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Results for “Low-temperature Chemistry”

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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Low-Temperature Catalyst Redispersion: A Route to Enhanced Stability of Supported Metal Catalysts?

Sintering poses a significant challenge to achieving the long-term stability of supported metal catalysts under reaction conditions. Here, in this study, we report a low-temperature catalyst redispersion mechanism, in which platinum single atoms, which aggregate into nanoparticles under Reverse Water Gas Shift (RWGS) conditions at elevated temperatures, fragment into atomically dispersed species upon cooling. Using multimodal operando characterization combined with first-principles theoretical modeling, we track the structural evolution of Pt single atoms supported on ceria nanodomes, deposited either on ceria or ceria–titania mixed oxides. We find that fragmentation is more pronounced when cooling occurs under RWGS conditions compared to CO alone, owing to a synergistic interplay of the effects of H 2 , CO 2 , and CO. The support architecture has a strong influence on the extent of redispersion: while CO alone induces fragmentation on ceria, interfacial confinement and vacancy pinning at the ceria–titania interface suppress restructuring. In contrast, RWGS conditions overcome these barriers, enabling redispersion across both supports. These findings point toward a pathway for catalyst stabilization via reaction-induced redispersion under mild conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Quantum Emitters Induced by High Pressure and UV Laser Irradiation in Multilayer GaSe

In this work, we report on defect generation in multilayer GaSe through hydrostatic pressure quenching and UV laser irradiation. The Raman line width from the UV 266 nm irradiated sample is much wider than that in pressure-quenched GaSe, corresponding to a wider defect energy distribution range in the former sample than the latter. After quenching from 11.2 GPa, three photoluminescence (PL) peaks from defect states are observed at 657, 681, and 695 nm at a low temperature of 93 K. Defect-related peaks at 649, 694, 750, and 774 nm also appear in low-temperature PL spectra after UV laser irradiation, with a nonmonotonous intensity dependence on irradiation duration. There are common features in defects produced by these two methods: the PL peaks with the lowest energy are sharp, and their PL intensities increase linearly with the excitation laser power and saturate above a certain excitation laser power. These two features are similar to those in defects for single-photon emission (SPE) in other 2D materials at even lower temperatures. Fluorescence lifetime imaging shows distinguished short (2.3 ns) and long (75.6 nm) lifetimes of the 695 nm PL line in pressure-quenched GaSe. The density functional theory predicts defect energy levels related to Se vacancy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Atomic Layer Deposition for Enhanced Light Confinement in Nonlinear Metasurfaces

Metasurfaces enable the generation of strong nonlinear signals, with nanoantenna resonances significantly enhancing the nonlinear response through tailored light–matter interactions. Commonly used nonlinear materials, such as lithium niobate and other similar crystals, have relatively moderate refractive indices, limiting their ability to achieve the strong mode localization attainable with high-refractive-index materials like silicon. Here, we report on enhancing mode confinement in nonlinear metasurfaces by employing conformal coatings of titania with atomic layer deposition (ALD). We develop a low-temperature ALD that enables the augmentation of resonances in materials that cannot withstand high-temperature processing, including polymers. We report on the design of a metasurface incorporating a nonlinear crystal and an ALD coating, achieving enhanced mode localization through this approach in the near-infrared wavelength range. We numerically demonstrate a significant enhancement in second-harmonic generation in the designed metasurface, achieved by optimizing the thickness of the ALD coating for the telecommunication wavelength.

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

Insights into Sustainable Nitrogen Fixation by Gas-phase Spectroscopic Measurements and Global Modeling of Reaction Intermediates in Humid Nitrogen Plasma

