SEARCH · Search NASA

Results for “Mixed solvent processing”

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.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 55 records · Page 3

All sources NASA NTRS DOE OSTI

NASA NTRS1972

Polymeric compositions and their method of manufacture

Filled polymer compositions are made by dissolving the polymer binder in a suitable sublimable solvent, mixing the filler material with the polymer and its solvent, freezing the resultant mixture, and subliming the frozen solvent from the mixture from which it is then removed. The remaining composition is suitable for conventional processing such as compression molding or extruding. A particular feature of the method of manufacture is pouring the mixed solution slowly in a continuous stream into a cryogenic bath wherein frozen particles of the mixture result. The frozen individual particles are then subjected to the sublimation.

Moser, B. G.↗

DOE OSTI2025

Developing Digital Twin Visualizations: A Methodology and Case Study on Chemical Separation Processing

As advances in digital engineering continue to push the technological boundaries, digital twin (DT) visualizations for diagnostics and safeguards advancement become much more feasible and practical. DTs generate large and complex data streams that require effective user interfaces to provide monitoring and diagnostic capabilities. Unfortunately, while these frameworks exist, there is not much research on the systematic documentation of human–computer interaction (HCI) for DT visualization. This work presents a dual-mode visualization methodology (two dimensional [2D] graphical user interface dashboard and 3D mixed reality) designed to support diagnostic tasks in DT systems and building on a validated framework and applying established HCI principles. The methodology is demonstrated through a case study of aqueous processing at Idaho National Laboratory, using experimental data from the chemical solvent extraction runs. Our interfaces display real-time alerts and monitoring to inform users of safeguards anomalies. The interfaces use immersive 3D mixed-reality visualization for further system and experiment investigation. This work demonstrates how the systematic application of HCI principles can inform DT visualization design for diagnostic and safeguards applications. While formal user evaluation studies remain as future work, this paper documents the systematic design methodology and demonstrates a proof-of-concept implementation.

3D visualization↗

NASA NTRS2004

PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

Smith, Joseph G.↗

DOE OSTI2020

Conversion of lignin into a water-soluble polyacid using a MOF catalyst

A process for valorization of lignin includes the steps of mixing lignin; a MOF catalyst metalated with a metal atom selected from the group consisting of Fe, Mn, Co, Cu, or Ni, and combinations thereof; an oxidizing agent; and an aqueous solvent. The product of this process, a charged polyacid-containing species derived from lignin, may be included in a dispersion with a dispersible particulate material, and an aqueous dispersing medium.

09 BIOMASS FUELS↗

DOE OSTI2022

The Importance of Nonequilibrium to Equilibrium Transition Pathways for the Efficiency and Stability of Organic Solar Cells

Controlled morphology of solution-processed thin films have realized impressive achievements for non-fullerene acceptor (NFA)–based organic solar cells (OSCs). Given the large set of donor–acceptor pairs, employing various processing conditions to realize optimal morphology for high efficiency and stable OSCs is a strenuous task. Therefore, comprehensive correlations between processing conditions and morphology evolution pathways have to be developed for efficient performance and stability of devices. Within the framework of the blend system, crystallization transitions of NFA molecules are tracked utilizing the first heating scan of differential scanning calorimeter (DSC) measurement correlating with respective morphology evolution of blend films. Real-time dynamics measurements and morphology characterizations are combined to provide optimal morphology transition pathways as NFA molecules are shown to be released from the mixed phase to form balanced ordered packing with variant processing conditions. Polymer:NFA films are fabricated using blade coating incorporating solvent additive or thermal annealing as processing conditions as a correlation is formulated between performance and stability of solar cells with morphology transition pathways. In conclusion, this work demonstrates the significance of processing condition-controlled transition pathways for the realization of optimal morphology leading to superior OSC devices.

14 SOLAR ENERGY↗

DOE OSTI2021

Effects of Ink Formulation on Construction of Catalyst Layers for High-Performance Polymer Electrolyte Membrane Fuel Cells

