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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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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Trends in Light and Temperature Sensitivity Recommendations among Licensed Biotechnology Drug Products

Inherent structural and functional properties of biotechnology-derived therapeutic biologics make them susceptible to light- and temperature-induced degradation and consequently can influence their quality. Photosensitivity of therapeutic proteins continues to be examined, but the commonalities and trends of storage conditions and information about light and temperature sensitivity among currently licensed therapeutic proteins has not been previously surveyed. Using a comprehensive and relational database approach, we conducted a scientific survey of all licensed biotechnology-derived drug products with the goal of providing evidence-based information about recommended storage conditions of formulations sorted by light- and temperature-related attributes as described for each product at licensure. We report the prevalence of indications for light and temperature sensitivity in formulations categorized by their presentation type, number of doses, container type, dosage form and active molecule type. We also report the storage temperature range across formulations and diluents for reconstitution and dilution. Formulations with excipients that potentially facilitate light-induced and thermal degradation were also noted. The result of our analysis indicates that light and temperature sensitivity are prevalent across therapeutic protein formulations. However, when a formulation is reconstituted or diluted, both light and temperature sensitivity are less clear. In addition, light and temperature sensitivity are more well defined in liquid formulations than lyophilized powder formulations, and more well defined in products manufactured in autoinjectors, prefilled-syringes, and pens than products in vials. Overall, our report provides a data-driven summary of storage conditions among therapeutic protein formulations to support the development of future biologic drug products.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2025

Enhancement of Uranium Ionization Efficiencies Using Zn-MOF-74 Derived Nanoporous Ion Emitters for Thermal Ionization Mass Spectrometry

The recent introduction of nano-porous ion emitters (nano-PIEs) formed from metal organic frameworks (MOFs) has demonstrated the potential to enhance sensitivity for thermal ionization mass spectrometry (TIMS). Nano-PIEs take advantage of the parent MOF’s chemical and structural tunability to form scaffolds for ion emitters. A study by Barpaga et al. 2023 on MOF-74 as the parent material found that with high volatility metals in their framework uranium sample utilization efficiency (SUE) increases by up to nine-fold (e.g., Zn-MOF-74) compared to that of the analyte on a bare filament (~0.05%). Here, in this study, we investigate the performance of Zn-MOF-74 to maximize uranium efficiencies at the trace level (= 10 -12 g) by altering the parent MOF morphology and chemistry (i.e., MOF crystal sizes and thermal degradation) and optimizing its integration with TIMS (i.e., MOF mass on a filament and ramp conditions). We observed improvement in SUE up to 20 times (≤1.0%) that of a bare filament load when nano-PIEs derived from nanocrystals of Zn-MOF-74 were heated under a specific current ramp condition. This demonstrates that rates of nano-PIE structural collapse during TIMS analysis and the subsequently formed nanomaterials (and their features) can be tuned to control analyte ionization.

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

PDMS ‐silica composite gas separation membranes by direct ink writing

Abstract Polydimethylsiloxane (PDMS)‐based membranes containing amine‐functionalized and unfunctionalized silica particles were fabricated via direct ink writing for CO 2 /N 2 gas separation. The printability of the inks was evaluated by rheological measurements, while spectroscopy, microscopy, thermal measurements, and mechanical testing were employed to characterize the printed membranes. The surface morphology of the membranes revealed the absence of voids, demonstrating their suitability for gas separation. The printed membranes also exhibited desirable thermal and mechanical properties (i.e., thermal degradation temperature of 518 °C and tensile strength as high as 1.178 MPa with 529% elongation). The PDMS‐based membranes generally displayed high permeability for CO 2 but slightly low selectivity for the CO 2 /N 2 gas pair. The best‐combined permeability‐selectivity performance of 8794 barrer and selectivity of 11.64 was demonstrated by the printed PDMS membrane containing no SiO 2 fillers. The inclusion of unfunctionalized SiO 2 particles generally increased the membrane's gas permeability but compromised the selectivity. In contrast, membranes with amine‐functionalized silica showed improved selectivity compared to membranes containing unfunctionalized silica. Overall, the performance and characteristics offered by the PDMS/silica composite membranes demonstrated the potential of 3D printing as an economical and sustainable fabrication approach to developing materials for carbon capture applications.

