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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Combining Fractional Calorimetry with Statistical Methods to Characterize Thermal Runaway
Thermal management systems designed to handle the impacts of thermal runaway (TR) are key to safe operation of lithium-ion (Li-ion) batteries. Critical factors for optimizing these systems include the total energy released and the fraction of the total energy that is released through the cell casing versus through the ejecta material. A unique calorimeter, designed to characterize said factors, was utilized to examine the TR behavior of a variety of 18650-format Li-ion cells. Statistical methods were implemented to interpret the data.
Coupling Fractional Thermal Runaway Calorimetry (FTRC) Results with Statistical Analysis Methods
Important factors to consider when optimizing Lithium-ion (Li-ion) battery thermal management systems, from a battery safety perspective, include the total energy released during a single cell thermal runaway (TR) event and the fraction of the total energy that is released through the cell casing versus through the ejecta material. A fractional thermal runaway calorimeter (FTRC) was used to examine the TR behavior of the following 18650-format Li-ion cells: (1) Molicel 18650-J, (2) LG 18650-HG2, (3) Samsung 18650-30Q, (4) 3.35 Ah LG 18650 test cell, (5) Sony 18650-VC7, and (6) LG 18650-MJ1. These cells were intentionally selected to represent a variety of manufacturers, chemistries, capacities, and safety features. Because of the large number of random and non-random variables associated with the FTRC results, a linear regression model, developed using engineering statistical methods, was utilized to provide final interpretation of the TR behavior for each cell type and design variable combination.
Miniaturized Laser Absorption Spectrometer for Combustion Calorimetry and Process Monitoring
A miniaturized tunable laser absorption spectrometer capable of measuring gas-phase concentrations of CO, CO2, and O2 has been developed for operation in spacecraft environments. As part of the Spacecraft Fire Safety Demonstration (Saffire) project, we previously demonstrated the Combustion Product Monitor (CPM) instrument to characterize pyrolysis of relevant test materials in low gravity aboard a transfer vehicle returning from low Earth orbit. Here, we adapted the CPM instrument design to achieve detection of CO, CO2, and O2 with improved minimum detection limits and dynamic range as well as reduced instrument size and power. The instrument can be operated in either an open or sealed configureation, allowing for ambient gas composition measuremnts or in-line monitoring of gas streams. By accurately monitoring CO, CO2, and O2 with broad pressure/temperature calibration and response time on the order of 1 s, the instrument can be used to characterize the dynamics of combustion reactions in a variety of environments.
Fractional Thermal Runaway Calorimetry (FTRC)
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A Boiloff Calorimetry Test Configuration for the Characterization of Thermal Insulation Systems in Flammable Background Gasses
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Low Cost Manufacturing of Ceramic Scintillator for HEP Calorimetry (Final Report)
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Readout for Calorimetry at Future Colliders: A Snowmass 2021 White Paper
Calorimeters will provide critical measurements at future collider detectors. As the traditional challenge of high dynamic range, high precision, and high readout rates for signal amplitudes is compounded by increasing granularity and precision timing the readout systems will become increasingly complex. This white paper reviews the challenges and opportunities in calorimeter readout at future collider detectors.
Applying Calorimetry Measurements to Determine Plutonium Mass Using a Thermal Camera and Infrared Thermometer
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Experimental Techniques for Thermodynamic Measurements of Ceramics
Experimental techniques for thermodynamic measurements on ceramic materials are reviewed. For total molar quantities, calorimetry is used. Total enthalpies are determined with combustion calorimetry or solution calorimetry. Heat capacities and entropies are determined with drop calorimetry, differential thermal methods, and adiabatic calorimetry . Three major techniques for determining partial molar quantities are discussed. These are gas equilibration techniques, Knudsen cell methods, and electrochemical techniques. Throughout this report, issues unique to ceramics are emphasized. Ceramic materials encompass a wide range of stabilities and this must be considered. In general data at high temperatures is required and the need for inert container materials presents a particular challenge.
