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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 OSTI2025

Using a recirculating anaerobic dynamic membrane bioreactor to treat hydrothermal liquefaction aqueous by-product

Hydrothermal liquefaction (HTL) has the potential to improve resource recovery at water resource recovery facilities (WRRF), but the production of a high-strength aqueous by-product (HTL-aq) is hampering HTL implementation. The formation of biofilms in anaerobic digestion have been shown to be useful when degrading recalcitrant compounds present in HTL-aq due to the promotion of direct interspecies electron transfer (DIET) and increase in the microbial activity of syntrophic and methanogenic populations. The Recirculating Anaerobic Dynamic Membrane Bioreactor (RAnDMBr) was able to degrade 65% of the chemical oxygen demand (COD) at 1.5 ± 0.2 g COD LR −1 day −1 and 5.6 ± 2.3 days producing 0.19 ± 0.02 LCH4 gCOD fed −1 . However, adding a solution rich in nutrients on a daily basis was necessary. The system presented microbial populations able to degrade aromatic compounds (i.e., Anaerolinaceae) to perform DIET and syntrophy (i.e., Syntrophus) and methanogens (i.e., Methanobacterium and Methanosarcina) with the biofilm having a higher relative abundance of methanogens than the suspended biomass. Increasing the organic loading rate to 2 g COD LR −1 day −1 caused inhibition in the system by accumulation of volatile fatty acids, probably due to an increase in phenol, N-heterocyclic and aromatic compounds. Overall, this research shows that the RAnDMBr can be used to treat HTL-aq in WRRF without inhibition at OLRs of 1.5 ± 0.2 g COD LR −1 day −1 or lower, making HTL-aq treatment more feasible. Future research should focus co-digestion of HTL-aq with a co-substrate rich in nutrients and on fouling mitigation strategies that will allow to increase the recirculation ratio to promote advective substrate transport through the biofilm.

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

A Critical Review of Challenges Faced by Converting Food Waste to Bioenergy Through Anaerobic Digestion and Hydrothermal Liquefaction

Here, the conventional approaches for handling food waste has been incineration, composting, landfilling, and anaerobic digestion for producing biogas. In light of organic waste bans and newly discovered presence of per- and polyfluorinated substances (PFAS) in food, food packaging materials, and compost, this review provides a critical summary of what has been investigated and reported and what needs to be considered when choosing suitable pathways for food waste. In addition to the fundamental principles inherent to anaerobic digestion and hydrothermal liquefaction, challenges for each process are identified followed by discussion of potential solutions to resolve the bottlenecks.

09 BIOMASS FUELS↗
DOE OSTI2025

Continuous Wet Air Oxidation of the Hydrothermal Liquefaction Aqueous Product from Various Wet Wastes

Wet air oxidation (WAO) offers an effective method for treating waste streams, converting pollutants into benign substances, and holds significant potential for processing the aqueous product from the hydrothermal liquefaction (HTL-AP) of wet wastes, a promising renewable fuel technology. Here, we conducted a comprehensive study of the WAO of HTL-AP from four different wet wastes. Through continuous testing under various conditions, we produced samples with different chemical oxygen demand (COD) levels, enhancing understanding of reaction parameters necessary for substantial COD reduction (>95%). Chemical analysis revealed that alcohols and ketones in the HTL-AP rapidly oxidized to acetic acid through aldehyde intermediates, while acetic acid, other carboxylic acids, and phenols oxidized relatively slowly. The light N-containing compounds were found to exhibit a change in concentration only after the whole sample reaches an 80% COD reduction, indicating their refractory nature under applied conditions. Energy released in the WAO reaction was calculated, and anaerobic toxicity assay demonstrated that WAO treatment enhanced methane production kinetics due to reduced inhibitory effects, suggesting partial oxidative transformation of inhibitory compounds into less toxic derivatives. These findings provide insights into designing effective WAO processes for valorizing HTL aqueous products, addressing key barriers to HTL process commercialization.

anaerobic digestion↗
DOE OSTI2021

Hydrothermal catalysis of waste greases into green gasoline, jet, and diesel biofuels in continuous flow supercritical water

