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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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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Measurement of partial vapor pressures of salt mixtures via combined horizontal transpiration and thermogravimetric analysis

A method combining thermogravimetric analysis (TGA) and horizontal transpiration with elemental analysis via inductively coupled plasma mass spectrometry or ion chromatography enabled calculation of partial pressures of individual salts in molten mixtures. TGA quantified total mass loss, while transpiration identified vapor-phase composition. Furthermore, two chloride (NaCl-MgCl 2 , NaCl-MgCl 2 + UCl 3 ) salts and one mixed halide (LiCl-LiF + Li 2 O) salt were analyzed at 750 °C and 550 °C, respectively. NaCl and MgCl 2 vapor pressures were 2.19–2.61 × 10 -4 atm and 2.47–2.48 × 10 -5 atm (dependent upon the identity of the invesitgated mixture); UCl 3 was 1.42 × 10 -7 atm. LiCl and LiF vapor pressures at 550 °C were 1.53 × 10 -6 and 6.32 × 10 -6 atm, respectively. Additionally, the TGA method was validated against values from the literature for unary LiCl and LiF.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Thermogravimetric Analysis (TGA) for Carbon Fiber and Glass Fiber Epoxy Composites and their Constituents

In this work, thermogravimetric analysis (TGA) was performed on samples of a carbon fiber epoxy composite, a glass fiber epoxy composite, and a mixed carbon fiber/glass fiber epoxy composite, as well on each constituent material (polymer epoxy, carbon fibers and glass fibers). TGA was conducted for heating rates from 1-20 C/min with purified purge gases of nitrogen and dry air. For the fiberglass composite, we find that ~70% of the material remains after heating in air to 1200 C. For the carbon fiber epoxy composite, we observe greater mass loss as the carbon fibers can oxidize, leaving little material by the end of the test. The mixed composite, which has a 2:1 ratio of glass fibers to carbon fibers, experienced a total mass loss between the two other composites. By determining the relationship between the thermal decomposition of a composite material and its constituent materials, we can predict the fire behavior of novel composites during the material design phase.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Parts-Per-Million Carbonate Mineral Quantification with Thermogravimetric Analysis–Mass Spectrometry

Mitigating the deleterious effects of climate change requires the development and implementation of carbon capture and storage technologies. To expand the monitoring, verification, and reporting (MRV) capabilities of geologic carbon mineralization projects, we developed a thermogravimetric analysis–mass spectrometry (TGA–MS) methodology to enable quantification of <100 ppm calcite (CaCO 3 ) in complex samples. We extended TGA–MS calcite calibration curves to enable a higher measurement resolution and lower limits of quantification for evolved CO 2 from a calcite–corundum mixture. We demonstrated <100 ppm carbonate mineral quantification with TGA–MS for the first time, an outcome applicable across earth, environmental, and materials science fields. We applied this carbonate quantification method to a suite of Columbia River Basalt Group (CRBG) well cuttings recovered in 2009 from Pacific Northwest National Laboratory’s Wallula #1 Well. Our execution of this new combined calcite and calcite–corundum calibration curve TGA–MS method on our CRBG sample suite indicated average carbonate contents of 0.050 wt % in flow interiors (caprocks) and 0.400 wt % in interflow zones (reservoirs) in the upper 1250 m of the Wallula #1 Well. Finally, by advancing our knowledge of continental flood basalt-hosted carbonates in the mafic subsurface and reaching new TGA–MS quantification limits for carbonate minerals, we expand MRV capabilities and support the commercial-scale deployment of carbon mineralization projects in the Pacific Northwest United States and beyond.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Proxy quality control of biomass particles using thermogravimetric analysis and Gaussian process regression models

Abstract The temperature experienced by reactants during preparation in a reactor is a key component in determining the yield and homogeneity of usable chemical products such as biomass particles. Thermocouples with sensors can be used to monitor spatial temperature gradients within reactors but these sensors are often too expensive and/or invasive. The present work proposes a strategy to identify optimal machine learning models to infer the maximum effective temperature experienced by particles during oxidative biomass torrefaction using key thermochemical combustion parameters. The maximum rate of weight loss, the corresponding temperature, and fixed carbon content on a dry‐ash‐free basis are used as literature‐based predictor variables obtained from thermogravimetric analysis. The evaluation of 24 machine‐learning models using the standard tenfold cross‐validation method suggests that the exponential Gaussian process regression (GPR) model is the most effective, followed by other GPR models. These high‐performing GPR models were also utilized to predict the effective preparation temperature distribution of reactor‐produced biomass particles under eight conditions of varying residence time and air‐to‐biomass ratio. The effective preparation temperature and residence time of individual biomass particles were then encoded into the torrefaction severity factor and used to estimate the energy yield of the reactor output as a novel quality control method. © 2023 The Authors. Biofuels, Bioproducts and Biorefining published by Society of Industrial Chemistry and John Wiley & Sons Ltd.