Calorimetric determination of thermal parameters for the Li/BrCl in SOCl2 (BCX) chemistry
The heat capacity of a Li-BCX DD-cell was found to be dependent on its state of charge by drop calorimetry measurements. The method of drop calorimetry involves measuring the energy (joules) gained or lost from a sample that is transferred from a bath at temperature A to one at temperature B. The thermoneutral potential is defined as the cell potential where the cell electrochemical reactions are neither exothermic nor endothermic. A Hart scientific calorimeter system, Model No. S77XX, designed for heat conduction calorimetry and drop calorimetry was used. Calorimetric analysis yielded a thermoneutral potential of 4.14 volts and a cell heat capacity dependent on the state of charge.
Calorimetric metal vapor adsorption energies for characterizing industrial catalyst support materials
Many important catalysts and electro-catalysts for energy and environmental technologies involve late transition metal atoms and nanoparticles dispersed across the surface of high-surface-area support materials, for example, oxide nanoparticles. The surface reactivity and long-term stability against deactivation of these materials depends strongly on the strength of bonding of the metal atom and nanoparticles to the support surface. Here, we introduce a novel calorimetry method that implements a LiTaO 3 crystal for heat detection and extends metal adsorption calorimetry to surfaces of nanomaterials that are deposited from liquid solutions, as is typical when preparing industrial catalyst supports. This allows one to measure the strength of metal atom bonding and the adhesion energy of metal nanoparticles to clean surfaces of technologically relevant catalyst supports. We demonstrate that here by measuring the heat of Ag vapor adsorption onto the clean surfaces of high-surface-area TiO 2 anatase powdered support materials (i.e., 5-nm-diameter nanoparticles). These heats of adsorption show a pulse-to-pulse standard deviation of only 9.3 kJ/mol (3.3%) for pulses containing only 1% of a monolayer of Ag vapor, with potential for a 5-fold reduction in noise if used with another metal evaporator. The calorimeter was also proven to work well measuring heats of Ag adsorption on calcium niobate(001) nanosheets deposited as thin films from liquid solution. Here, this calorimeter opens up the possibility of using metal adsorption calorimetry to screen catalyst support materials for the strengths with which they bind metal atoms and metal nanoparticles, offering new opportunities to discover better support materials or for basic scientific study of structure / function relationships with respect to metal / support bond energies.
Low- and high-temperature heat capacity of metallic technetium
The heat capacity of technetium metal has been measured from 2.1 K to 293 K using relaxation calorimetry and the enthalpy increment up to 1700 K using drop calorimetry. The low-temperature calorimetry measurements revealed a superconducting transition temperature of T C = (7.76 ± 0.08) K. The zero-degree Debye temperature(θ E ) and the electronic heat capacity coefficient ($γ_{e}$) of the normal state were derived as (307 ± 5) K and (4.22 ± 0.20) mJ·K –2 ·mol –1 , respectively. The standard entropy of the superconducting standard state was derived as $S^{°}_{m}$ (298.15) = (36.8 ± 1.3) J·K –1 ·mol –1 . The fitting of enthalpy-increment data together with high-temperature heat capacity data reported in literature yielded a heat capacity equation up to 1700 K.