Production of green gasoline, jet, and diesel biofuels from waste greases was achieved using a novel hydrothermal, continuous-flow catalytic process operating under supercritical water conditions, with recycled water the only added chemical. Thermally and chemically stable catalysts were explored to optimize yields of liquid biofuels and to minimize production of gases and acidic compounds. A 50:50 mixture of brown and yellow waste greases converted into 76.6 wt% liquid biocrude (BC); the remainder converted to water and gases. Less than 0.2% of the FS formed carbon char (mainly amongst catalyst particles). Various tubular reactors (Inconel, ® Hastelloy®, titanium, stainless) showed no interior defects, erosion, or mass loss after runs. Here, the titanium catalyst was fully recovered and regenerated back to its original potency. The BC was further refined into 28%, 48%, 20%, and 4 wt%, respectively for green gasoline, jet, diesel, and bunker. Biofuels were analyzed for compound class compositions and reaction mechanisms were proposed. The hundreds of identified fuel products (C3-C35) from processing oleic acid as a pure model compound were identified. The neat green gasoline and diesel biofuels along with a 50% green jet blend (with petroleum Jet A) were tested in appropriate spark ignition, turbine, and diesel engines at University of MN Engine Labs. Biofuels achieved 107.7%, 97.2%, and 101.3% engine power performance levels relative to petroleum fuels (91-Octane, Jet A, #2 Diesel) along with lower CO and pollutant emissions. Biofuels passed ASTM fuel specifications (D4814, D7566, D975) including mandated corrosion and low sulfur limits of all three biofuels.

09 BIOMASS FUELS↗
DOE OSTI2021

Spray and combustion characteristics of pure hydrothermal liquefaction biofuel and mixture blends with diesel

Hydrothermal liquefaction (HTL) is the process in which biological compounds can be converted into biocrude diesel; various feedstocks, such as algae and wet biowaste, can be utilized. Almost 20 million dry tons of wet biowaste is deposited in U.S. municipal wastewaters annually. If recovered and converted into biodiesel, it can act as a massive source of renewable energy. Preliminary experiments on a diesel engine show that HTL fuel can achieve similar performance and emission levels to diesel. In order to further understand the influence of the HTL fuel properties, the HTL fuel and blends with diesel are observed in a constant volume chamber. Previously, 10% and 20% of the HTL fuel were blended with diesel by volume and demonstrated properties that roughly matched diesel in terms of combustion. In this study, 50% and 100% HTL fuel blends are tested on the same apparatus. It was discovered that the workability of HTL is almost the same as that of diesel and is less sensitive to ambient temperatures. When the ambient temperature is reduced from 1200 K to 800 K, the change ratio of ignition delay is only 62% of diesel. By analyzing the combustion process, it can be seen that there is no need to make major modifications to the engine control strategy if HTL fuel is applied to diesel engines. Though, under low temperature and low oxygen conditions, the soot luminosity peak of HTL100 is 3.12 times than that of diesel.

09 BIOMASS FUELS↗
DOE OSTI2020

Improving Electronic Conductivity of Layered Oxides through the Formation of Two-Dimensional Heterointerface for Intercalation Batteries

Synthetic strategies for the improvement in electronic conductivities and electrochemical stabilities of transition metal oxide cathodes, which are limiting factors in the performance of commercial intercalation batteries, are required for next-generation, high-performance battery systems. Furthermore, the chemical preintercalation approach, consisting of a combined sequence of a sol–gel process, extended aging, and a hydrothermal treatment, is a versatile, wet synthesis technique that allows for the incorporation of a polar species between the layers of transition metal oxides. Here, formation of a layered 2D δ-C x V 2 O 5 · n H 2 O heterostructure occurs via chemical preintercalation of dopamine molecules between bilayers of vanadium oxide followed by the hydrothermal treatment of the precipitate, leading to carbonization of the organic molecules. The presence of carbon layers within the structure has been confirmed via a combined analysis of scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, Raman spectroscopy, X-ray photoelectron spectroscopy, electrochemical impedance spectroscopy, four-probe conductivity measurements, and scanning transmission electron microscopy characterization. 2D δ-C x V 2 O 5 · n H 2 O heterostructure electrodes demonstrated significantly improved electrochemical performance, particularly at higher current densities, in Li-ion cells. The heterostructure electrodes exhibited 75% of the capacity retention when the current was changed from 20 mA g –1 (206 mAh g –1 ) to 300 mA g –1 (155 mAh g –1 ), while the reference δ-V 2 O 5 · n H 2 O electrodes exhibited only 10% capacity retention in the same experiment. Remarkably, 2D δ-C x V 2 O 5 · n H 2 O heterostructure electrodes demonstrated significantly improved capacity retention (94% after 30 cycles) for bilayered vanadium oxide electrodes in Li-ion cells during galvanostatic cycling at 20 mA g –1 . The improved electrochemical performance, in both extended cycling and rate capability studies, of the 2D δ-C x V 2 O 5 · n H 2 O heterostructure electrodes in the Li-ion system is ascribed to the intermittent formation of carbon layers within the bilayered structure, which leads to increased electronic conductivity and improved structural stability of the heterostructure compared to the reference δ-V 2 O 5 · n H 2 O electrodes.