09 BIOMASS FUELS↗
DOE OSTI2024

Adsorption of molecular iodine and alkyl iodides from spent-nuclear-fuel-reprocessing off-gas using reduced silver mordenite

Radioactive iodine is a hazardous byproduct of spent-nuclear-fuel reprocessing that must be removed from the off-gas stream before it can be discharged. Reduced silver mordenite (Ag 0 Z) is currently the baseline material for iodine capture in the U.S. Although the performance characteristics and capture mechanisms of I 2 and CH 3 I have been established, similar investigations into long-chain organic iodides have yet to be performed. In this study, thin beds of Ag 0 Z were loaded with I 2 , CH 3 I, C 4 H 9 I, and C 12 H 25 I (5 ppm to 50 ppm) carried in a dry air stream at 150°C. The maximum iodine capacity was 105 ± 5 mg I/g Ag 0 Z for all species. Saturated Ag 0 Z samples were characterized using scanning electron microscopy, X-ray fluorescence, X-ray photoelectron spectroscopy, diffuse reflectance UV–visible spectroscopy, pair distribution function analysis, and thermogravimetric analysis. Further, near-complete Ag utilization and similar physical/chemical properties were observed for all samples. Through a comparison with previous studies and an investigation of aged Ag 0 Z, we propose that iodine species react with Ag + at exchange sites, forming α-AgI within the mordenite channels, and with surface Ag 0 nanoparticles, yielding β-/γ-AgI. The available Ag sites in the interior (Ag + ) and exterior (Ag 0 ) of mordenite determine the adsorption capacity since α-AgI formation is limited by the total pore volume. Potential iodine uptake routes were summarized for aging and non-aging environments. A scalable predictive model was implemented for deep-bed iodine removal, and predictions were in good agreement with experimental data. Sensitivity analysis suggests that iodine uptake kinetics is governed by pore diffusion.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Syntheses and crystal structures of four new d 0 transition metal tellurites

Four new d 0 transition metal tellurites, namely InVTeO 6 (1), β-InVTe 2 O 8 (2), FeVTe 2 O 8 (3), and Fe 2 MoTe 2 O 10 (4), were synthesized under hydrothermal conditions, and their crystal structures were determined using single-crystal X-ray diffraction. Compound 1 crystallizes in the noncentrosymmetric space group P2 1 2 1 2 1 (No. 19), with unit cell parameters of a = 5.0759(2) Å, b = 8.5030(3) Å, c = 11.6376(5) Å, V = 502.28(3) Å 3 , and Z = 4, while the other three compounds crystallize in centrosymmetric structures, with space group Cmca and unit cell parameters of a = 7.0633(7) Å, b = 8.962(1) Å, c = 20.162(2) Å, V = 1276.3(2) Å 3 , and Z = 8 for compound 2, space group P2 1 /n and unit cell parameters of a = 7.8901(2) Å, b = 4.9617(1) Å, c = 16.4290(3) Å, β = 93.6198(8)°, V = 641.88(2) Å 3 , and Z = 4 for compound 3, and space group Pnma and unit cell parameters of a = 8.7878(2) Å, b = 6.1327(2) Å, c = 15.2423(4) Å, V = 821.45(4) Å 3 , and Z = 4 for compound 4. Compound 3 adopts a two-dimensional (2D) sheet structure composed of FeO 6 octahedra, VO 4 tetrahedra, and TeO 4 polyhedra. The other three compounds exhibit three-dimensional (3D) framework structures: Compound 1 is built from InO 6 octahedra, VO 4 tetrahedra, TeO 4 polyhedra; Compound 2 consists of InO 6 octahedra, VO 5 square pyramids, and TeO 3 polyhedra; and Compound 4 is composed of FeO 6 octahedra, MoO 6 octahedra, and TeO 3 polyhedra. The band structures, density of states, and electron localization functions of all four compounds were calculated. The vibrational spectra were examined for compounds 1, 2, and 4. Furthermore, powder X-ray diffraction, element analysis, and thermogravimetric analysis were conducted for compound 4.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Simultaneous Thermal Analysis of Anion and Cation Exchange Resins

