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Understanding Thermal Stability in Zirconia-Based Aerogels

For lightweight, thermal insulation needs above 1000ºC, the high surface to volume ratios of ceramic-based aerogels are practically unparalleled. Yet realizing the full potential of aerogel-based thermal protection systems requires not only increased thermal stability, but also a broadened menu of stabilizing mechanisms. Here we will review our recent efforts to understand the impact of synthetic parameters and dopant chemistry on the evolution of zirconia-based ceramics. A broad parametric window for thermal stability is established, in which the more sensitive variable of composition has been probed. However, dopant chemistry is actually an aggregate for many closely related material parameters including surface energy, enthalpy of formation, each of which may contribute uniquely to aerogel destabilization. A truly predictive design framework for ceramic-based aerogels requires further decoupling of these underlying properties through systematic and comprehensive evaluation of thermodynamic properties.

aerogel↗

DOE OSTI2024

Unveiling the Thermal Stability of Sodium Ion Pouch Cells Using Accelerating Rate Calorimetry

The thermal stability of ~420 mAh Na 0.97 Ca 0.03 [Mn 0.39 Fe 0.31 Ni 0.22 Zn 0.08 ]O 2 (NCMFNZO)/hard carbon (HC) pouch cells was investigated using accelerating rate calorimetry (ARC) at elevated temperatures. 1 m NaPF 6 in propylene carbonate (PC):ethyl methyl carbonate (EMC) (1:1 by volume) was used as a control electrolyte. Adding 2 wt% fluoroethylene carbonate to the electrolyte improves the cell's thermal stability by decreasing the self-heating rate (SHR) across the whole testing temperature range. The selected states-of-charge (SoC), including 70%, 84%, and 100%, exhibit minimal impact on the exothermic behavior, except for a slight decrease in SHR after ~275 °C at 70% SoC. When compared to traditional lithium-ion batteries operating at 100% SoC, NCMFNZO/HC pouch cells demonstrate inferior thermal stability compared to LiFePO 4 (LFP)/graphite pouch cells, displaying a higher SHR from 220 to 300 °C. LiNi 0.8 Mn 0.1 Co 0.1 O 2 /graphite + SiO x pouch cells exhibit the worst safety performance, with an early onset temperature of ~100 °C and the highest SHR across the entire temperature range. These results offer a direct comparison of the impact of SoC and electrolyte compositions on the thermal stability of SIBs at elevated temperatures, highlighting that there is still room for improvement in SIBs safety performance compared to LFP/graphite chemistry.

42 ENGINEERING↗

DOE OSTI2021

Improving Thermal Stability of Perovskite Solar Cells by Suppressing Ion Migration Using Copolymer Grain Encapsulation

Thermal stability of organic–inorganic hybrid perovskites (OIHPs) remains as one of the critical challenges against the stable operation of perovskite solar cells (PSCs) in direct sunlight with elevated temperatures. Here, we show that the addition of a polystyrene-co-polyacrylonitrile (SAN) copolymer can significantly enhance thermal stability of OIHPs and improve the stability of the corresponding PSCs by suppressing the migration of organic cations in OHIP. The methylammonium lead iodide (MAPI) with SAN incorporated within the perovskite layer featured a superior thermal stability compared to pure MAPI without SAN, only displaying an average of 5–15% decrease in PCE even after continuous thermal aging for 24 h at 100 °C. The secondary ion mass spectrometry revealed that the thermal degradation of the pure MAPI was largely associated with MA+ out-migration. Conducting atomic force microscopy analysis further indicated that the incorporated SAN led to a suppression of ionic currents present at the grain boundaries of the perovskite film, which was understood by high immiscibility between SAN and MA+ components as confirmed by the experimentally estimated Flory–Huggins parameter between them. This study newly identifies a potential of using polymer grain encapsulation for enhancing thermal stability of OIHPs and their solar cell performance by suppressing the out-diffusion of cationic organic components.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Thermal Stability of Silica for Application in Thermal Energy Storage

