular Sieve 4A for large-scale LAr systems. This advancement enhances DUNE's precision and demonstrates the impact of international collaboration on cryogenic research.

Doubnik, Roza [Fermilab]↗
NASA NTRS1974

High purity silica reflective heat shield development

Progress is reported on the development of a high purity reflective heat shield material. Silicon dioxide was selected as the material because it is highly reflective in the correct wavelength band, has good ablation characteristics, is thermal shock resistant, and is readily fabricated to full size at reasonable cost. Conclusions indicate that: reflectance is affected by purity and morphology; the pure material is readily available; required purity and morphology can be maintained with reasonable care; high reflectances are determined (0.99 from 0.4 to 1.2 microns); major processing steps are defined; and the material appears to be cost effective. It is indicated that the materials are developed to the point of readiness for full scale fabrication and characterization.

Blome, J.↗
NASA NTRS1987

High purity silane and silicon production

Silicon tetrachloride, hydrogen and metallurgical silicon are reacted at about 400.degree.-600.degree. C. and at pressures in excess of 100 psi, and specifically from about 300 up to about 600 psi to form di- and trichlorosilane that is subjected to disproportionation in the presence of an anion exchange resin to form high purity silane. By-product and unreacted materials are recycled, with metallurgical silicon and hydrogen being essentially the only consumed feed materials. The silane product may be further purified, as by means of activated carbon or cryogenic distillation, and decomposed in a fluid bed or free space reactor to form high purity polycrystalline silicon and by-product hydrogen which can be recycled for further use. The process results in simplified waste disposal operations and enhances the overall conversion of metallurgical grade silicon to silane and high purity silicon for solar cell and semiconductor silicon applications.

Breneman, William C.↗
NASA NTRS2011

Spectroscopic Determination of Trace Contaminants in High Purity Oxygen

Oxygen used for extravehicular activities (EVA) must be free of contaminants because a difference in a few tenths of a percent of argon or nitrogen content can mean significant reduction in available EVA time. These inert gases build up in the extravehicular mobility unit because they are not metabolized or scrubbed from the atmosphere. Measurement of oxygen purity above 99.5% is problematic, and currently only complex instruments such as gas chromatographs or mass spectrometers are used for these determinations. Because liquid oxygen boil-off from the space shuttle will no longer be available to supply oxygen for EVA use, other concepts are being developed to produce and validate high purity oxygen from cabin air aboard the International Space Station. A prototype optical emission technique capable of detecting argon and nitrogen below 0.1% in oxygen was developed at White Sands Test Facility. This instrument uses a glow discharge in reduced pressure gas to produce atomic emission from the species present. Because the atomic emission lines from oxygen, nitrogen, and argon are discrete and in many cases well-separated, trace amounts of argon and nitrogen can be detected in the ultraviolet and visible spectrum. This is a straightforward, direct measurement of the target contaminants and may lend itself to a device capable of on-orbit verification of oxygen purity. System design and optimized measurement parameters are presented.

Hornung, Steven D.↗
NASA NTRS2015

Sample Acquisition and Analytical Chemistry Challenges to Verifying Compliance to Aviators Breathing Oxygen (ABO) Purity Specification

