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DOE OSTI2022

Crystal Chemistry and Thermodynamics of HREE (Er, Yb) Mixing in a Xenotime Solid Solution

Rare earth elements (REEs), the 15 naturally occurring lanthanides plus yttrium and scandium, are ubiquitously used in modern life as they are critical components of many advanced devices and technologies. However, the demand for REEs is not equal, with the heavy rare earth elements (HREEs) having a higher demand. Xenotime (HREEPO 4 ) is an important HREE ore mineral and globally is an economical source of HREE. Most of the crystallographic and thermodynamic properties of xenotime endmembers have been elucidated by calorimetric, solubility, and high-pressure studies. Yet, in natural systems, endmembers are rarely encountered, and instead, REE solid solutions are more commonly observed. Here, we characterize the crystal chemistry, thermodynamics of HREE mixing, and high-temperature material behaviors and thermochemistry of a synthetic erbium (Er)-ytterbium (Yb) binary xenotime solid solution (Er (x) Yb (1-x) PO 4 ) using a suite of experimental techniques, including X-ray fluorescence spectroscopy, synchrotron X-ray powder diffraction implemented with Rietveld analysis, Fourier transform infrared spectroscopy coupled with attenuated total reflectance, Raman spectroscopy, thermogravimetric analysis coupled with differential scanning calorimetry, and high-temperature oxide melt drop solution calorimetry. Our results shed light on the formation of natural xenotimes and lay the foundation for their industrial applications as thermal coating materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

PISCES-RF: a liquid-cooled high-power steady-state helicon plasma device

Radio-frequency (RF) driven helicon plasma sources can produce relatively high-density plasmas (n > 1019 m -3 ) at relatively moderate powers (<2 kW) in argon. However, to produce similar high-density plasmas for fusion relevant gases such as hydrogen (H), deuterium (D) and helium (He), much higher RF powers are needed. For very high RF powers, thermal issues of the RF-transparent dielectric window, used in the RF source design, limit the plasma operation timescales. To mitigate this constraint, we have designed, built and tested a novel helicon plasma source assembly with a fully liquid-cooled RF-transparent window which allows steady state operations at high power (up to 20 kW) and successfully produces high-density plasma with both argon and H. Deionized (DI) water, flowing between two concentric dielectric RF windows, is used as the coolant. We show that a full azimuthal blanket of DI water does not prevent high-density plasma production. From calorimetry on the DI water, we measure the net heat removed by the coolant at steady state conditions. Using infra-red imaging, we calculate the constant plasma heat deposition and measure the final steady state temperature distribution patterns on the inner surface of the ceramic layer. The heat deposition pattern follows the helical shape of the antenna. We also show the consistency between the heat absorbed by the DI water, as measured by calorimetry, and the total heat due to the combined effect of the plasma heating and the absorbed RF. These results are being used to answer critical engineering questions for the 200 kW RF device materials plasma exposure experiment being designed at the Oak Ridge National Laboratory as a next generation plasma material interaction device.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2026

Experimental evaluation of the vapor box divertor concept with an open vapor box module in Magnum-PSI

A promising approach to handle the intense plasma heat flux in the divertor region of a tokamak is the Vapor Box Divertor (VBD). Here plasma-lithium interaction creates a dense lithium vapor cloud which interacts with the incoming plasma, effectively shielding the tungsten surface beneath, therefore preventing overheating and sputtering of the tungsten and increasing the component’s lifetime. Two key steps must be addressed to validate this concept: investigating plasma-Li interactions and the transport mechanism of the latter in the presence of plasma. To explore this, a Vapor Box Module (VBM) has been designed for use with the linear plasma generator Magnum-PSI. The VBM consists of a series of three cylindrical boxes, with Li being evaporated at a controlled temperature in the central box (CB). Divertor-like plasma enters the VBM from an upstream aperture, interacts with the Li vapor cloud and exits through a downstream aperture ultimately impacting a target equipped with a calorimetry system. Optical diagnostics Thomson scattering, Filtered fast camera Imaging and optical emission spectroscopy provided information on plasma parameters in terms of electron density n e , temperature T e and plasma composition before and after this interaction. A significant reduction in plasma power was observed upon the establishment of lithium vaporization determined via cooling water calorimetry and embedded thermocouples at the downstream target. This resulted in a drop of the target temperature from ∼800 °C to ∼350 °C (57%) at the highest applied power (11.1 MW m −2 ) and CB temperature (∼700 °C). Lithium condensation at the side boxes of the VBM in combination with strong plasma momentum transfer effectively prevented upstream migration of lithium, while enhancing Li transport toward the target. The achievement of the two main goals of reducing plasma power and confining the Li in the VBM, are consistent with earlier published preliminary SOLPS-ITER simulations. This study shows that the presence of lithium in a VBD-like configuration can result in a strong reduction of power to the target surface, while at the same time the lithium vapor is effectively confined by the VBM, aided by the incoming plasma, preventing its escape from the VBM geometry. This represents a valuable step toward validating the feasibility of the VBD configuration in future fusion reactors.