Gutierrez, Dianne B.↗
DOE OSTI2025

Investigating the Role of Acid Sites in the Hydrocracking of Polyethylene-EVOH Multilayer Film Waste over Pt/BEA Catalyst

Multilayer polymer films (MFs) containing poly(ethylene-co-vinyl alcohol) (EVOH) and polyolefins are ubiquitous in single-use food and medical packaging. MFs are currently landfilled or incinerated rather than mechanically recycled because of the processing difficulties associated with their form factor and complex multicomponent structures. Advanced chemical recycling is a promising solution. Prior reports have explored hydrogenolysis and hydrodeoxygenation to convert EVOH, but these technologies are limited by catalyst deactivation and slow apparent kinetics, respectively. Alternatively, in this work, we demonstrate the efficient hydrocracking of commercial MFs into naphtha range (C5-C12) alkanes over platinum (Pt) supported on acidic zeolites. Mixtures of low-density polyethylene (LDPE) and EVOH are utilized as MF surrogates to gain fundamental insights. Pt deposited on BEA supports with varying Lewis acid site (LAS) concentrations are synthesized and tested for hydrocracking. Surprisingly, Pt/BEA with high LAS concentrations demonstrate improved activity for LPDE/EVOH blends over LDPE alone. In contrast, LAS concentrations are shown to have no influence on LDPE hydrocracking. LAS and Brønsted acid sites (BAS) catalyze the dehydration of EVOH to form water, which improves LDPE hydrocracking. Polyaromatics formed primarily via EVOH thermal degradation lead to detrimental coke formation, which hinders hydrocracking activity. Reaction conditions and feed ratios of LDPE and EVOH are tuned to balance these competing effects. Reusability tests demonstrate that Pt/BEA maintains high activity (81% conversion in 2 h) and high selectivity towards naphtha (78%) over multiple reuse cycles. Furthermore, these findings position hydrocracking as a promising technology for the circularity of complex MF plastic waste.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Generalized Analysis of Dynamic Flow Fouling on Heat Transfer Surfaces

Several energy applications involve flow of untreated heat transfer fluids that contain trace amounts of mineral salts, such as calcium carbonate and calcium sulfate, which show reverse solubility with temperature. The gradual accretion of these salts onto the heat transfer surfaces causes fouling that degrades thermal performance over time. While fouling of bare surfaces has been extensively studied, fouling of nonwetting superhydrophobic or liquid-infused surfaces is less understood, especially under dynamic flow conditions. This study presents a systematic experimental analysis to elucidate dynamic flow fouling of calcium carbonate and calcium sulfate on smooth, superhydrophobic and liquid-infused surfaces in a generalized manner. Here, copper tubes with modified inner surface wettability are fabricated and subjected to forced convection at different flow rates and fouling salt concentrations. Fouling characteristics of the two salts on the different surfaces are examined through microstructural analysis, and quantified in terms of asymptotic fouling resistance that measures the total extent of fouling, and a threshold time, which correlates to the onset of significant fouling. Using Taguchi design of experiments, the study reports, for the first time, closed-form analytical relationships for the asymptotic fouling thermal resistance and threshold time on the Reynolds number, dimensionless concentration of fouling agent and dimensionless infused liquid viscosity that represents the different surface types in a unified manner. It is shown that the analytical model accurately predicts the fouling characteristics in up to about 97% of the data, based on which contour maps of optimum surface designs for minimizing fouling resistance are presented. The results provide information on designing surfaces for reduced fouling or for estimating the fouling characteristics for a given surface in applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Glassy carbon formation from pyrolysis of polymeric coatings on fiber-optic sensors