Energetics of oxidation and formation of uranium monocarbide
To enable better implementation of uranium monocarbide (UC) as an advanced nuclear fuel for future high-temperature reactors, it is essential to have a thorough knowledge of its thermal and thermodynamic properties under reactor operational conditions. In this work, we studied thermal bulk oxidation of UC by simultaneous thermal analysis consisting of thermogravimetric analysis – differential scanning calorimetry coupled with evolved gas mass spectrometry (TGA-DSC-MS), and we examined the thermodynamic stability of UC using high temperature oxide melt drop solution calorimetry. Further, in air, our studied UC sample (which contains ~5 mol% UO 2 ) was found to undergo a step-wise thermal oxidation process consisting of consecutive oxidations and thermal decomposition reactions: 0.95UC·0.05UO 2 → UO 3 ·0.29(C x O y ) + 0.66CO 2 → UO 3 ·0.20(C x O y ) + 0.09CO 2 → UO 3 ·0.03(C x O y ) + 0.17CO 2 → U 3 O 8 + 0.03CO 2 + 0.166O 2 . DSC was further used to determine the enthalpies of reactions associated with this series of oxidation reactions. Synchrotron X-ray diffraction (XRD) and extended X-ray absorption spectroscopy (EXAFS) were performed to characterize both the long- and short-range structures of UC. The standard enthalpy of formation (ΔH° f ) of UC was determined to be –50.7 ± 10.8 kJ/mol·atom, in good agreement with previous values measured by bomb calorimetry. Lastly, the enthalpic landscape of U-C compounds, including UC, U 2 C 3 , and α-UC 1.94 , were established based on the enthalpy normalized per mole atom, which suggests that U-C phases are thermodynamically stable at lower C/U ratios.
Identifying Molecular Scale Interactions of Nucleating Agents with Salt Hydrates for Thermal Energy Storage Applications
Latent heat based thermal energy storage is of interest as a method to mitigate and time-shift thermal load peaks and hence reduce energy demands for heating and cooling buildings. Notably, Glauber’s salt (GS) presents a good choice as a phase change material (PCM) for building applications because it has a melting point near room temperature (i.e., 32.4 °C), a large heat of fusion and energy density, and is low cost (~ $100/ton). However, there are several known limitations to using GS as a PCM, such as incongruent melting, high degree of supercooling, and formation of other hydration states, which renders GS unsuitable for practical use. Inorganic crystals acting as nucleating agents can avoid some of these issues with GS [1]. Understanding nucleation behavior through typical calorimetry experiments offers limited insight into the molecular-scale mechanisms. Here, we report isothermal titration calorimetry [2] to investigate the interactions between sodium sulfate salt and an organic nucleating agent - glycine. Our experiments provide qualitative and quantitative understanding of how glycine interacts with sodium sulfate across various temperatures. The findings offer insights into the nucleation onset temperature (24°C) and underscore the pivotal role of glycine's zwitterionic structure in facilitating nucleation. This preliminary work provides a foundation for subsequent exploration of nucleating agents that would be incorporated in different salt hydrate systems. 1. Purohit, B. K., and V. S. Sistla. "Inorganic salt hydrate for thermal energy storage application: A review." Energy Storage 3, no. 2 (2021): e212. 2. Velázquez-Campoy, Adrián, Hiroyasu Ohtaka, Azin Nezami, Salman Muzammil, and Ernesto Freire. "Isothermal titration calorimetry." Current protocols in cell biology 23, no. 1 (2004): 17-8.
Estimation of Sorption Behavior of Europium to Calcium Silicate Hydrate by Thermal Analysis - 20172
High-level radioactive waste generated from reprocessing processes will be disposed in a geological disposal that is deep underground. Calcium silicate hydrate is formed as a secondary mineral in the repository via the reaction of calcium ions leaching from the cement and the silicic acid dissolved from the host rocks. In this study, the sorption behavior of europium, which is also known as a chemical analog of americium, on calcium silicate hydrate was examined. The solid phase was analyzed via thermogravimetry- differential thermal analysis, differential scanning calorimetry, Raman spectroscopy, fluorescence spectroscopy, and fluorescence lifetime analysis. To understand the behavior of calcium silicate hydrate under conditions saturated with groundwater, the study samples were analyzed using the above methods, except for deferential scanning calorimetry, without a drying process. The results of the differential scanning calorimetry analyses showed that the temperatures for the endothermic peaks of calcium silicate hydrate for the lower Ca/Si ratios were larger than those for the higher Ca/Si ratios for coexistent conditions of europium ions. Hence, the relationships of the temperatures of the endothermic peaks and the Ca/Si ratios were reversed by the addition of europium ions. These study results suggest that calcium silicate hydrate can immobilize europium ions, thus preventing the production of colloidal forms. (authors)