Rational design of catalyst layers in a membrane electrode assembly (MEA) is crucial for achieving high-performance polymer electrolyte membrane fuel cells. Establishing a clear understanding of the property (catalyst ink)–structure (catalyst layer)–performance (MEA) relationship lays the foundation for this rational design. Here, a synergistic approach was taken to correlate the ink formulation, the microstructure of catalyst layers, and the resulting MEA performance to establish such a property–structure–performance relationship. The solvent composition (n-PA/H 2 O mixtures) demonstrated a strong influence on the performance of the MEA fabricated with an 830-EW (Aquivion) ionomer, especially polarization losses of cell activation and mass transport. The performance differences were studied in terms of how the solvent composition affects the catalyst/ionomer interface, ionomer network, and pore structure of the resulting catalyst layers. The ionomer aggregates mainly covered the surface of catalyst aggregates acting as oxygen reduction reaction active sites, and the aggregate sizes of the ionomer and catalyst (revealed by ultrasmall angle X-ray scattering and cryo-transmission electron microscopy) were dictated by tuning the solvent composition, which in turn determined the catalyst/ionomer interface (available active sites). In n-PA/H 2 O mixtures with 50~90 wt % H 2 O, the catalyst agglomerates could be effectively broken up into small aggregates, leading to enhanced kinetic activities. The boiling point of the mixed solvents determined the pore structure of ultimate catalyst layers, as evidenced by mercury porosimetry and scanning electron microscopy. For mixed solvents with a higher boiling point, the catalyst–ionomer aggregates in the ink tend to agglomerate during the solvent evaporation process and finally form larger catalyst–ionomer aggregates in the ultimate catalyst layer, resulting in more secondary pores and thus lower mass transport resistance. Both the enlarged catalyst/ionomer interface and appropriate pore structure were achieved with the catalyst layer fabricated from an n-PA/H 2 O mixture with 90 wt % H 2 O, leading to the best MEA performance.

25 ENERGY STORAGE↗

DOE OSTI2024

Chemical recycling of mixed textile waste

Globally, less than 0.5% of postconsumer textile waste is recycled, with the majority incinerated or ending up in landfills. Most postconsumer textiles are mixed fibers, complicating mechanical recycling due to material blends and contaminants. Here, we demonstrate the chemical conversion of postconsumer mixed textile waste using microwave-assisted glycolysis over a ZnO catalyst followed by solvent dissolution. This approach electrifies the process heat while allowing rapid depolymerization of polyester and spandex to their monomers in 15 minutes. A simple solvent dissolution enables the separation of cotton and nylon. We assess the quality of all components through extensive material characterization, discuss their potential for sustainable recycling, and provide a techno-economic analysis of the economic feasibility of the process.

Science & Technology - Other Topics↗

NASA NTRS1985

Elastomeric Cathode Binder

Soluble copolymer binder mixed with cathode material and solvent forms flexible porous cathode used in lithium and Ni/Cd batteries. Cathodes prepared by this process have lower density due to expanding rubbery binder and greater flexibility than conventional cathodes. Fabrication procedure readily adaptable to scaled-up processes.

Yen, S. P. S.↗

DOE OSTI2022

An Integrated Flame Spray Process for Low Cost Production of Battery Materials for Lithium Ion Batteries and Beyond

The overall objective of this project was to develop an advanced manufacturing technology for Li-ion battery materials production at low cost and in a green chemical process using glycerol as solvent to replace water. It was aimed at developing a prototype pilot production line to reduce production cost by at least 25% to the baseline. During the course of this project, research was conducted to understand spray drying and combustion of eutectic solvent precursors of glycerol and metal salts (acetates) in the formation of mixed metal oxide powders. Reactor design and optimization were done to facilitate spray drying and combustion in powder formation and processing. Various cathode materials powders were produced, including lithium nickel-cobalt-manganese oxide (NCM) and lithium nickel-cobalt-aluminum oxide (NCA). These cathode materials powders were tested in half coin cells for their performances, with materials performances of 160 mAh/g for NCM111 and 200 mAh/g for NCA. NCA powders were also produced using a slurry spray-drying process and tested in full pouch cells. A pilot scale flame assisted spray drying reactor was constructed and demonstrated for its production rate exceeding the target of production rate of four metric tons per year. The work performed in this project has been documented in 9 peer reviewed journal publications, 8 conference presentations, and two IP disclosures/patent applications.

25 ENERGY STORAGE↗

DOE OSTI2024

Mixed-Salt Based Transformational Solvent Technology for CO 2 Capture

SRI International developed a novel, water-lean, mixed-salt-based transformational solvent technology under a U.S. Department of Energy (DOE)/National Energy Technology Laboratory (NETL)-funded project. This advanced mixed-salt process (A-MSP) can be operated with high cyclic CO 2 loading, and the solution can be regenerated with greater than 10 bar CO 2 pressure at temperatures less than 120°C. The team has created a process model and performed a techno-economic evaluation (TEA) to identify development pathways for technology advancement. The A-MSP will provide a reduction in the CO 2 capture cost and energy penalties and will have the potential for accelerated scale-up to meet the DOE’s new target of <30/tonne-CO 2 by 2030 for coal-fired power plant applications.