The decomposition reactions of one anion exchange resin (Bio-Rad AG MP-1) and one cerium-loaded cation exchange resin (DOWEX 50W-X8), both in nitrate form, were analyzed using simultaneous thermal analysis methods. Thermogravimetric analysis, dynamic scanning calorimetry, and evolved gas analysis were deployed in combination to probe the temperature profiles, reaction enthalpies, and off-gases from these resins under process-relevant temperature ranges. Analysis indicates that both resins undergo three clear phases during heating. The first is a dehydration step with prominent off-gassing of water, the second is a decomposition step with evolution of several gaseous species, and lastly is a combustion step with a large release of CO 2 . The temperature at which combustion ends varies slightly between AG MP-1 and DOWEX 50W: combustion completed at ~690°C and ~810°C, respectively. For the DOWEX cation resin, the combustion reaction showed greater sensitivity to the availability of oxygen under the test conditions. Both resins displayed broad exotherms during the combustion step of the decomposition, but the DOWEX cation resin demonstrated a 4.5 times higher specific enthalpy than that of the AG MP-1.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Grain size dependence of thermally induced oxidation in zirconium carbide

Here complementary analytical approaches were employed to probe the effect of grain size on thermally induced oxidation of zirconium carbide (ZrC) utilizing thermogravimetric analysis, differential scanning calorimetry, and Raman spectroscopy, as well as synchrotron-based and laboratory-based X-ray diffraction (XRD) experiments. The oxidation mechanism and phase behavior of nanocrystalline ZrC (grain size ~ 20 nm) were compared with that of the more documented microcrystalline ZrC (grain size ~ 1 µm). Synchrotron XRD at the Advanced Photon Source with a hydrothermal diamond anvil cell (HDAC) used as a sample chamber revealed that the onset of oxidation is at ~ 380 °C for microcrystalline ZrC which is in agreement with previous work. In contrast, the critical oxidation temperature was ~ 330 °C for nanocrystalline ZrC. Additional high-temperature synchrotron XRD experiments at the National Synchrotron Light Source II using a lamp furnace in combination with Raman analysis showed that tetragonal ZrO 2 forms as an initial oxidation product and transforms at higher temperatures to the monoclinic phase. Thermogravimetric analysis (TGA) coupled with differential scanning calorimetry (DSC) confirmed the X-ray results of a lower critical oxidation temperature for the nanocrystalline sample. The phase transformations in the oxide phase with associated critical temperatures were also evident in the thermodynamic data as exothermic heat events.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

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.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Characterization of Aluminum Metal Powders for Plutonium-238 Program

As part of radioisotope thermoelectric generator (RTG) production for power sources in deep space exploration, Oak Ridge National Laboratory (ORNL) produces plutonium-238 ( 238 Pu). To produce 238 Pu, neptunium-237 ( 237 Np) targets are fabricated at ORNL and subsequently irradiated at the High Flux Isotope Reactor (HFIR) at ORNL and the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL). Specifically, current flowsheets utilize neptunium dioxide ( 237 NpO 2 ) targets. Aluminum (Al) powder is blended with 237 NpO 2 target material to improve thermal conductivity during irradiation. The current composition of 237 NpO 2 /Al pellets (i.e., cermets, or ceramic–metallics) is 20% 237 NpO 2 , 70% Al, and 10% void space. Al powders utilized by the 238 Pu program are high-fired under vacuum before blending into targets. The primary objective of this work is to measure the physical, chemical, and thermal properties of Al before and after the high-firing process. Properties of interest include the morphology, surface texture, particle size, crystal phase(s), and thermal conductivity of the material. These properties are measured with existing materials characterization equipment at ORNL, including powder x-ray diffraction (pXRD), scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS), laser flash analysis (LFA), and thermogravimetric analysis (TGA). A secondary objective of this work is to compare the Al powders before and after the high-firing procedure to determine the effects of high-firing on chemical, physical, and thermal properties and to determine the efficacy of the high-firing process.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Microwave-Assisted Catalytic Conversion of Tar Using Iron Catalyst Doped with Ni/La/Ce