Thermal energy storage (TES) systems have enabled concentrating solar power (CSP) to remain competitive in the modern energy mix by providing economical load shifting grid services and firming up intermittent solar resource. Free from siting constraints, TES also shows promise as an economical alternative to traditional pumped-storage hydropower (PSH) and compressed air energy storage (CAES). As potential thermal energy storage media, some solid particles demonstrate stability over wide temperature ranges which allows for increased sensible energy storage density and is essential in achieving low-cost storage. Silica sand, in the form of a-quartz, is one such candidate. This work presents a brief review of relevant silica thermophysical properties and further investigates the thermal stability of silica particles as a candidate TES media by subjecting them to two different thermal tests: (1) a 500-hour thermal treatment at 1200 degrees C under varied atmospheres; and (2) cycling 25, 50, and 100 times between 300 degrees C and 1200 degrees C. For both tests, particle stability is examined by means of pre- and post-treatment Mie scattering. An additional XRD analysis is conducted for the 500-hour treatment in air. Results indicate limited changes in both particle distribution and crystallographic structure which is promising for the application as solid particle media for thermal energy storage.

concentrating solar power↗

DOE OSTI2020

Thermal Stability of Silica for Application in Thermal Energy Storage

Free from siting constraints, thermal energy storage (TES) shows promise as an economical alternative to traditional pumped-storage hydropower (PSH) and compressed air energy storage (CAES). As potential thermal energy storage media, many solid particles demonstrate stability over wide temperature ranges which allows for increased sensible energy storage density and is essential in achieving low-cost storage. Silica sand, in the form of a-quartz, is one such candidate. This work presents a brief review of relevant silica thermophysical properties and further investigates the thermal stability of silica particles as a candidate TES media by subjecting them to two different thermal campaigns: (1) a 500-hour thermal treatment at 1200°C under varied atmospheres; and (2) cycling 25, 50, and 100 times between 300°C and 1200°C. For both campaigns, particle stability is examined by means of pre- and post-treatment Mie scattering. An additional XRD analysis is conducted for the 500-hour treatment in air. Results indicate limited changes in both particle distribution and crystallographic structure which is promising for the application as solid particle media for thermal energy storage.

27 ARPA - Advanced Research Projects Agency-Energy↗

DOE OSTI2020

Thermal Stability of Silica for Application in Thermal Energy Storage: Preprint

27 ARPA - Advanced Research Projects Agency-Energy↗

DOE OSTI2021

Thermal stability of additively manufactured austenitic 304L ODS alloy

Thermal stability and high-temperature mechanical properties of a 304L austenitic oxide dispersion strengthened (ODS) alloy manufactured via laser powder bed fusion (LPBF) are examined in this work. Additively manufactured 304L ODS alloy samples were aged at temperatures of 1000, 1100, and 1200 °C for 100 h in an argon atmosphere. Microstructure characterization of LPBF 304L ODS alloy before and after the thermal stability experiments revealed that despite the annihilation of dislocations, induced cellular substructure by the LPBF process was partially retained in the ODS alloy even after aging at 1200 °C. The size of Y-Si-O nanoparticles after aging at 1200 °C increased from 25 to 50 nm. EBSD analysis revealed that nanoparticles retained the microstructure of LPBF 304L ODS and hindered recrystallization and further grain growth. At 600 °C and 800 °C, the yield stress of the 290 and 145 MPa were measured, respectively, which are substantially higher than 113 MPa, and 68 MPa for 304L at the same temperatures. Furthermore, the creep properties of LPBF 304L ODS alloy were evaluated at a temperature of 700 °C under three applied stresses of 70, 85, and 100 MPa yielding a stress exponent (n) of ~7.7; the minimum creep rate at 100 MPa was found to be about two orders of magnitude lower than found in the literature for wrought 304L stainless steel.