Deploying fiber-optic sensors in nuclear reactors requires a detailed understanding of radiation effects on the fiber materials and the transmitted signals. Previous work has shown large wavelength shifts in the reflected spectra obtained from polymer-coated fiber-optic temperature sensors exposed to high neutron fluences. The sensor drift resulting from these wavelength shifts cannot be explained by radiation effects on fused silica glass. These shifts are hypothesized to be caused by the conversion of the polymeric fiber coating to a glassy carbon via radiolysis and/or pyrolysis and subsequent radiation-induced compaction. Here, thermal degradation of these polymeric coatings was studied to provide insight into the potential origins of the sensor drift phenomenon. Acrylate- and polyimide-coated fibers were heated under various temperatures (250–1300 °C) and environments (oxidative and inert), and the resulting coating products were characterized via mass-loss data, scanning electron microscope imaging, and Raman spectroscopy. Results suggest that the polymer decomposition product of both coating types, at least under inert conditions, is indeed a glassy carbon. Analytical models that account for radiation-induced glassy carbon coating compaction show significant compressive fiber strains and predicted wavelength shifts that agree well with experimental measurements, providing additional evidence that supports the hypothesized origins of the sensor drift.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Boron Nitride-Driven Strengthening of Aluminum Composites via Friction Stir Processing

Friction stir welding and processing (FSW/P) has emerged as an effective solid-state joining technique for fabricating metal matrix composites (MMCs), offering improved mechanical properties through refined microstructural evolution. In this study, an aluminum-boron nitride nanoparticle (Al-BNNP) composite was synthesized via FSW, and its indentation-based mechanical properties were systematically evaluated. Microhardness mapping across the weld cross-section revealed a progressive increase in hardness toward the stir zone (SZ), attributed to severe plastic deformation, dynamic recrystallization (DRX), and the reinforcing effect of BNNPs. Profilometry-based indentation plastometry (PIP) inferred yield strength (YS) demonstrates a 47.8% increase compared to the base metal (BM) and a 75% improvement compared to FSP pure aluminum reported in literature. This enhancement is attributed to strengthening mechanisms, including grain boundary pinning, load transfer, and increased dislocation density. The strain rate sensitivity (SRS) measurements at the nanoscale demonstrated a substantial decrease in the SZ, correlated with ultrafine grain structures and strong BNNP-matrix interactions. Activation volume analysis revealed a significant reduction in the SZ, suggesting that dislocation motion is increasingly restricted by dislocation-dislocation and dislocation-particle interactions. These findings suggest that incorporating BNNPs in FSW/P enables tailoring the microstructure without thermal degradation of the secondary particles, thereby significantly enhancing the mechanical performance of aluminum composites, particularly for structural applications in aerospace and automotive industries.

Aluminum↗
DOE OSTI2022

Aging of UV curable PDMS developed for large-scale, high viscosity stereolithography

Polydimethylsiloxane (PDMS) elastomers are silicone rubbers that find widespread application in both academic and industrial settings. This study investigates the use of photosensitive platinum catalysts for UV-activated hydrosilylation of PDMS, which enables the additive manufacturing of PDMS objects through techniques such as stereolithography. Specifically, this study focuses on understanding the aging behavior of Pt-catalyzed, UV-curable PDMS samples, including their mechanical behavior under thermal and UV-accelerated aging conditions. The results show that the Pt-catalyzed, UV-curable PDMS introduced in this research is ‘under-cured’ after being printed and will slowly evolve over time resulting in increased stiffness and decreased elongation, likely due to the formation of additional crosslinks. FTIR spectroscopy indicates that no new chemical bonds or functional groups are generated through the aging process, suggesting that no thermal degradation or polymer chain scissions occur in the polymer matrix. Overall, this PDMS formulation exhibits greater mechanical strength and significantly less reduction in strength with aging, compared with the commonly used, UV-curable thiol-ene PDMS.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Thermal Stability of LiNi x Mn y Co z O 2 Cathode Materials