01 COAL, LIGNITE, AND PEAT↗

NASA NTRS1982

Isothermal separation processes

The isothermal processes of membrane separation, supercritical extraction and chromatography were examined using availability analysis. The general approach was to derive equations that identified where energy is consumed in these processes and how they compare with conventional separation methods. These separation methods are characterized by pure work inputs, chiefly in the form of a pressure drop which supplies the required energy. Equations were derived for the energy requirement in terms of regular solution theory. This approach is believed to accurately predict the work of separation in terms of the heat of solution and the entropy of mixing. It can form the basis of a convenient calculation method for optimizing membrane and solvent properties for particular applications. Calculations were made on the energy requirements for a membrane process separating air into its components.

England, C.↗

DOE OSTI2022

Teaching an Old Reagent New Tricks: Synthesis, Unusual Reactivity, and Solution Dynamics of Borohydride Grignard Compounds

Grignard reagents of general formula RMgX (X = Cl - , Br - , I - ) have been utilized in various chemistries for over 100 years. Here, we report that replacing the halide in a Grignard reagent with a reactive borohydride anion adds a new synthetic dimension for these influential compounds. Here, we synthesized the series RMgBH 4 (R=Et, n-Bu, Ph, Bn) and characterized the reactivity toward both organic and inorganic molecules. Using butylmagnesium borohydride (BuMgBH 4 ) as an exemplar, we demonstrate that these compounds possess unique reactivity due to the presence of reducing borohydride groups, resulting in tandem reactivity with organic amides/esters to generate secondary and primary alcohols. Molecular dynamics simulations indicate the stability of BuMgBH 4 is comparable to that of Mg(BH 4 ) 2 + MgBu 2 , validating the Schlenk equilibrium in borohydride Grignard compounds. Metadynamics simulations confirm that the equilibrium is kinetically accessible through solvent-mediated processes. BuMgBH 4 also reacts with CO 2 and NH 3 , revealing potential uses for CO 2 utilization and as a mixed-anion metal borohydride/amide precursor.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Cooperative Role of Mixed Solvent in the Evaporation-Induced Self-Assembly of Polypeptoid Nanocrystals

Peptoids, or polypeptoids, are biomimetic polymers that can self-assemble into nanocrystals for biomedical and biotechnological applications. Polypeptoid nanocrystals can be prepared by evaporation-induced self-assembly, but the roles of solvent components for this process have long been overlooked at the molecular level, leaving a tunable parameter for improving self-assembly protocols. This work utilized molecular dynamics simulations to study the effects of water and the commonly used tetrahydrofuran (THF) on the assembly of nanosheets from molecules of acetylated diblock polypeptoid, poly-(N-decylglycine)-b-poly-(N-2-(2-(2-methoxyethoxy)-ethoxy) ethylglycine), abbreviated as Ac-Ndc10-Nte10. To probe the stages of self-assembly, isolated molecules and preassembled nanofibers/nanosheets were simulated in pure THF, water, and their mixtures, respectively. The assembly energies show that the THF/water mixture has a greater tendency to form nanosheets than pure water. In a THF/water mixture, polypeptoids were found more uncoiled in isolated states, less compact in disordered agglomerates, and with reduced requirement for the Nte block to cover hydrophobic Ndc surfaces in the nanocrystals. Mixed solvent is vital to initiating self-assembly, as THF assists in the opening of coiled polypeptoid molecules, while water provides the thermodynamics to aggregate and ultimately form nanocrystals. To obtain wider nanosheets, it is recommended that some THF be maintained in the aqueous solvent before it becomes exhausted by evaporation. Near the nanosheet surface, the THF concentration is higher than that in bulk solution (3-4 times in 4 M THF/water). The strong adsorption of THF indicates the self-assembly in a de facto mixed solvent. These results are expected to guide the refinement of evaporation-induced self-assembly protocols for polypeptoid nanocrystals.

Luo, Xubo↗

DOE OSTI2024

Functionalization of Cathode–Electrolyte Interface with Ionic Liquids for High-Performance Quasi-Solid-State Lithium–Sulfur Batteries: A Low-Sulfur Loading Study