Magnum-PSI↗

DOE OSTI2021

Spatially inhomogeneous superconductivity in UTe 2

The newly discovered superconductor UTe 2 is a strong contender for a topological spin-triplet state wherein a multicomponent order parameter arises from two nearly degenerate superconducting states. A key issue is whether both of these states intrinsically exist at ambient pressure. Through thermal expansion and calorimetry, we show that UTe 2 at ambient conditions exhibits two detectable transitions only in some samples, and the size of the thermal expansion jump at each transition varies when the measurement is performed in different regions of the sample. This result indicates that the two transitions arise from two spatially separated regions that are inhomogeneously mixed throughout the volume of the sample, each with a discrete superconducting transition temperature (T c ). Notably, samples with higher T c only show a single transition at ambient pressure. Above 0.3 GPa, however, two transitions are invariably observed in ac calorimetry. Our results not only point to a nearly vertical line (constant pressure) in the pressure-temperature phase diagram but also provide a consistent scenario for the sample dependence of UTe 2 .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Benefits of MeV-scale reconstruction capabilities in large liquid argon time projection chambers

Using truth-level Monte Carlo simulations of particle interactions in a large volume of liquid argon, we demonstrate physics capabilities enabled by reconstruction of topologically compact and isolated low-energy features, or “blips,” in large liquid argon time projection chamber (LArTPC) events. These features are mostly produced by electron products of photon interactions depositing ionization energy. The blip identification capability of the LArTPC is enabled by its unique combination of size, position resolution precision, and low energy thresholds. Here, we show that consideration of reconstructed blips in LArTPC physics analyses can result in substantial improvements in calorimetry for neutrino and new physics interactions and for final-state particles ranging in energy from the MeV to the GeV scale. Blip activity analysis is also shown to enable discrimination between interaction channels and final-state particle types. In addition to demonstrating these gains in calorimetry and discrimination, some limitations of blip reconstruction capabilities and physics outcomes are also discussed.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2021

Effects of Al:Si and (Al + Na):Si ratios on the properties of the international simple glass, part I: Physical properties

Understanding composition-structure-property relationships of high-alumina nuclear waste glasses are important for vitrification of nuclear waste at the Hanford Site. Two series of glasses were designed, one with varying Al:Si ratios and the other with (Al+Na):Si ratios based on the International Simple Glass (ISG, a simplified nuclear waste model glass), with Al2O3 ranging from 0 to 23 mol % (0 to 32 wt. %). The glasses were synthesized and characterized using electron probe microanalysis, X-ray photoelectron spectroscopy, small angle X-ray scattering, high temperature oxide melt solution calorimetry, and infrared spectroscopy. Glasses were crystal free, and the lowest Na2O and Al2O3 glass formed an immiscible glass phase. Evolution of various properties - glass transition temperature, percentage of 4-coordinated B, enthalpy of glass formation - and infrared spectroscopy results indicate that structural effects differ based on the glass series.