Here, the thermal evolution of LiNi x Mn y Co z O 2 (NMC) lithium-ion battery electrode materials is examined at various states of charge (SOC) or lithium concentrations for a variety of Ni:Mn:Co ratios or electrode compositions. Synchrotron X-ray diffraction (XRD) combined with Rietveld analysis shows the onset decomposition temperatures of phases, decomposition products, lattice parameters, and phase fractions as a function of composition and SOC. SOC impacts the lattice parameters of the NMC phase, where a collapse of the c-axis in the NMC phases is noted due to lithium extraction. Among the compositions examined, the low-Ni NMC111 uncycled sample (NMC111 0% SOC) exhibited the highest thermal stability, with a decomposition temperature approximately 250 °C higher than that of NMC532 0% and NMC811 0%. When the SOC exceeds 50% (i.e., more than 0.4 mol of Li ions extracted), the influence of Ni content on the decomposition temperature becomes negligible, with decomposition occurring around 250−300 °C for all compositions. Ni content also affects the decomposition pathways: NMC111 tends to first form a TM 3 O 4 -type phase, where TM represents transition metals, before transforming into a TMO-type phase, whereas most of the NMC811 samples directly decompose into the TMO phase. The presence of metallic phases was confirmed by both XRD and thermogravimetric-differential scanning calorimetry (TGA-DSC) analysis, as a result of heating under inert conditions. The TGA-DSC results suggest that metallic phase formation is favored at lower SOC in samples with a higher Ni content. This work provides comprehensive insight into the thermal degradation pathways of NMC materials as a function of composition, SOC, and temperature.

Peng, Jian [Univ. of New South Wales, Sydney, NSW ↗
DOE OSTI2021

Emissions from Heated Terpenoids Present in Vaporizable Cannabis Concentrates

Vaporizable cannabis concentrates (VCCs) consumed as a liquid (vaping) or a waxy solid (dabbing) are becoming increasingly popular. However, their associated emissions and impacts have not been fully described. Mixtures containing different proportions of 12 VCC terpenoids and high MW compounds were heated at 100-500 °C inside a room-sized chamber to simulate emissions. Terpenoids, thermal degradation byproducts, and ultrafine particles (UFPs) were quantified in the chamber air. Air samples contained over 50% of emitted monoterpenes and less than 40% of released sesquiterpenes and terpene alcohols. Eleven degradation byproducts were quantified, including acrolein (1.3-3.9 μg m -3 ) and methacrolein (2.0 μg m -3 ). A large amount of UFPs were released upon heating and remained airborne for at least 3 h. The mode diameter increased from 80 nm at 100 °C to 140 nm at 500 °C, and particles smaller than 250 nm contributed to 90% of PM 1.0 . Here, the presence of 0.5% of lignin, flavonoid, and triterpene additives in the heated mixtures resulted in a threefold increase in the particle formation rate and PM 1.0 concentration, suggesting that these high-molecular-weight compounds enhanced aerosol inception and growth. Predicted UFP emission rates in typical consumption scenarios (6 × 10 11 -2 × 10 13 # min -1 ) were higher than, or comparable with, other common indoor sources such as smoking and cooking.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Electro-Optic Modulation Using Metal-Free Perovskites

Electro-optic (EO) modulation is of interest to impart information onto an optical carrier. Inorganic crystals—most notably LiNbO 3 and BaTiO 3 —exhibit EO modulation and good stability, but are difficult to integrate with silicon photonic technology. Solution-processed organic EO materials are readily integrated but suffer from thermal degradation at the temperatures required in operating conditions for accelerated reliability studies. Hybrid organic–inorganic metal halide perovskites have the potential to overcome these limitations; however, these have so far relied on heavy metals such as lead and cadmium. Here, we report linear EO modulation using metal-free perovskites, which maintain the crystalline features of the inorganic EO materials and incorporate the flexible functionality of organic EO chromophores. We find that, by introducing a deficiency of cations, we reduce the symmetry in the perovskite crystal and produce thereby an increased EO response. The best-engineered perovskites reported herein showcase an EO coefficient of 14 pm V –1 at a modulation frequency of 80 kHz, an order of magnitude higher than in the nondefective materials. Furthermore, we observe split peaks in the X-ray diffraction and neutron diffraction patterns of the defective sample, indicating that the crystalline structure has been distorted and the symmetry reduced. Density functional theory (DFT) studies link this decreased symmetry to NH 4 + deficiencies. This demonstration of EO from metal-free perovskites highlights their potential in next-generation optical information transmission.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Catalytic Deconstruction of Ethylene Vinyl Acetate Copolymer and Polyethylene Mixtures via Hydroconversion: Challenges and Solutions