In this article, there is growing interest in reacting molecular nitrogen and water to sustainably synthesize fixed forms of nitrogen such as ammonia. In particular, low-temperature plasmas can activate these relatively inert feedstocks at or near room temperature without a catalyst. However, because of the enhanced reactivity and nonequilibrium chemistry, a diverse range of products is formed, and the underlying reaction mechanisms are exceedingly complex. In this work, we studied a simplified reactor consisting of a gaseous plasma containing controlled mixtures of nitrogen gas and water vapor. Densities of key chemical species such as N, H, OH, NH, and NO were measured by emission and laser-based spectroscopy as a function of the relative humidity. A global model was constructed and the reaction network was validated by comparing calculated species densities with experiments. We discover that N, a key initial intermediate for ammonia, strongly decreases in the presence of water vapor, and as a result, ammonia formation becomes limited at high relative humidity. This decrease is surprisingly not because N itself reacts, but because one of its main sources, an excited molecular nitrogen state, is reacted away. In addition, oxidation pathways for nitrogen, which lead to NO and related products, are found to be favored over reduction pathways because the corresponding reverse reactions are less significant. Together, this understanding helps explain previously reported observations of selectivity toward nitrogen oxides over ammonia, particularly at higher relative humidities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Emissive Colloidal GaAs Quantum Dots

Colloidal quantum dots offer tunable optical properties for optoelectronic applications, but the synthesis of high-quality III–V quantum dots (QDs) other than indium pnictides, and particularly GaAs, has remained elusive due to synthetic challenges. Colloidal GaAs QDs have been reported very recently and have shown only weak band-edge photoluminescence. Here, we demonstrate a large-scale synthesis of colloidal GaAs QDs in molten salts, followed by a high-temperature surface treatment with K 2 S, which removes native oxide and enables uniform zinc chalcogenide shell growth on GaAs. These QDs demonstrate bright band-edge photoluminescence and electroluminescence in QD LED devices. Low-temperature spectroscopy reveals a well-resolved exciton fine structure with distinct bright-state splitting and temperature-independent decay dynamics from 4 to 100 K. These results establish a practical pathway for the preparation of high-quality colloidal GaAs QDs from molten salts with potential applications in quantum technologies and optoelectronics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Surface Hydration of Porous Nickel Hydroxides Facilitates the Reversible Adsorption of CO 2 from Ambient Air

Direct air capture (DAC) under humid ambient conditions typically requires the use of organic components, with sorbents that are purely inorganic in composition for the most part operating hundreds of degrees above room temperature. In this work, we report porous metal hydroxides as a novel class of water-tolerant, oxidatively and hydrothermally stable low-temperature sorbents that exhibit competitive DAC working capacities of 1.25 mmol/g over 5 consecutive temperature swing adsorption–desorption cycles in the presence of steam and oxygen. Aqueous miscible organic solvent treatments are used to create highly porous structures with surface areas exceeding 700 m 2 /g that capture CO 2 in the form of bicarbonates under dry conditions, and carbonates under wet conditions. Water exerts a facilitative rather than an inhibiting effect on CO 2 binding, and the presence of hydrating multilayers serves to stabilize carbonate species akin to moisture swing adsorbents except for the fact that solvation results in a remarkable (upto 10-fold) increase, not decrease, in DAC capacity. High-valent doping with cerium is used to improve DAC capacities by amplifying surface basicity, evidencing porous nickel hydroxides specifically (and porous metal hydroxides more generally) as a novel class of robust, earth-abundant DAC sorbents.

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

Active species in chloroaluminate ionic liquids catalyzing low-temperature polyolefin deconstruction

Abstract Chloroaluminate ionic liquids selectively transform (waste) polyolefins into gasoline-range alkanes through tandem cracking-alkylation at temperatures below 100 °C. Further improvement of this process necessitates a deep understanding of the nature of the catalytically active species and the correlated performance in the catalyzing critical reactions for the tandem polyolefin deconstruction with isoalkanes at low temperatures. Here, we address this requirement by determining the nuclearity of the chloroaluminate ions and their interactions with reaction intermediates, combining in situ 27 Al magic-angle spinning nuclear magnetic resonance spectroscopy, in situ Raman spectroscopy, Al K-edge X-ray absorption near edge structure spectroscopy, and catalytic activity measurement. Cracking and alkylation are facilitated by carbenium ions initiated by AlCl 3 - tert -butyl chloride (TBC) adducts, which are formed by the dissociation of Al 2 Cl 7 − in the presence of TBC. The carbenium ions activate the alkane polymer strands and advance the alkylation cycle through multiple hydride transfer reactions. In situ 1 H NMR and operando infrared spectroscopy demonstrate that the cracking and alkylation processes occur synchronously; alkenes formed during cracking are rapidly incorporated into the carbenium ion-mediated alkylation cycle. The conclusions are further supported by ab initio molecular dynamics simulations coupled with an enhanced sampling method, and model experiments using n-hexadecane as a feed.