25 ENERGY STORAGE↗
DOE OSTI2022

Achieving low-temperature hydrothermal relithiation by redox mediation for direct recycling of spent lithium-ion battery cathodes

Lithium-ion battery (LIB) recycling is an urgent need to address the massive generation of spent LIBs from portable devices and electrical vehicles. However, the large-scale recycling is hampered by economic and safety issues associated with today's recycling processes. In this study, we demonstrate a safe and energy efficient direct regeneration process based on low-temperature hydrothermal relithiation (LTHR) at low pressure for spent LiNi x Co y Mn z O 2 (0 < x,y,z <1, x + y + z = 1, or NCM) cathode materials. A low concentration of low-cost redox mediator is employed to improve the relithiation kinetics of spent NCM materials, enabling full relithiation temperature to be reduced from 220 °C to 100 °C or below. Correspondingly, the pressure incurred in the relithiation process can be reduced from ~25 bar to 1 bar, offering significantly improved operation safety. Specifically, three NCM materials, including chemically delithiated NCM111, cycled (degraded) NCM111, and cycled NCM622, were successfully regenerated with complete recovery of composition, crystal structure, and electrochemical performance, achieving the same effectiveness as that achieved at high temperature process. Meanwhile, the total energy consumption of spent cell recycling and the greenhouse gas emission is also reduced. This work provides a facile and scalable way to more sustainable LIB recycling with high economic return, high operation safety and low cost.

25 ENERGY STORAGE↗
DOE OSTI2022

Discovering hydrothermalism from Afar: In Situ methane instrumentation and change-point detection for decision-making

Seafloor hydrothermalism plays a critical role in fundamental interactions between geochemical and biological processes in the deep ocean. A significant number of hydrothermal vents are hypothesized to exist, but many of these remain undiscovered due in part to the difficulty of detecting hydrothermalism using standard sensors on rosettes towed in the water column or robotic platforms performing surveys. Here, we use in situ methane sensors to complement standard sensing technology for hydrothermalism discovery and compare sensors on a towed rosette and an autonomous underwater vehicle (AUV) during a 17 km long transect in the Northern Guaymas Basin in the Gulf of California. This transect spatially intersected with a known hydrothermally active venting site. These data show that methane signalled possible hydrothermal-activity 1.5–3 km laterally (100–150 m vertically) from a known vent. Methane as a signal for hydrothermalism performed similarly to standard turbidity sensors (plume detection 2.2–3.3 km from reference source), and more sensitively and clearly than temperature, salinity, and oxygen instruments which readily respond to physical mixing in background seawater. We additionally introduce change-point detection algorithms—streaming cross-correlation and regime identification—as a means of real-time hydrothermalism discovery and discuss related data supervision technologies that could be used in planning, executing, and monitoring explorative surveys for hydrothermalism.

58 GEOSCIENCES↗
DOE OSTI2022

Low-Cost Cellulosic Sugars Produced by NREL's Deacetylation and Mechanical Refining Process

The National Renewable Energy Laboratory has developed a deacetylation and mechanical refining (DMR) process that combines low-severity chemical pretreatment and mechanical refining to sidestep the expenses and challenges of traditional pretreatments, such as hydrothermal and dilute acid technologies. The DMR process is an important step in turning agricultural waste to sustainable aviation fuel.

biofuel↗
DOE OSTI2022

Post‐Annealing Treatment on Hydrothermally Grown Antimony Sulfoselenide Thin Films for Efficient Solar Cells

Herein, antimony sulfoselenide (Sb 2 (S, Se) 3 ) thin‐film solar cells are fabricated by a hydrothermal method followed by a post‐deposition annealing process at different temperatures and the impact of the annealing temperature on the morphological, structural, optoelectronic, and defect properties of the hydrothermally grown Sb 2 (S, Se) 3 films is investigated. It is found that a proper annealing temperature leads to high‐quality Sb 2 (S, Se) 3 films with large crystal grains, high crystallinity, preferred crystal orientation, smooth and uniform morphology, and reduced defect density. These results show that suppressing deep‐level defects is crucial to enhance solar cell performance. After optimizing the annealing process, Sb 2 (S, Se) 3 solar cells with an improved power conversion efficiency 2.04 to 8.48% are obtained.