36 MATERIALS SCIENCE↗

NASA NTRS2017

Jet Fuel Thermal Stability Investigations Using Ellipsometry

Jet fuels are typically used for endothermic cooling in practical engines where their thermal stability is very important. In this work the thermal stability of Sasol IPK (a synthetic jet fuel) with varying levels of naphthalene has been studied on stainless steel substrates using spectroscopic ellipsometry in the temperature range 385-400 K. Ellipsometry is an optical technique that measures the changes in a light beam’s polarization and intensity after it reflects off of a thin film to determine the film’s thickness and optical properties. All of the tubes used were rated as thermally unstable by the color standard portion of the Jet Fuel Thermal Oxidation Test, and this was confirmed by the deposit thicknesses observed using ellipsometry. A new amorphous model on a stainless steel substrate was used to model the data and obtain the results. It was observed that, as would be expected, increasing the temperature of the tube increased the overall deposit amount for a constant concentration of naphthalene. The repeatability of these measurements was assessed using multiple trials of the same fuel at 385 K. Lastly, the effect of increasing the naphthalene concentration in the fuel at a constant temperature was found to increase the deposit thickness.In conclusion, ellipsometry was used to investigate the thermal stability of jet fuels on stainless steel substrate. The effects of increasing temperature and addition of naphthalene on stainless steel tubes with Sasol IPK fuel were investigated. It was found, as expected, that increasing temperature lead to an increase in deposit thickness. It wasAmerican Institute of Aeronautics and Astronautics6also found that increasing amounts of naphthalene increased the maximum deposit thickness. The repeatability of these measurements was investigated using multiple tests at the same conditions. The present work provides as a better quantitative tool compared to the widely used JFTOT technique. Future work will expand on the fuel types, temperature, and substrate materials.

thermal stability↗

DOE OSTI2021

Complex Relationship between Side-Chain Polarity, Conductivity, and Thermal Stability in Molecularly Doped Conjugated Polymers

Molecularly doped conjugated polymers with polar side chains are an emerging class of conducting materials exhibiting enhanced and thermally stable conductivity. In this work, we study the electronic conductivity (σ) and the corresponding thermal stability of two polythiophene derivatives comprising oligoethylene glycol side chains: one having oxygen attached to the thiophene ring (poly(3-(methoxyethoxyethoxy)thiophene) (P3MEET)) and the other having a methylene spacer between the oxygen and the thiophene ring (poly(3-(methoxyethoxyethoxymethyl)thiophene) (P3MEEMT)). Thin films were vapor-doped with fluorinated derivatives of tetracyanoquinodimethane (FnTCNQ, n = 4, 2, 1) to determine the role of dopant strength (electron affinity) in maximum achievable σ. Specifically, when vapor doping with F 4 TCNQ, P3MEET achieved a substantially higher σ of 37.1 ± 10.1 S/cm compared to a σ of 0.82 ± 0.06 S/cm for P3MEEMT. Structural characterization using a combination of X-ray and optical spectroscopy reveals that the higher degree of conformational order of polymer chains in the amorphous domain upon doping with F 4 TCNQ in P3MEET is a major contributing factor for the higher σ of P3MEET. Additionally, vapor-doped P3MEET exhibited superior thermal stability compared to P3MEEMT, highlighting that the presence of polar side chains alone does not ensure higher thermal stability. Molecular dynamics simulations indicate that the dopant–side-chain nonbond energy is lower in the P3MEET:F 4 TCNQ mixture, suggesting more favorable dopant–side-chain interaction, which is a factor in improving the thermal stability of a polymer/dopant pair. Our results reveal that additional factors such as polymer ionization energy and side-chain–dopant interaction should be taken into account for the design of thermally stable, highly conductive polymers.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Thermal Stability of Nanocrystalline Gradient Inconel 718 Alloy

Gradient structures containing nanograins in the surface layer have been introduced into Inconel 718 (IN718) nickel-based alloy using the surface mechanical grinding treatment technique. The thermal stability of the gradient IN718 alloy was investigated. Annealing studies reveal that nanograins with a grain size smaller than 40 nm exhibited significantly better thermal stability than those with larger grain size. Transmission electron microscopy analyses reveal that the enhanced thermal stability was attributed to the formation of grain boundaries with low energy configurations. This study provides new insight on strategies to improve the thermal stability of nanocrystalline metals.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Insights into the Enhanced Oxidative Thermal Stability of Nanoparticle Organic Hybrid Materials Developed for Carbon Capture and Energy Storage