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

Site requirements for inhibition-free CO oxidation over silica-supported bimetallic PdCu alloys

Pd catalysts are highly active for CO oxidation but suffer from inhibition by NO at low temperatures (<150 °C). We posit that incorporation of Cu into the Pd catalyst will improve low-temperature CO oxidation activity and reduce inhibition from competitive adsorbers. To probe this hypothesis, a series of PdCu alloys with different Pd : Cu ratios were synthesized and tested in the temperature-programmed oxidation of CO in the presence and absence of NO. Incorporation of small amounts of Cu into Pd improves the reactivity, as well as the resistance to NO inhibition. Beyond this, Cu incorporation into the Pd has a detrimental effect on the activity for CO oxidation. Based on combined infrared and X-ray absorption spectroscopy studies, here we show that high activity and resistance to inhibition requires alloying of Pd and Cu and the formation of a diverse surface, while surface segregation of Cu results in poor activity and inhibition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Size-dependent second-order-like phase transitions in Fe nanocluster melting from low-temperature structural isomerization

Here, in this work, the melting phase transitions of Fe n nanoclusters with 10 ≤ n ≤ 100 atoms are investigated using classical many-body molecular dynamics simulations. For many cluster sizes, surface melting occurs at much lower temperatures than core melting. Surface and core melting points and energetic melting points (temperatures of maximum heat capacity, C v ) are calculated for all cluster sizes. Melting properties are found to be strong functions of cluster structure. Cluster sizes with closed-shell structures always have first-order-like phase transitions. Almost one-third of cluster sizes in the analyzed range exhibit second-order-like phase transitions due to the presence of multiple structural configurations close in energy. 1-shell clusters with one to a few more atoms than a neighboring closed-shell structure have very low surface melting points and very high energetic melting points compared to their closed-shell counterparts. In clusters above 50 atoms with certain core structures, melting of the surface before the core was observed.

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

Synthesizing Highly Crystalline Graphite Powder from Bulk Polyethylene Waste for Lithium-Ion Battery Anodes

Upcycling plastic waste into graphite can potentially be used, in conjunction with other methods, to manage existing waste materials and diversify graphite supply chains. However, synthesizing large quantities of crystalline graphite powder from plastic waste, particularly polyethylene (PE), remains a challenge because PE decomposes into light gases during thermal processing, and simple methods do not exist at any appreciable size scale to address this challenge. In this work, a method is developed for air processing bulk forms of PE waste to create a stable carbon char that does not readily decompose during high-temperature processing. This method employs solid additives in the form of salts, which are combined with the PE melt during air processing to increase the effective surface area of the melt and improve the oxygen-driven chemistry that stabilizes the PE for high-temperature processing. After removing the solid salt additives from the PE-derived char, it is converted into a highly crystalline bulk graphite powder using a Fe-based low-temperature (<1500 °C) catalytic process. The PE-derived graphite powder showed excellent electrochemical performance as an anode material for lithium-ion batteries (LIBs) with a capacity of up to 302 mAh/g at 0.5 discharge/charge cycles per hour (0.5 C) and capacity retention of 100% after 415 cycles.