NASA has been developing and testing two different types of oxygen separation systems. One type of oxygen separation system uses pressure swing technology, the other type uses a solid electrolyte electrochemical oxygen separation cell. Both development systems have been subjected to long term testing, and performance testing under a variety of environmental and operational conditions. Testing these two systems revealed that measuring the product purity of oxygen, and determining if an oxygen separation device meets Aviator's Breathing Oxygen (ABO) specifications is a subtle and sometimes difficult analytical chemistry job. Verifying product purity of cryogenically produced oxygen presents a different set of analytical chemistry challenges. This presentation will describe some of the sample acquisition and analytical chemistry challenges presented by verifying oxygen produced by an oxygen separator - and verifying oxygen produced by cryogenic separation processes. The primary contaminant that causes gas samples to fail to meet ABO requirements is water. The maximum amount of water vapor allowed is 7 ppmv. The principal challenge of verifying oxygen produced by an oxygen separator is that it is produced relatively slowly, and at comparatively low temperatures. A short term failure that occurs for just a few minutes in the course of a 1 week run could cause an entire tank to be rejected. Continuous monitoring of oxygen purity and water vapor could identify problems as soon as they occur. Long term oxygen separator tests were instrumented with an oxygen analyzer and with an hygrometer: a GE Moisture Monitor Series 35. This hygrometer uses an aluminum oxide sensor. The user's manual does not report this, but long term exposure to pure oxygen causes the aluminum oxide sensor head to bias dry. Oxygen product that exceeded the 7 ppm specification was improperly accepted, because the sensor had biased. The bias is permanent - exposure to air does not cause the sensor to return to its original response - but the bias can be accounted for by recalibrating the sensor. After this issue was found, continuous measurements of water vapor in the oxygen product were made using an FTIR. The FTIR cell is relatively large, so response time is slow - but moisture measurements were repeatable and accurate. Verifying ABO compliance for oxygen produced by commercial cryogenic processes has a different set of sample acquisition and analytical chemistry challenges. Customers want analytical chemists to conserve as much as possible. Hygrometers are not exposed to hours of continuous flow of oxygen, so they don't bias, but small amounts of contamination in valves can cause a "fail". K bottles are periodically cleaned and recertified - after cleaning residual moisture can cause a "fail". Operators let bottle pressure drop to room pressure, introduce outside air into the bottle, and the subsequent fill will "fail". Outside storage of K‐bottles has allowed enough in‐leakage, so contents will "fail".

Graf, John↗
DOE OSTI2025

Exploiting the PRISM Feature and Purity Monitors of the SBND Neutrino Detector

The Short-Baseline Neutrino (SBN) program at Fermilab will pursue neutrino properties searches, exploiting three Liquid Argon Time Projection Chamber (LArTPC) experiments to investigate neutrino oscillations with neutrinos from the Booster Neutrino Beam (BNB). SBND will be the near detector in the program, measuring the un-oscillated flux. It is anticipated to begin operating in 2023. Thanks to its peculiar proximity to the neutrino source of about 110 meters, SBND will collect extremely high statistics data of the flux in the GeV energy range, providing unprecedented precision measurements. SBND particular setting also allows to take measurements at different distances from BNB’s center maintaining statistics high enough at each range. LArTPC and the cold electronics technologies, as well as the argon-neutrino interaction studies, will play a key role in future neutrino physics. In this prospect, this work was focused on two SBND features: SBND PRISM tool, with the aim of investigating neutrino flux at different distances from the beam axis, and Purity Monitors, which provide a clever measurement of argon purity in the detector, whose value is fundamental in neutrino-argon interaction.

43 PARTICLE ACCELERATORS↗
DOE OSTI2026

Effects of gas purity on backgrounds of collision reaction cell-equipped MC-ICP-MS

The advent of multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) instruments equipped with collision reaction cells (CRCs) facilitates interference removal/mitigation via online gas phase separations. This approach has proven effective for high intensity ion beams measured on Faraday collectors; however, it has been observed that introduction of gas in the CRC can result in significant background signals relative to the more sensitive ion counters. These backgrounds hinder use of these instruments for low level concentration and isotopic ratio measurements when employing a reaction gas. Here, this work directly evaluates the effect of gas purity on backgrounds of CRC-MC-ICP-MS instruments. Introducing high-purity research grade O 2 (99.999%) into the CRC produces complex background spectra with intensities >10 4 cps observed at most masses across the measured mass range (7-300 m / z ). Some features of the observed spectra (i.e., positive mass defects) can be attributed to molecular compounds comprised of significant hydrogen. Additionally, some specific molecular species can be identified (i.e., MoO x H y + ) and appear to be derived from molybdenum rods comprising the CRC. Further purifying the gas reduces the intensity of these backgrounds by several orders of magnitude, to <10 2 cps in many cases, and reduces complexity of the resulting spectra. This reduction in background appears to be in part driven by removal of impurities (i.e., H 2 O) from the gas. This work demonstrates that additional purification of reaction gases prior to introduction into the CRC significantly reduces backgrounds detected, potentially expanding the utility of CRC-MC-ICP-MS for making low level measurements using inline gas phase ion separations.