Nuclear Waste Glass↗

DOE OSTI2024

Formation kinetics and thermodynamic stability of the Aurivillius compounds in Bi 4 Ti 3 O 12 –BiFeO 3 system

Abstract The Aurivillius compounds in the Bi 2 O 3 –Fe 2 O 3 –TiO 2 system, combining ferroelectric, semiconducting, and ferromagnetic properties, have attracted particular interest. Formation kinetics and thermodynamic stability are the fundamental knowledge needed for modeling and predicting the temporal microstructure and property evolution during materials processing but have not yet been addressed by quantitative experimental measurement. This article focuses on the Bi n +1 Fe n –3 Ti 3 O 3 n +3 Aurivillius compounds on the Bi 4 Ti 3 O 12 –BiFeO 3 tie‐line to elucidate the mechanisms and thermodynamic controls responsible for phase formation of compounds with various perovskite‐like layers. Five high‐purity Aurivillius compounds Bi 4 Ti 3 O 12 , Bi 5 FeTi 3 O 15 , Bi 6 Fe 2 Ti 3 O 18 , Bi 7 Fe 3 Ti 3 O 21 , and Bi 8 Fe 4 Ti 3 O 24 with integer n = 3–7 values were synthesized and their phase transformation properties and enthalpies of formation were studied by X‐ray diffraction in situ, high temperature differential scanning calorimetry, and high temperature oxide melt solution calorimetry. Thermodynamic stability of the compounds decreases with increasing n , and formation kinetics gradually slow down, demonstrating the inherent difficulty to synthesize pure Aurivillius compounds with n larger than 8. This difficulty was confirmed by an impurity phase coexisting with Bi 9 Fe 5 Ti 3 O 27 .

Gong, Weiping↗

DOE OSTI2025

Impact of Testing Method on Safety Assessment of Aged Li-Ion Cells: Part II – Aged Cells Without Li Plating

Understanding the safety profile of aged Li-ion batteries is essential for developing effective battery management and hazard mitigation strategies. However, most safety assessments have focused on fresh batteries, with just a few calorimetry studies on aged batteries with metal oxide positive electrodes. This study provides a broad assessment of commercial 18650-type Li-ion batteries with NCA, NMC, and LFP positive electrodes, both uncycled and aged under conditions that promoted solid electrolyte interphase (SEI) growth as the dominant degradation mechanism. The cells underwent mechanical (nail penetration, crush), electrical (overcharge, overdischarge), and thermal (accelerating rate calorimetry) abuse tests. Safety was rated on general characteristics such as mass loss, maximum temperature, and EUCAR (European Council for Automotive R&D) hazard level, as well as characteristics specific to individual abuse tests. Generally, aged cells with SEI growth exhibited similar or improved safety compared to uncycled cells, contrasting with our previous findings on NCA cells with Li plating as the dominant aging mechanism (Part I of this series). Yet, some tests and characteristics indicated reduced aged cell safety, such as earlier triggering of mechanical failure. These results emphasize the need to examine aged battery safety across diverse empirical techniques, degradation modes, and chemistries.

Lithium-ion cells↗

DOE OSTI2024

Fluoropolymer Aging Phenomena

This project aims to investigate structural and morphological changes in fluoropolymers induced by both processing and aging phenomena such as heat, time, and irradiation. Fluoropolymers are an important class of thermoplastics that are broadly used in industry as o-rings and seals when chemical resistance and thermal performance are important. They are also often used in thin film geometries as binders in batteries, insulation layers, water barriers, and anti-fouling coatings. For all of these applications, mechanical integrity and aging are important aspects of their use. Changes in the crystalline morphology are known to impact the mechanical properties of the polymer and can lead to failure. The broad goals of this project are to correlate compositional changes, morphological changes, and mechanical changes. report focuses on the morphological changes that are correlated with nuclear magnetic resonance (NMR), calorimetry and mechanical testing. We plan to compare structure and morphology measurements across complementary bulk and surface techniques. We use in situ atomic force microscopy (AFM) to measure domain shape and crystallization kinetics; in situ NMR to measure crystalline composition; and differential scanning calorimetry (DSC) to measure melting temperatures.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Functional Data Analysis in Wearable Body Sensor Networks