Huynh, Ngoc Tien↗
DOE OSTI2024

Generative Physics-Informed Neural Network Solving Multi-Scale and Multi-Phase Plasma Chemical Flow Field

Low-temperature plasmas (LTPs) are non-equilibrium systems with near-room-temperature gas and highly energetic electrons. This makes them ideal for delicate applications in biomedicine and semiconductor manufacturing, enabling processes like wound healing, sterilization, etching, and plasma-enhanced chemical vapor deposition without thermal damage. However, LTPs involve complex chemistries, with hundreds of species and thousands of reactions, complicating their diagnosis, prediction, and control. Conventional diagnostics, such as Fourier-transform infrared spectroscopy (FTIR), laser-induced fluorescence (LIF), and optical emission spectroscopy (OES), offer limited species detection, while mass spectrometry (MS) struggles with low-sensitivity species. Additionally, LTP simulations face multi-scale challenges, as macroscopic fluid dynamics and microscopic particle collisions operate on vastly different timescales. To address these issues, we developed an artificial intelligence (AI) based diagnostic system: a generative physics-informed neural network (PINN-Gen) that can predict spatially resolved species concentrations and temperatures in LTPs by integrating experimental data from planar LIF with microscopic plasma chemical kinetics and macroscopic fluid mechanics, including plasma-liquid interactions at the interface between two phases. PINN-Gen solves no equations but checks the errors of physical laws by substituting the output from neural network, and the comparison with the experimental results. Thus, it naturally avoids the multi-scale difficulty of numerical simulations and predicts the results of conventionally unsolvable multi-scale and multi-phase problems. The real-time prediction will be robust due to the physical information used in the training of such a neural network, and only very limited input of condition required due to its generative feature.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

Synthesizing Highly Crystalline Graphite Powder from Bulk Polyethylene Waste for Lithium-Ion Battery Anodes

Upcycling plastic waste into graphite can potentially be used, in conjunction with other methods, to manage existing waste materials and diversify graphite supply chains. However, synthesizing large quantities of crystalline graphite powder from plastic waste, particularly polyethylene (PE), remains a challenge because PE decomposes into light gases during thermal processing, and simple methods do not exist at any appreciable size scale to address this challenge. In this work, a method is developed for air processing bulk forms of PE waste to create a stable carbon char that does not readily decompose during high-temperature processing. This method employs solid additives in the form of salts, which are combined with the PE melt during air processing to increase the effective surface area of the melt and improve the oxygen-driven chemistry that stabilizes the PE for high-temperature processing. After removing the solid salt additives from the PE-derived char, it is converted into a highly crystalline bulk graphite powder using a Fe-based low-temperature (<1500 °C) catalytic process. The PE-derived graphite powder showed excellent electrochemical performance as an anode material for lithium-ion batteries (LIBs) with a capacity of up to 302 mAh/g at 0.5 discharge/charge cycles per hour (0.5 C) and capacity retention of 100% after 415 cycles. This method illustrates there are opportunities for upcycling large quantities of PE waste to produce graphite powders.

Huynh, Ngoc Tien [NETL Site Support Contractor, Na↗
DOE OSTI2025

Advancing a Low-Temperature, Low-Cost Direct Air Capture System Based on Organic Chemistry

Holocene Climate Corporation (Holocene) partnered with Oak Ridge National Laboratory (ORNL) to conduct bench-scale testing of a new optimized Direct Air Capture (DAC) process to assist the U.S. Department of Energy (DOE) in achieving the Carbon Negative Shot target of under $\$$100/net tonne CO₂ removed by 2031. Holocene’s DAC process for carbon dioxide (CO₂) removal uses amino acids and guanidine compounds, an ORNL-invented chemical process and licensed by Holocene. Holocene will use this novel chemistry to develop a new process and deploy the technology commercially.

36 MATERIALS SCIENCE↗
DOE OSTI2026

HydroGEN Consortium: Advancements in Hydrogen Production

HydroGEN Energy Materials Network (EMN) is an U.S. Department of Energy (DOE) EERE Hydrogen and Fuel Cell Technologies Office (HFTO)-funded consortium that aims to accelerate the discovery and development of advanced water splitting materials (AWSM) for clean, low-cost hydrogen production. Materials innovations are key to enhancing performance, durability, and cost of hydrogen generation technologies. HydroGEN is focused on low technology readiness level AWS technologies, including low- (alkaline exchanged membrane electrolysis) and high-temperature electrolysis (proton-conducting solid oxide electrolysis), photoelectrochecmical (PEC) and thermochemical (TCH) water splitting. The AWS technologies in this consortium study proton conduction in solid oxide electrolysis and hydroxide conduction in polymer electrolysis, and proton transport in photoelectrochemical water splitting. This presentation will provide an overview of the HydroGEN EMN and technical highlights of a few lab-led and DOE-awarded "seedling" R&D projects. HydroGEN continues to grow its community of industry, university, and national laboratories, forming a national innovation ecosystem focused on renewable hydrogen production.