The goal of this research is to study the microwave-assisted catalytic dry reforming of toluene using Fe/Al2O3 as a catalyst in the presence of various dopants such as Ni/La/Ce in a conventional fixed-bed reactor. Initial studies show that both CO2 and toluene conversion can be achieved up to 85% at 500 °C. Higher toluene conversion and syngas production was achieved under microwave conditions compared to conventional thermal conditions. The pre and post-reaction catalyst characterizations were performed using X-ray diffraction analysis (XRD) and thermogravimetric analysis (TGA). The tar analysis was performed using gas chromatography–mass spectrometry (GC-MS). The product gas mainly consisted of H2, CO, methane, propane, ethylene, and ethane along with small amounts of benzene, and naphthalene. The production of benzene indicates the hydrodemethylation (HDM) process of toluene, which requires hydrogen to initiate the reaction. The reaction pathway was proposed based on the observed product gas.

Linge Gowda, Anitha Shankara↗
DOE OSTI2024

Development and Characterization of Densified Biomass-plastic Blend for Entrained Flow Gasification (Final Technical Report)

Supported by the U.S. DOE NETL Award DE-FE0032043, this project was a collaborative effort. Project participants included the University of Kentucky Institute for Decarbonization and Energy Advancement (UK IDEA), Biosystems and Agricultural Engineering department (UK BAE), and Wabash Valley Resources, LLC. The goal of this final technical project report is to comprehensively summarize the work conducted on project DE-FE0032043. In accordance with the Statement of Project Objectives (SOPO), the University of Kentucky (UK) (Project Prime Recipient) has developed and studied a biomass/plastic fuel with a hydrophobic surface area less than 10 m 2 /m 3 that is suitable for oxygen-blown entrained flow gasification with slurry feed. The project involved the utilization of an existing thermogravimetric analysis (TGA)-mass spectrometer (MS), 1.5” drop tube furnace, 1 ton per day (TPD) coal gasifier, and high-pressure extruder operated at UK. The pilot-scale production of blended material was done at the Polymers Technology Center in Charlotte, North Carolina. Parametric testing and solid fuel blend slurry performance validation was completed using the UK entrained flow gasifier with multiple opposed burners to narrow the major near-term technical gaps that impede gasification of biomass and carbonaceous mixed wastes such as plastics in order to achieve net-negative CO 2 emissions. Project results validated the UK approach to address the major technical challenges on the biomass/plastic pretreatment and gasification. Previously, this has been limited in application to fluidized-type or moving bed-type gasifiers due to the high-water uptake of porous biomass containing hydroxyl groups during the conventional slurry preparation, resulting in a highly viscous, un-pumpable slurry. The biomass pretreatment with plastic developed for this project demonstrates advantages in cost and flexibility, which include: 1) the development of a blended solid fuel slurry with 55-60 wt% solids and comparable heating value to 100% coal-based water slurry; 2) the collection of gasification kinetic data and identification of preliminary operating conditions by performing thermogravimetric analysis, gasification experiments by using a 1.5” drop tube furnace; and finally 3) the demonstrated gasification of the blended solid fuel in the UK entrained flow gasifier with a long-lasting stable solid fuel blend slurry, dataset detailing operating conditions, and characterization of slag phase formation and solidification. The lab-scale data and experience obtained during this project encourages the development of technologies and commercial approaches to enable a hydrogen-based energy economy while achieving net-negative CO 2 emissions through gasification of coal, biomass, and carbonaceous mixed wastes such as plastics.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2023

Mechanistic insights into the pyrolysis of poly (vinyl chloride)

The accumulation of unmanaged plastic waste in the environment has a devastating impact upon marine life and human health. Catalytic and thermal pyrolysis are promising technologies toward the efficient utilization of plastic waste. Yet, the processing of polymers, such as polyvinyl chloride (PVC), that decompose into corrosive compounds remains a major challenge. In this work, we employ density functional theory (DFT) and thermogravimetric analysis (TGA) to explore the elementary chemical steps that underpin the thermal decomposition of PVC. We determine that the dehydrochlorination reaction (i.e., 1 st stage of thermal decomposition) begins in tertiary chloride defects and propagates via HCl–mediated autocatalysis of internal allylic (IA) chloride groups. The latter groups, when in the vicinity of π–conjugated polymer segments, release HCl in a facile manner. We predict that other compounds, including hydrogen halides and H 2 O could also catalyze PVC’s dehydrochlorination. We suggest that hydrogen halides are the most efficient catalysts for this process, while other compounds like H 2 O may slow down the dehydrochlorination compared to purely HCl-catalyzed process, because of the dilution of the produced HCl. This result is corroborated by TGA experiments. Additionally, we study the thermochemistry and kinetics of polyene chain crosslinking and the formation of aromatics. The former reaction proceeds in parallel with the dehydrochlorination process (i.e., during the 1st stage of thermal decomposition), whilst the latter may occur at high temperatures (i.e., during the 2 nd stage of thermal decomposition). Furthermore, this work contributes to the fundamental understanding of molecular scale phenomena that take place during PVC pyrolysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Optical properties enhancement of thermal energy media for consistently high solar absorptivity