We explore hydrogenolysis over ruthenium supported on zirconia (Ru/ZrO 2 ) and hydrocracking over platinum (Pt) supported on zeolites as an effective end-of-life strategy for ethylene vinyl acetate (EVA)–a widely used performance heat sealant in hard-to-recycle multilayer packaging. For Ru/ZrO 2 hydrogenolysis, EVA reacts slower than low-density polyethylene (LDPE) and the catalyst deactivates due to carbonaceous deposits originating from polyenes generated in situ during EVA thermal degradation. High H 2 pressures and temperatures can overcome catalyst deactivation; however, CH 4 yields are excessive due to cascade hydrogenolysis stemming from strong C=C/metal interactions. Polyene hydrogenation allows chains anchored by C=C to desorb from Ru, shifting product selectivity from CH 4 to higher-value liquids. Hydrogenolysis of mixed EVA and linear low-density polyethylene (LLDPE), mirroring typical frozen food packaging formulations, results in comparable catalyst activity and CH 4 yield as the pure EVA resin. For Pt/zeolite hydrocracking, pure EVA and EVA:LLDPE mixtures are deconstructed to propane or light naphtha with minimal CH 4 production. Among catalysts tested, Pt/HY gives the highest liquid productivity (g C5+products /g cat ·h). Furthermore, these findings showcase the recalcitrant nature of EVA and its associated mixtures for Ru/ZrO 2 hydrogenolysis, highlighting that hydrocracking catalysts may be superior for complex packaging waste.

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

Cell-Free-Based Thermophilic Biocatalyst for the Synthesis of Amino Acids from One-Carbon Feedstocks

Bioproduction from one-carbon compounds, such as formate, is an attractive prospect due to reduced energy requirements and the possibility for using CO 2 as a sustainable feedstock. Formate-fixing pathways engineered using Escherichia coli lysate-based cell-free expression (CFE) biocatalysts have the potential to route 100% of feedstock carbon toward chemical synthesis but are undermined by siphoning of in-pathway metabolites and cofactors by the CFE background metabolism. To address this limitation, we engineer a CFE-based thermophilic multienzyme biocatalyst for the synthesis of serine and glycine from formate, bicarbonate, and ammonia. After expression of the thermophilic formate-to-serine pathway in a one-pot reaction, the mesophilic E. coli CFE background machinery is removed by simple heat denaturation, eliminating the siphoning of cofactors, inpathway metabolites, and products. After bioprocess optimization, including pathway gene expression duration and chemical synthesis temperature, we achieve near stoichiometric conversion of formate and bicarbonate to serine and glycine, reaching 97% of stoichiometric yield. The use of a moderately thermophilic biocatalyst allowed chemical synthesis to take place at mesophilic temperatures, enabling the balance of optimal enzyme activity with minimal metabolite/cofactor thermal degradation. In a fed-batch experiment, the biocatalyst shows sustained chemical synthesis rates for 8 h, paving the way toward a continuous bioprocess. Finally, a sensitivity analysis of cofactor usage revealed that the most expensive cofactors, THF and NADPH, can be reduced by 5-fold without significantly lowering product yields. To the best of our knowledge, this is the first instance of expressing a thermophilic pathway in an E. coli lysate-based CFE system to generate a thermophilic biocatalyst for use at mesophilic temperatures. The CFEbased thermophilic formate-to-serine biocatalyst triples the combined serine and glycine yield previously obtained by a CFE-based mesophilic formate-to-serine biocatalyst (30%), and quadruple the yield obtained by a purified enzyme system (22%). Ultimately, this work opens the door to using E. coli lysate-based CFE for thermophilic biocatalyst generation to achieve high chemical synthesis yields.

bacteria↗
DOE OSTI2023

Subsurface spectroscopy of heterogeneous materials using optical wavefront shaping