We introduce a quasi-solid-state electrolyte lithium-sulfur (Li–S) battery (QSSEB) based on a novel Li-argyrodite solid-state electrolyte (SSE), Super P–Sulfur cathode, and Li-anode. The cathode was prepared using a water-based carboxymethyl cellulose (CMC) solution and styrene butadiene rubber (SBR) as the binder while Li6PS5F0.5Cl0.5 SSE was synthesized using a solvent-based process, via the introduction of LiF into the argyrodite crystal structure, which enhances both the ionic conductivity and interface-stabilizing properties of the SSE. Ionic liquids (IL) were prepared using lithium bis(trifluoromethyl sulfonyl)imide (LiTFSI) as the salt, with pre-mixed pyrrolidinium bis(trifluoromethyl sulfonyl)imide (PYR) as solvent and 1,3-dioxolane (DOL) as diluent, and they were used to wet the SSE–electrode interfaces. The effect of IL dilution, the co-solvent amount, the LiTFSI concentration, the C rate at which the batteries are tested and the effect of the introduction of SSE in the cathode, were systematically studied and optimized to develop a QSSEB with higher capacity retention and cyclability. Interfacial reactions occurring at the cathode–SSE interface during cycling were also investigated using electrochemical impedance spectroscopy, cyclic voltammetry, and X-ray photoelectron spectroscopy supported by ab initio molecular dynamics simulations. This work offers a new insight into the intimate interfacial contacts between the SSE and carbon–sulfur cathodes, which are critical for improving the electrochemical performance of quasi-solid-state lithium–sulfur batteries.

25 ENERGY STORAGE↗

DOE OSTI2026

Solventless, Ambient-Pressure Production of Bio-Based Lactones Over Earth-Abundant, Mixed Metal Oxide Catalysts for Circular Polyesters

Transitioning to a circular plastics economy will require use of renewable feedstocks, energy-efficient processes, and closed-loop recyclable polymers, such as polyesters. A key challenge lies in sustainably sourcing monomers used to make recyclable polyesters. This work presents a catalytic platform utilizing earth-abundant Cu(x)Ca(1-x)O mixed metal oxides for the oxidative dehydrocyclization of bio-based diols to lactones, which are advantaged for energy-efficient ring-opening polymerization. Operating below 200 degrees C, at ambient pressure, and without solvent, the process uses air as the sole oxidant, achieving high yields of lactones across a broad substrate scope of C4-8 diols in the liquid phase. The oxidative dehydrocyclization reaction is thermodynamically downhill due to water formation and energy-efficient compared to incumbent, non-redox pathways utilized in fossil carbon-based industrial processes for lactone production. Mechanistic studies reveal facile redox cycling of Cu2+-O(Ca2+)-Cu2+ interfacial sites unique to the developed catalyst. Techno-economic analysis and life cycle assessment estimate 40% lower energy demand and 15% lower GHG intensity per mass of butyrolactone produced compared to the fossil carbon-based route. Liquid-phase oxidative dehydrocyclization offers a promising approach for scalable lactone production from renewable, bio-based diols to enable circular polyesters.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Advanced CO 2 Capture Solvent Systems for Dynamic Power Generation: Quarterly Research Performance Progress Report, QR4 (Q4FY24)

We developed an integrated Computational Fluid Dynamics (CFD) model to simulate the multi-physics coupled cooling process of mixed gas by cold water within a Direct Contact Cooler (DCC) equipped with a rotating packing bed (RPB). The model captures the interactions between fluid dynamics, heat transfer, mass transport, and phase transitions, while accounting for key operational variables such as RPB rotational speed and the mass flow rates of both liquid and gas. The CFD model has been validated using experimental data, specifically by comparing predicted outflow gas and liquid temperatures to measured results. Our findings demonstrate the significant effects of RPB rotational speed and mass flow rates on cooling performance, providing valuable insights for optimizing DCC efficiency in industrial applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2020

Universal and versatile morphology engineering via hot fluorous solvent soaking for organic bulk heterojunction

After explosive growth of efficiency in organic solar cells (OSCs), achieving ideal morphology of bulk heterojunction remains crucial and challenging for advancing OSCs into consumer market. Herein, by utilizing the amphiphobic nature and temperature-dependent miscibility of fluorous solvent, hot fluorous solvent soaking method is developed to optimize the morphology with various donor/acceptor combinations including polymer/small-molecule, all-polymer and all-small-molecule systems. By immersing blend film into hot fluorous solvent which is utilized as liquid medium with better thermal conductivity, the molecular reorganization is accelerated. Furthermore, fluorous solvent can be miscible with the residue of chloroform and chloronaphthalene above upper critical solution temperature. This mixed solvent diffuses around inside the active layer and selectively promotes molecular reorganization, leading to optimized morphology. Compared to widely-used thermal annealing, this approach processed under mild conditions achieves superior photovoltaic performance, indicating the practicality and universality for morphological optimization in OSCs as well as other optoelectronic devices.

14 SOLAR ENERGY↗

NASA NTRS1973

Preparation of prepreg graphite tape with insoluble polymer

Powdered polymer is finely ground. Second polymer, soluble, is mixed with appropriate solvent. Milled polymer and graphite filaments are added to soluble polymer-solvent solution to create slurry. Slurry is dried, and when ready for processing, the soluble, binder-polymer is removed by heat during precure or cure cycle.

Yates, C. I.↗