08 HYDROGEN↗
DOE OSTI2024

Metal-Catalyzed Thermo-Catalytic Decomposition and Continuous Catalyst Generation

In this study, metal dusting is utilized to initiate a two-stage thermo-catalytic decomposition (TCD) process. Stage 1 starts with metal-catalyzed TCD, and in stage 2 the metal-catalyzed carbon catalyzes additional TCD. TEM is presented of the early- versus late-stage TCD to qualitatively illustrate the second-stage TCD by the metal-catalyzed carbons. Corresponding SEM illustrates differences in growth type and surface density between early versus late reaction times, with backscattered imaging differentiating the first- versus second-stage TCD. TGA supports the microscopic inference of a second carbon phase by the presence of an early (low-temperature) reaction peak, characteristic of low-structure or disordered carbon as the second-stage TCD carbon. Raman analysis confirms that the second-stage carbon deposit is more disordered and unstructured, especially at 1000 °C, supported by the ID/IG and La value changes from 0.068 to 0.936 and 65 nm to 4.7 nm, respectively. To further confirm second-stage TCD occurrence upon pre-catalyzed carbons, two carbon blacks are tested. Exposing a combination of edge and basal or exclusively basal sites for the graphitized form, they afford a direct comparison of TCD carbon nanostructure dependence upon the initial carbon catalyst nanostructure. Pre-oxidation of the stainless-steel wool (SSW) prior to TCD is advantageous, accelerating TCD rates and increasing carbon yield relative to the nascent SSW for an equivalent reaction duration.

Chemistry↗
DOE OSTI2024

Exploring pH Dynamics in Amino Acid Solutions Under Low-Temperature Plasma Exposure

Low-temperature plasma (LTP) offers a promising alternative for cancer therapy, as it targets malignant cells selectively while minimizing damage to healthy tissues. Upon interaction with an aqueous solution, LTP generates reactive oxygen and nitrogen species and thereby influences the solution’s pH, which is a crucial factor in cancer proliferation and response to treatment. This study investigated the effects of LTP on the pH of aqueous solutions, with a focus on the effect of LTP parameters such as voltage, frequency, and irradiation time. In addition, it explored the influence of solution composition, specifically the presence of the amino acids, glycine and serine, on pH changes; these amino acids are known to play significant roles in cancer proliferation. Our results indicated that LTP induces acidification in deionized water, in which the extent of acidification increased proportionally with plasma parameters. In glycine-containing solutions, pH changes were concentration-dependent, whereas serine-containing solutions maintained a constant pH across all tested concentrations. To investigate potential changes to the structural properties of glycine and serine exposed to LTP that could be responsible for different pH responses, we analyzed the samples using FTIR spectroscopy. A significant decrease in absorbance was observed for solutions with low concentrations of amino acids, suggesting their degradation.