Plastic-bonded explosives and propellants consist of energetic molecular crystals embedded in a polymer matrix that also includes additives, such as taggants, plasticizers, grit, antioxidants, etc. Furthermore, this heterogeneous composition renders these materials optically opaque, limiting optical characterization techniques (e.g., Raman spectroscopy) to probing chemical reactions at the sur-face. However, many reactions of interest are believed to occur inside the material where current optical techniques can not probe. To address this challenge, we have developed a new optical technique that utilizes feedback assisted wavefront shaping (using spatial light modulators) to focus probe light inside a heterogeneous material, such that we can perform subsurface spectroscopy. Recently, we demonstrated this technique by monitoring subsurface photodegradation and thermal degradation of Eu-doped molecular crystals using both fluorescence and Raman spectroscopy. Based off these successes we are now looking into improvements to this technique to allow for greater time resolution, including replacing our spatial light modulators with fast digital mirror devices, using ns optical phase conjugation, and self-healing optical beams.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Rare earth elements from waste

Rare earth elements (REEs) are critical materials in electronics and clean technologies. With the diminishing of easily accessible minerals for mining, the REE recovery from waste is an alternative toward a circular economy. Present methods for REE recovery suffer from lengthy purifications, low extractability, and high wastewater streams. Here, we report an ultrafast electrothermal process (~3000°C, ~1 s) based on flash Joule heating (FJH) for activating wastes to improve REE extractability. FJH thermally degrades or reduces the hard-to-dissolve REE species to components with high thermodynamic solubility, leading to ~2× increase in leachability and high recovery yields using diluted acid (e.g., 0.1 M HCl). The activation strategy is feasible for various wastes including coal fly ash, bauxite residue, and electronic waste. The rapid FJH process is energy-efficient with a low electrical energy consumption of 600 kWh ton –1 . The potential for this route to be rapidly scaled is outlined.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2020

Corrosion-Resistant Coatings for Mitigation and Repair of Spent Nuclear Fuel Dry Storage Canisters

This report summarizes the results of a literature survey on coatings and surface treatments that are used to provide corrosion protection for exposed metal surfaces. The coatings are discussed in the context of being used on stainless steel spent nuclear fuel (SNF) dry storage canisters for potential prevention or repair of corrosion and stress corrosion cracking. The report summarizes the properties of different coating classes, including the mechanisms of protection, their physical properties, and modes of degradation (thermal, chemical, radiological). Also discussed are the current standard technologies for application of the coatings, including necessary surface pretreatments (degreasing, rust removal, grinding) and their effects on coating adhesion and performance. The coatings are also classified according their possible use for in situ repair; ex situ repair, requiring removal from the overpack; and ex situ prevention, or application prior to fuel loading to provide corrosion protection over the lifetime of the canister.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Unraveling the Pyrolytic Behavior and Kinetics of Single Polymers and Plastic-Rich Municipal Solid Waste Using Thermal Analysis

Pyrolysis is a highly promising thermochemical recycling technology for converting heterogenous plastic waste into sustainable fuels in a single step. Therefore, understanding the pyrolysis mechanism is essential for enabling rational reactor design and enhancing efficient recycling techniques. In this study, the thermal degradation behaviors and corresponding kinetics of pure polymers (PE, PP, and PET) and plastic-rich MSW were examined using simultaneous thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Experiments were carried out in the temperature range of 30-800°C with variable heating rates from 5°C/min to 20°C/min in an ultra-high purity Argon atmosphere. Our results indicated that the plastic pyrolysis was an endothermic process, with varying decomposition temperature ranges depending on their structure and composition. Various iso-conversional model-free methods (Friedman, Flynn-Wall-Ozawa, Starink, and Kissinger-Akahira-Sunose) were utilized to determine the apparent activation energy of the plastic degradation, which increased in the following order: PET (214 kJ/mol), PP (218 kJ/mol), PE (245 kJ/mol), and MSW (249 kJ/mol). Finally, Criado’s master plots were employed to identify the best-fitting reaction model and the pre-exponential factor was subsequently determined.

Bashir, Muhammad Aamir↗