Due to the growing need for Direct Air Capture (DAC) and integrated carbon capture and conversion technologies, CO 2 capture materials that can withstand a wide range of environmental conditions, including fluctuating ambient temperatures and high concentrations of oxidizing agents (i.e., oxygen and moisture), are critically needed. Liquid-like Nanoparticle Organic Hybrid Materials (NOHMs) have been proposed as candidates for DAC and electrolyte additives enabling sustainable energy storage (i.e., integrated CO 2 capture and conversion and flow batteries). Liquid-like NOHMs functionalized with an ionic bond have been shown to display greatly enhanced oxidative thermal stability compared to the untethered polymer. However, these studies were limited in terms of reaction conditions and the detailed mechanisms of the oxidative thermal degradation were not reported. In this work, a kinetic thermal degradation analysis was performed on NOHM-I-HPE and the neat polymer, Jeffamine M2070 (HPE), in both non-oxidative and oxidative conditions. NOHM-I-HPE displayed similar thermal stability to the untethered polymer in a nitrogen environment, but interestingly, the thermal stability of the ionically tethered polymer was significantly enhanced in the presence of air. This observed enhancement of oxidative thermal stability is attributed to the orders of magnitude larger viscosity of the liquid-like NOHMs compared to untethered polymer and the bond stabilization of the ionically tethered polymer in the NOHMs canopy. Further, spectroscopic analyses of the liquid residue revealed that in the presence of oxygen, the degradation of HPE and NOHM-I-HPE occurs through the formation of trace amounts of carbonyls. This study illustrated that NOHMs can serve as functional materials for sustainable energy storage applications because of their excellent oxidative thermal stability.

25 ENERGY STORAGE↗

NASA NTRS1987

Thermal Stability of Distillate Hydrocarbon Fuels

Thermal stability of fuels is expected to become a severe problem in the future due to the anticipated use of broadened specification and alternative fuels. Future fuels will have higher contents of heteroatomic species which are reactive constituents and are known to influence fuel degradation. To study the degradation chemistry of selected model fuels, n-dodecane and n-dodecane plus heteroatoms were aerated by bubbling air through the fuels amd stressed on a modified Jet Fuel Thermal Oxidation Tester facility operating at heater tube temperatures between 200 to 400 C. The resulting samples were fractionated to concentrate the soluble products and then analyzed using gas chromatographic and mass spectrometric techniques to quantify and identify the stable reaction intermediate and product specifically. Heteroatom addition showed that the major soluble products were always the same, with and without heteroatoms, but their distributions varied considerably.

Reddy, Kishenkumar Tadisina↗

DOE OSTI2022

Flammability and thermal stability of thermoplastic-based composites filled with natural carbon

This investigation characterized flammability and thermal stability for a novel sustainable composite engineered for use in building applications. Flammability and thermal stability of coal plastic composites composed of coal (40–60 wt.%) and high-density polyethylene were compared to commercial wood–plastic composites. Pyrolysis thermogravimetric analysis results indicated that coal plastic composites possessed a single-step decomposition and higher char residue, while wood–plastic composites had two-step decomposition, with the first peak occurring at much lower temperatures. Thermogravimetric analyses in air suggest coal plastic composites, compared to wood–plastic composites and neat high-density polyethylene, were more thermally stable. Flash ignition temperatures for coal plastic composites were higher than high-density polyethylene and wood–plastic composites, while self-ignition temperatures were in the same range as wood–plastic composites. Rate of burning data indicated coal plastic composites were slower burning than wood–plastic composites, with increasing coal content slowing burning rate by 19.9%–27.6%. Cone calorimeter testing showed 27% and 59% reduction in total heat release and total smoke release as coal content increased while coal plastic composite with 60 wt.% coal possessed lower overall flammability in comparison with predominant commercially available wood–plastic composite products. Coal improved composite overall thermal stability and flammability by acting as char former and foaming agent.

Engineering↗

NASA NTRS1979

Jet Fuel Thermal Stability

Various aspects of the thermal stability problem associated with the use of broadened-specification and nonpetroleum-derived turbine fuels are addressed. The state of the art is reviewed and the status of the research being conducted at various laboratories is presented. Discussions among representatives from universities, refineries, engine and airframe manufacturers, airlines, the Government, and others are presented along with conclusions and both broad and specific recommendations for future stability research and development. It is concluded that significant additional effort is required to cope with the fuel stability problems which will be associated with the potentially poorer quality fuels of the future such as broadened specification petroleum fuels or fuels produced from synthetic sources.