Improving response time of indirect room-size calorimeters is still an outstanding problem in metabolic research. Accurate estimates of instantaneous rates of gaseous exchange require numerical differentiation of measured gaseousgas concentrations. We propose a new method to estimate the instantaneous gaseousgas exchange rates in indirect calorimetry. In contrast to the previously developed techniques, the method addresses the problem of differentiation of gaseous concentrations as an ill-posed problem. By applying the method of regularization, the problem of differentiation is converted into a well-posed problem resulting in smooth and consistent gaseous exchange rates. The validity of the method is tested on a large dataset of calorimeter experiments which included 313 human experiments along with 231 alcohol combustion experiments. It is demonstrated that the method is able to reliably differentiate between the “unphysiological” process of alcohol combustion and physiological variations produced by human metabolism. The method also allowed unraveling the previously unreported relative kinetics of O2 consumption and Respiratory Quotient (RQ) in humans. It was found that the kinetics of oxidative fuel selection lags behind the energy expenditure in humans exhibiting some sort of oxidative inertia. The time lag varies from 2-3 min up to 30 min, depending on particular individual. No such lag was found in alcohol combustion experiments. In addition to the relative kinetics of substrate oxidation, two statistical indexes reflecting variability of minute-by-minute RQ were estimated. The indexes were the RQ’s standard deviation and RQ’s first-order derivative. Both indexes showed statistically significant difference between human experiments and alcohol combustion experiments. We conclude that the proposed method can consistently extract physiologically-relevant information from noisy calorimetry data and the aforesaid information can provide additional insights into the mechanism of metabolic fuel selection in humans.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Energy Reconstruction and Calibration of the MicroBooNE LArTPC

MicroBooNE uses a liquid argon time projection chamber (LArTPC) for simultaneous tracking and calorimetry. Neutrino oscillation experiments plan to use LArTPCs over the next several decades. A challenge for these current and future experiments lies in characterizing detector performance and reconstruction capabilities with thorough associated systematic uncertainties. This work includes updates related to LArTPC detector physics challenges by reviewing MicroBooNE’s recent publications on calorimetry and its applications. Highlights include discussions on signal processing, calorimetric calibration, and particle identification.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2021

Chapmanite [Fe 2 Sb(Si 2 O 5 )O 3 (OH)]: thermodynamic properties and formation in low-temperature environments

Abstract. of synthetic Sb 2 O 5 , MgSb 2 O 6 (analogue of the mineral byströmite), Mg[Sb(OH) 6 ] 2 ∙6H 2 O (brandholzite), and natural chapmanite [(Fe 1.88 Al 0.12 )Sb(Si 2 O 5 )O 3 (OH)]. Enthalpies of reactions, including formation enthalpies, were evaluated using reference compounds Sb, Sb 2 O 3 , Sb 2 O 5 , and other phases, with high-temperature oxide melt solution calorimetry in lead borate and sodium molybdate solvents. Heat capacity and entropy were determined by relaxation and differential scanning calorimetry. The best set of Δ f H o (kJ mol -1 ) and S o (J mol -1 K -1 ) is byströmite -1733.0±3.6, 139.3±1.0; brandholzite -5243.1±3.6, 571.0±4.0; and chapmanite -3164.9±4.7, 305.1±2.1. The data for chapmanite give Δ f G o of -2973.6±4.7 kJ mol -1 and log K=-17.10 for the dissolution reaction (Fe 1.88 Al 0.12 )Sb(Si 2 O 5 )O 3 (OH) + 6H + → 1.88Fe 3+ + 0.12Al 3+ + 2SiO$_2^0$ + Sb(OH)$_3^0$ + 2H 2 O. Analysis of the data showed that chapmanite is finely balanced in terms of its stability with schafarzikite (FeSb 2 O 4 ) and tripuhyite (FeSbO 4 ) under a specific, narrow range of conditions when both aqueous Fe(III) and Sb(III) are abundant. In such a model, chapmanite is metastable by a narrow margin but could be stabilized by high SiO$_2^0$(aq) activities. Natural assemblages of chapmanite commonly contain abundant amorphous silica, suggesting that this mechanism may be indeed responsible for the formation of chapmanite. Chapmanite probably forms during low-temperature hydrothermal overprint of pre-existing Sb ores under moderately reducing conditions; the slightly elevated temperatures may help to overcome the kinetic barrier for its crystallization. During weathering, sheet silicates may adsorb Sb 3+ in tridentate hexanuclear fashion, thus exposing their chapmanite-like surfaces to the surrounding aqueous environment. Formation of chapmanite, as many other sheet silicates, under ambient conditions, is unlikely.