This study aimed to evaluate the optical properties of particles intended for use as thermal energy absorbers in generation 3 concentrated solar power systems. Their characterization involved UV–Vis NIR measurements with an integrating sphere for solar absorptivity, while a reflectometer was employed to measure thermal emittance. By combining absorptivity and emittance data, the solar absorption efficiency was calculated. Laser flash analysis, differential scanning calorimetry, and thermogravimetric analysis were utilized to determine thermal conductivity and specific heat. The solar absorptivity of the particles was initially measured at 0.90. After exposure to air at 1000 °C, it decreased to 0.73. However, following a reduction process, the particle recovered absorptivity of 0.90. The thermal aging and recovery were repeated multiple times, consistently achieving an absorptivity of 0.90. The thermal conductivity of the particles ranged from 0.50 to 0.88 W/(m-K). Solar absorptivity was found to be influenced by the types of iron oxide present in the particles. Particles with a predominance of hematite exhibited decreased solar absorptivity, while those containing magnetite, wüstite, and iron showed increased absorptivity. The estimated cost of the developed particles was more than ten times lower than that of current products. Given that component costs significantly impact the levelized cost of electricity (LCOE), this price reduction corresponded to an 8 % decrease in LCOE compared to other products. The low-cost thermal energy media show great promise for contributing to a reduced LCOE in the third generation of concentrating solar power systems.

14 SOLAR ENERGY↗
DOE OSTI2024

Photovoltaic Cable Connectors: A Comparative Assessment of the Present State of the Industry

The consequences of failure for balance-of-systems components (such as photovoltaic (PV) cable connectors) include offline module string(s); low system voltage; arc, ground, insulation, and overtemperature faults; triggered fuse(s); system shutdown; and fire. The degradation modes for connectors are studied here through an industry survey and its subsequent examination, which are compared with field-degraded specimens. A total of 117 specimens were obtained from a variety of locations and climates or accelerated tests. A failure analysis for connectors from PV installations was developed (and applied to 54 specimens), including nondestructive examinations (photography, a custom resistance-current scan, and X-ray computed tomography) and destructive examinations (featuring milling of the external plastic, extraction of the internal convolute spring, and potting and polishing in cross section). Surface and through-thickness composition of the metal pins and springs was quantified using scanning electron microscopy with energy-dispersive X-ray spectroscopy. Fourier transform infrared spectroscopy was used to verify the base polymer materials and compare the chemical structure of the connector body, bushing, end nut, and o-ring. Thermogravimetric analysis and differential scanning calorimetry were used to further verify the degradation of the same polymeric components.

cable connectors↗
DOE OSTI2023

Influence of Oxygen Uptake on Pitch Carbon Fiber

Carbon fiber precursor materials, such as polyacrylonitrile, pitch, and cellulose/rayon, require thermal stabilization to maintain structural integrity during conversion into carbon fiber. Thermal stabilization mitigates undesirable decomposition and liquification of the fibers during the carbonization process. Generally, the thermal stabilization of mesophase pitch consists of the attachment of oxygen-containing functional groups onto the polymeric structure. In this study, the oxidation of mesophase pitch precursor fibers at various weight percentage increases (1, 3.5, 5, 7.5 wt%) and temperatures (260, 280, 290 °C) using in situ differential scanning calorimetry and thermogravimetric analysis is investigated. The results are analyzed to determine the effect of temperature and weight percentage increase on the stabilization process of the fibers, and the fibers are subsequently carbonized and tested for tensile mechanical performance. Finally, the findings provide insight into the relationship between stabilization conditions, fiber microstructure, and mechanical properties of the resulting carbon fibers.

36 MATERIALS SCIENCE↗