Taylor, W. F.↗

NASA NTRS1982

Experimental study of the thermal stability of hydrocarbon fuels

The thermal stability of two hydrocarbon fuels (premium diesel and regular diesel) was determined in a flow reactor under conditions representing operation of an aircraft gas turbine engine. Temperature was varied from 300 to 750 F (422 to 672 K) for fuel flows of 2.84 to 56.8 liters/hr (corresponding to 6.84 x 0.00010 to 1.63 x 0.010 kg/sec for regular diesel fuel and 6.55 x 0.00010 to 1.37 x 0.010 kg/sec for premium diesel fuel); test times varied between 1 and 8 hr. The rate of deposition was obtained through measurement of weight gained by metal discs fixed along the channel wall. The rate of deposit formation is best correlated by an Arrhenius expression. The sample discs in the flow reactor were varied among stainless steel, aluminum and brass; fuels were doped with quinoline, indole, and benzoyl perioxide to yield nitrogen or oxygen concentrations of approximately 1000 ppm. The most substantial change in rate was an increase in deposits for brass discs; other disc materials or the additives caused only small perturbations. Tests were also conducted in a static reactor at temperatures of 300 to 800 F for times of 30 min to 2 1/2 hr. Much smaller deposition was found, indicating the importance of fluid transport in the mechanism.

Marteney, P. J.↗

NASA NTRS1958

The Thermal Stability of Unsymmetrical Dimethylhydrazine

The thermal stability of unsymmetrical dimethylhydrazine was investigated in a static system simulating conditions in an almost-empty fuel tank. The self-ignition temperature and spontaneous decomposition temperature of the pure fuel were determined at atmospheric pressure to be 454 and 740 F. respectively, with the larger (740 F) value, obtained in an inert atmosphere of nitrogen, representing the minimum temperature that would cause a rapid exothermic reaction. The addition of 40 weight percent dimethylenetriamine to unsymmetrical dimethylhydrazine did not significantly affect these properties.

Spakowski, Adolph E.↗

DOE OSTI2026

Citric Acid Functionalized Natural Fibers to Enhance Thermal Stability and Moisture Resistance in Polylactic Acid Composites

Cellulosic fibers can impart many unique benefits into composite applications, such as reduced weight or structural reinforcement; however, these materials also increase hygroscopicity and decrease thermal stability, restricting broader applications. The present work adapted an experimental process for functionalizing the cellulose surface using citric acid (CA) for three fibers: a 100% cellulose bleached soft Kraft pulp (e.g., creafill) and two natural fibers with similar composition but different fiber morphology, flax fiber and banana fiber. The process uses CA with a sodium hypophosphite (SHP) catalyst to chemically functionalize fiber surfaces, and the reaction mechanism was investigated through Fourier Transform Infrared Spectroscopy (FTIR), which suggested a grafting mechanism rather than a surface-based crosslinking between neighboring sites. Functionalized fibers were compounded into polylactic acid (PLA) at 20 wt.% to better understand how this functionalization might impact critical performance properties like thermal stability, crystallization, thermal mechanical properties, and water uptake of these composites. The study demonstrated varying levels of efficacy for the functionalization of cellulosic fibers with CA/SHP and the fiber with the most open microstructure, e.g., banana fiber, exhibited the largest change in its properties with a 38% reduction in water uptake compared to untreated banana fiber composites. Parallel evaluation of the functionalization process for different fibers demonstrates the importance of fiber morphology on surface modification and can enable their use in composites by demonstrating the efficacy of this potentially low-cost, low-toxicity method for reducing hygroscopicity and improving thermal stability.

citric acid↗

NASA NTRS1993

Research and development of high thermal stability fuels

Increases in aircraft performance are leading to increases in the thermal stress on the primary aircraft coolant--the fuel. Fuel thermal stability limitations may offset future aircraft performance gains. The Air Force's Wright Laboratory is sponsoring several research programs to address this problem. The development of an additive package for JP-8 to improve its thermal stability is the primary focus of this paper. This program involves extensive testing of fuels and additives in a variety of test devices, culminating in tests in a fuel system simulator and engine tests. These tests involve Air Force personnel, on-site contractors (University of Dayton Research Institute, Systems Research Laboratories), Pratt and Whitney Aircraft Co., additive manufacturers, and Sandia National Laboratory. The test devices include several flowing and static tests, where the behavior of a fuel is investigated in a wide variety of environments. The study of several baseline fuels in these devices has led to some new insights into the mechanisms of fuel thermal (in)stability. It is becoming clear that a fuel's tendency to oxidize (to form peroxides, for example) is often inversely proportional to its tendency to form insoluble deposits.

T Edwards↗