Biochemistry & Molecular Biology↗
DOE OSTI2025

Examples of X-Ray Characterization Techniques in Energy Storage Research

Lithium-ion batteries have revolutionized the portable electronics and transportation sectors. Their performance is often critically dependent on the crystal structures of the anode and cathode electrode materials, which must enable the transport and reversible storage of lithium ions into and out of the lattice. Because lithium is a low-Z element, characterization of materials for lithium-ion batteries can be particularly challenging. Regardless, X-ray techniques enable analysis of material structures to better understand how battery materials perform and degrade, particularly when combined with other materials characterization and electrochemical characterization techniques. While X-ray techniques are most often used in battery research for phase identification of crystal structures, X-ray characterization techniques are also used for a wide variety of other purposes. I will discuss several examples from my research with various collaborators on several projects that highlight the impact that X-ray characterization techniques can have on battery research. The first example will focus on low-temperature microwave-assisted solvothermal synthesis of vanadium-doped LiFePO4 cathode materials for lithium-ion batteries. (1,2) Through a combination of electrochemical and materials characterization, we determined that low temperature synthesis resulted in metastable phases that enabled incorporation of higher dopant levels than resulting from high-temperature synthesis of thermodynamically stable phases. Rietveld refinement of X-ray diffraction data enabled understanding of how lattice parameters changed with doping levels and synthesis temperature. X-ray absorption near edge spectroscopy enabled understanding of the vanadium and iron oxidation states to confirm how vacancies in the structure caused by doping were charge compensated. This was important to understand because the literature suggests doping can improve LiFePO4 electrical conductivity, which improves battery charge and discharge rates. The second example will focus on understanding residual strain in lithium metal anodes. Lithium-ion batteries typically use graphite anodes, but the charge-storage capacity can be theoretically improved ~10x by using lithium metal as the anode material instead. However, lithium anodes suffer from growth of high-aspect-ratio features, such as dendrites, that can pierce nanoporous polymer separators and lead to short circuits and fires. External pressure is commonly applied to cells to enable better morphological control. We hypothesized that applied pressure may promote strain and possibly work hardening during electrochemical cycling, which motivated us to look for evidence of residual strain in lithium metal cycled under applied pressure using X-ray diffraction and sin2(..psi..) analysis. We found that lithium electrodeposited under high pressure exhibited in-plane compressive strain and that that lithium electrodeposited under low pressure did not. (3) The residual strain that accompanies electrodeposition under high pressure may lead to work hardening, which may explain how a soft metal like lithium can puncture separators and why higher pressure does not always decrease short circuits. (4-6) References: 1) Harrison, K. L.; Manthiram, A. Microwave-Assisted Solvothermal Synthesis and Characterization of Metastable LiFe1- x (VO) x PO4 Cathodes. Inorganic chemistry 2011, 50(8), 3613-3620. 2) Harrison, K. L.; Bridges, C. A.; Paranthaman, M. P.; Segre, C. U.; Katsoudas, J.; Maroni, V. A.; Idrobo, J. C.; Goodenough, J. B.; Manthiram, A. Temperature Dependence of Aliovalent-Vanadium Doping in LiFePO4 Cathodes. Chemistry of Materials 2013, 25(5), 768-781. 3) Rodriguez, M. A.; Harrison, K. L.; Goriparti, S.; Griego, J. J.; Boyce, B. L.; Perdue, B. R. Use of a Be-Dome Holder for Texture and Strain Characterization of Li Metal Thin Films via Sin2 (..psi..) Methodology. Powder Diffraction 2020, 35(2), 89-97. 4) Jungjohann, K. L.; Gannon, R. N.; Goriparti, S.; Randolph, S. J.; Merrill, L. C.; Johnson, D. C.; Zavadil, K. R.; Harris, S. J.; Harrison, K. L. Cryogenic Laser Ablation Reveals Short-Circuit Mechanism in Lithium Metal Batteries. ACS Energy Letters 2021, 6(6), 2138-2144. 5) Harrison, K. L.; Merrill, L. C.; Long, D. M.; Randolph, S. J.; Goriparti, S.; Christian, J.; Warren, B.; Roberts, S. A.; Harris, S. J.; Perry, D. L. Cryogenic Electron Microscopy Reveals That Applied Pressure Promotes Short Circuits in Li Batteries. Iscience 2021, 24(12). 6) Harrison, K. L.; Goriparti, S.; Merrill, L. C.; Long, D. M.; Warren, B.; Roberts, S. A.; Perdue, B. R.; Casias, Z.; Cuillier, P.; Boyce, B. L. Effects of Applied Interfacial Pressure on Li-Metal Cycling Performance and Morphology in 4 M LiFSI in DME. ACS Applied Materials & Interfaces 2021, 13(27), 31668-31679.

batteries↗