14 SOLAR ENERGY↗
DOE OSTI2020

High solids loading biorefinery for the production of cellulosic sugars from bioenergy sorghum

A novel process applying high solids loading in chemical-free pretreatment and enzymatic hydrolysis was developed to produce sugars from bioenergy sorghum. Hydrothermal pretreatment with 50% solids loading was performed in a pilot scale continuous reactor followed by disc refining. Sugars were extracted from the enzymatic hydrolysis at 10% to 50% solids content using fed-batch operations. Here, three surfactants (Tween 80, PEG 4000, and PEG 6000) were evaluated to increase sugar yields. Hydrolysis using 2% PEG 4000 had the highest sugar yields. Glucose concentrations of 105, 130, and 147 g/L were obtained from the reaction at 30%, 40%, and 50% solids content, respectively. The maximum sugar concentration of the hydrolysate, including glucose and xylose, obtained was 232 g/L. Additionally, the glucose recovery (73.14%) was increased compared to that of the batch reaction (52.74%) by using two- stage enzymatic hydrolysis combined with fed-batch operation at 50% w/v solids content.

09 BIOMASS FUELS↗
DOE OSTI2020

Transformation of Ferrihydrite to Goethite and the Fate of Plutonium

Understanding the interactions between plutonium and iron (oxy)hydroxide minerals is necessary to gain a predictive understanding of plutonium environmental mobility and to evaluate long-term performance of nuclear waste repositories. We investigated the fate of plutonium during the formation of ferrihydrite and its subsequent transformation into goethite. Ferrihydrite was synthesized with varying quantities of Pu(IV) following either a sorption or coprecipitation process; the ferrihydrite was then aged hydrothermally to yield goethite. Additionally, the synthesized materials were characterized via extended X-ray absorption fine structure spectroscopy, transmission electron microscopy, and acid leaching to elucidate the nature of plutonium association with ferrihydrite and goethite. In samples prepared following the sorption method, plutonium was identified in two different forms: a PuO 2 precipitate and a surface-sorbed plutonium complex. For the samples prepared via coprecipitation, no PuO 2 formation occurs in the ferrihydrite precursor and in the goethite experiments where plutonium concentration is ≤1000 ppm (mg kg –1 ). In these coprecipitation products, plutonium is strongly bound to the minerals either via formation of an inner sphere complex, or via an incorporation process. In the coprecipitation experiments, PuO 2 formation only occurs at the highest plutonium concentration (3000 ppm), suggesting that during ferrihydrite transformation into goethite, part of the plutonium can be remobilized to form PuO 2 nanoparticles. Collectively, our results demonstrate that the nature of plutonium associated with the precursor ferrihydrite (adsorbed vs coprecipitated) will have a direct impact on the association of plutonium with its alteration product (goethite). Furthermore, the data illustrate that some properties of plutonium association with the precursor ferrihydrite are retained through the transformation into goethite. These findings show that plutonium strongly associates with iron (oxy)hydroxides formed through coprecipitation processes and in these materials, plutonium can be strongly retained by the iron minerals.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Unveiling the Role of Critical Impurities in Spent LiFePO 4 Cathodes for Scalable Direct Regeneration

Direct regeneration offers a promising alternative to recycling End-of-Life (EoL) batteries by restoring metal elements and preserving the material structure, yet scaling these technologies to handle practical cathode black mass (CBM) with impurities remains challenging. Here, this study investigates the evolution of impurities, including aluminum (Al), polyvinylidene difluoride (PVDF) binder, and residual carbon (C), during direct recycling of spent LiFePO 4 (LFP) cathodes and their impact on electrochemical performance. Using various ex situ and in situ analyses, it is shown that the formation of lithium fluoride (LiF) during the traditional direct recycling process hinders lithium diffusion and deteriorates the reversible capacity. To address this major challenge, the combination of pH-controlled hydrothermal purification and the two-step sintering process is proposed effectively to regenerate spent LFP cathodes, eliminating the negative effect of Al and fluorine (F) impurities while mitigating any potential impacts of carbon residuals. The regenerated LFP from spent CBM achieves superior performance, retaining 152.5 mAh g −1 at 0.1 C and 133 mAh g −1 at 1 C with 98.7% capacity retention after 200 cycles. This approach is further validated using three distinct waste feedstocks from battery modules, enhancing impurity management and scalability in direct recycling. These findings present a sustainable and economically viable solution for large-scale LFP regeneration.