58 GEOSCIENCES↗

NASA NTRS1974

Cycles in metabolism and heat loss

Using calorimetric techniques, subjects' metabolism, thermoregulation, and body temperatures were monitored continuously for 24-hour days, using three types of experimental routines. A water cooling garment (WCG) was used for direct calorimetry, while partitional calorimetry was used to establish a non-suited comparison for one of the routines. In this replicated routine, called the quiet day, the subjects were sedentary throughout the daytime hours and slept normally at night. Results indicate that the WCG may act to reduce 24-hour total oxygen consumption (VO2) or heat production, possibly due to the lowered energy cost of thermoregulation.

Annis, J. F.↗

NASA NTRS1974

An evaluation: The potential of discarded tires as a source of fuel

Collins, L. W.↗

NASA NTRS1974

An evaluation of discarded tires as a potential source of fuel

The destructive distillation of rubber tire samples was studied by thermogravimetry, differential scanning calorimetry, combustion calorimetry, and mass spectroscopy. The decomposition reaction was found to be exothermic and produced a mass loss of 65%. The products from the distillation process were a solid residue with a heating value of about -30 MJ/kg, a liquid with a heating value of about -40 MJ/kg, and a combustible gas of undetermined heating value. The gas evolution curves which were obtained indicate that a variety of organic materials are evolved simultaneously during decomposition of the rubber polymer.

Collins, L. W.↗

NASA NTRS1982

Development of quality assurance methods for epoxy graphite prepreg

Quality assurance methods for graphite epoxy/prepregs were developed. Liquid chromatography, differential scanning calorimetry, and gel permeation chromatography were investigated. These methods were applied to a second prepreg system. The resin matrix formulation was correlated with mechanical properties. Dynamic mechanical analysis and fracture toughness methods were investigated. The chromatography and calorimetry techniques were all successfully developed as quality assurance methods for graphite epoxy prepregs. The liquid chromatography method was the most sensitive to changes in resin formulation. The were also successfully applied to the second prepreg system.

Chen, J. S.↗

NASA NTRS1990

Small scale demand type neon liquefaction plant

Low-temperature measurement of the thermal conductivity of insulating materials is generally made using a boil-off calorimetry technique involving liquid hydrogen (LH2). Liquid neon (LNe) has nearly the same normal boiling point as LH2, but has a much larger heat of vaporization, allowing extended run times. The main drawback of using LNe has been its excessive cost; $170.00 versus $1.50/l for LH2 (1989 prices). A neon liquefaction plant has been designed and constructed to capture, purify, and refrigerate the neon boil-off from calorimetry experiments. Recycling the neon reduces operating costs to approximately $20/l. The system consists of a purification section, a heat exchanger, LNe and LH2 storage dewars, and a fully automated control system. After purification, neon is liquified in the heat exchanger by LH2 flowing countercurrently through stainless steel cooling coils. Hydrogen flow is automatically adjusted to keep the neon at its normal saturation temperature, 27 K. The liquid neon is then stored in a dewar placed directly below the heat exchanger.

Dube, W. P.↗

NASA NTRS1994

Perfluoropolyalkylether decomposition on catalytic aluminas

The decomposition of Fomblin Z25, a commercial perfluoropolyalkylether liquid lubricant, was studied using the Penn State Micro-oxidation Test, and a thermal gravimetric/differential scanning calorimetry unit. The micro-oxidation test was conducted using 440C stainless steel and pure iron metal catalyst specimens, whereas the thermal gravimetric/differential scanning calorimetry tests were conducted using catalytic alumina pellets. Analysis of the thermal data, high pressure liquid chromatography data, and x-ray photoelectron spectroscopy data support evidence that there are two different decomposition mechanisms for Fomblin Z25, and that reductive sites on the catalytic surfaces are responsible for the decomposition of Fomblin Z25.

Morales, Wilfredo↗