Schlieder, Tyler D. [Pacific Northwest National La↗
DOE OSTI2025

The impact of nickel concentration and stacking fault energy on deformation mechanisms in high-purity austenitic Fe-Cr-Ni alloys

Understanding how composition affects deformation mechanisms in austenitic stainless steels is essential for developing accurate predictive models of stress-induced failures and stress corrosion cracking. Nickel (Ni), an element classified as a critical element, plays a crucial role in these processes. It is important to examine how Ni concentration influences stacking fault energy (SFE) and, consequently, the deformation mechanisms of austenitic stainless steels. However, in commercial stainless steels, the effects of other alloying elements and impurities can obscure Ni's role, complicating efforts to isolate its impact. Here, in this study, we use two high-purity Fe-Cr-Ni alloys to investigate how Ni concentration and SFE interact to alter deformation mechanisms and induce martensitic transformation. By combining in situ synchrotron X-ray diffraction (XRD) tensile testing and post-mortem electron microscopy with density functional theory simulations, we gain precise insights into these phenomena. We find that the Fe18Cr10Ni (wt%) alloy, with its low SFE, exhibits higher stacking fault probability, deformation-induced martensitic transformation, and a lesser increase in dislocation density with plastic strain. In contrast, the Fe18Cr14Ni (wt%) alloy, with its higher SFE, shows enhanced deformation twinning and greater dislocation density with increasing strain. These findings from high-purity ternary alloys provide valuable insights that can guide the search for alternative elements to replace Ni while achieving similar effects on phase stability and deformation behavior.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Experimental investigation of the dependence of void nucleation and growth on initial microstructure in high-purity titanium under tension

An experimental investigation of failure mechanisms in relation to the initial microstructure in high-purity titanium samples is presented. The initial microstructure of the specimens was measured in 3D using diffraction-contrast tomography (DCT). Ex-situ X-ray computed tomography (XCT) was used to visualize voids in specimens at various levels of deformation attained by interrupted tensile testing. Electron backscatter diffraction (EBSD) mapping was used to characterize the deformed microstructures per specimen. The investigation showed that the location of failures was unrelated to the formation of the first voids, but rather the nucleation and growth of cracks were from heavily deformed surface regions. The areas surrounding the failure-causing cracks had the highest propensity for void development of any area in the specimen. This facilitated crack propagation through the specimen via “linking up”. The failure of the specimens by microvoid coalescence was bolstered by “dimpled” fracture surfaces. Paint composed of gallium embedded in rubber was used to track the displacement of points along the loading direction of the specimens, to relate the location of failure to the material's initial microstructure. However, the correlation proved difficult, due to complex microstructural evolution involving voids, grain fragmentations, and profuse twinning. Nevertheless, it was shown that necking occurred near the largest grain in the gauge section of the specimens. This is likely caused by the decrease in strength of larger grains, causing strain to concentrate in their vicinity. Here, a comprehensive picture of the failure processes in high-purity titanium under axial loading is presented and discussed in the paper.

36 MATERIALS SCIENCE↗
DOE OSTI2026

High-Purity Quantum Emission from an Au 24 (S-CH 2 Ph- t Bu) 20 Nanocluster at Room Temperature

Atomically precise gold nanoclusters have garnered significant attention for their diverse applications, ranging from biological labeling to optoelectronics. Their potential in optical quantum computing, which calls for ideal single-photon sources, has recently become a key area of interest. In the current work, we use photon antibunching experiments to explore the single-photon emission efficiency of atomically precise Au 24 nanoclusters protected by 4-tert-butylbenzyl mercaptan ligands (Au 24 (TBBM) 20 ). This cluster exhibits quantum emission with good photostability and without any observable blinking or spectral drift at room temperature under an inert gas atmosphere, with antibunching dips (g 2 (0)) as low as 0.07 in the solid state or, equivalently, a single-photon purity of 93% under time-gated conditions. Transient absorption and time-gated antibunching studies reveal that the short emission lifetime of this cluster and its high photoluminescence quantum yield in the solid state play critical roles in enhancing the emitted single-photon purity. This research advances the understanding of single-emitter behavior in atomically precise gold nanoclusters, contributing to the development of stable quantum emitters that are essential for quantum computing and cryptography.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