25 ENERGY STORAGE↗
DOE OSTI2021

Evolution of Pore Structure and Permeability of Rocks Under Hydrothermal Conditions (Final Report)

The physical and transport properties of porous rocks can be altered by a variety of diagenetic, metamorphic, and tectonic processes, and the changes that result are of critical importance to such industrial applications as resource recovery, carbon dioxide sequestration, and waste isolation in geologic formations. The associated interrelationships between rocks, pore fluids and deformation are also key to understanding many natural processes, including dynamic metamorphism, fault mechanics, fault stability and pressure solution creep. In this project, we investigated the changes of permeability and pore geometry owing to inelastic deformation by solution-transfer, brittle fracturing and dislocation creep. In particular, we studied the coupling between pore fluids and deformation in fluid-filled quartz, calcite, mudstones and ultramafic rocks and examine the effects of coupled mechanical and chemical processes on the evolution of porosity and permeability under hydrothermal conditions. The investigations used a combination of techniques, that included triaxial laboratory experiments; uniaxial compressive loading with in situ observations of microstructure; permeability under hydrostatic compression; observations of microstructure using optical and electron microscopes, and micro-CT imaging; and numerical calculations. Laboratory experiments were designed to provide mechanical and transport data under conditions that isolate the particular mechanisms responsible for the changes. The data obtained were used to quantify changes in surface roughness, porosity, pore dimensions and their spatial fluctuations. The results of the experiments and data from image analyses were compared to the results of network, finite-difference and other numerical models to verify the validity of experimentally established relations between permeability and other rock properties. A bibliography for the period from 2015-2019 is appended below. New results obtained in the final year and the unfunded extension period are detailed below.

58 GEOSCIENCES↗
DOE OSTI2020

Chemical Free Two-Step Hydrothermal Pretreatment to Improve Sugar Yields from Energy Cane

Energy cane is an attractive lignocellulosic feedstock for processing into biofuels and bioproducts. A low-severity two-step hydrothermal pretreatment was investigated on energy cane for the production of monomeric sugar. Pretreatment temperature and time, in addition to the effect of disk milling, were observed for the glucose and xylose yields during hydrolysis. At residence times above 5 min in case of pretreatment at 200 °C, all of the hemicellulose was observed to be solubilized. The pretreatment condition of 200 °C for 10 min with disk milling was observed to provide the highest glucose concentration of 5.4%, and 200 °C for 5 min with disk milling provided the highest xylose concentration of 2.15%. The effect of disk milling in improving the sugar concentrations during hydrolysis was significant, especially at lower pretreatment temperatures and times. Low xylose yields at higher temperatures were attributed to the formation of degradation products at increased severity.

09 BIOMASS FUELS↗
DOE OSTI2026

Pyrite (001) Interface Chemistry is Controlled by a Sulfoxy Termination

Pyrite (FeS 2 ) is the most common sulfide mineral on Earth, forming through inorganic reactions in the crust and oceanic hydrothermal systems and via microbially driven processes in anaerobic sediments. The pyrite–water interface is the site of a wide range of adsorption and reaction processes in Earth systems including oxidation that dramatically affects the geochemistry of surface waters and influences global carbon and oxygen cycles. Mechanistic geochemical models of pyrite interfacial reactivity, however, are limited by the lack of experimentally derived atomistic structures of the reduced and reacting surfaces. Here, in this work, we reveal the atomic-scale structure of the pyrite (001)-water interface that forms at very low oxygen partial pressures, relevant to suboxic environments in Earth. The interface structure and surface speciation were obtained using the crystal truncation rod method supported by ambient-pressure photoelectron spectroscopy and density functional theory calculations. The surface is dominantly composed of disulfide groups bound to a single oxygen atom, forming a sulfoxy group that has no known molecular or bulk mineral analog. This surface is interpreted as the first step in the oxidative dissolution of pyrite. The sulfoxy group is readily protonated through surface acid–base reactions that alter the structure of interfacial water and the free energy of interfacial reactions. Surface iron sites are not oxidized. Surprisingly, this interface can likely develop in equilibrium with bulk pyrite in some reducing and acidic solutions. This termination is therefore likely representative of pyrite surfaces under a vast range of experimental, industrial and Earth conditions.

oxidation↗