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All sources NASA NTRS DOE OSTI

DOE OSTI2026

Identifying Bounds of Inorganic Content in Solventless Processing of Hybrid Solid Electrolytes

Solid-state lithium batteries require safe, robust electrolytes to enable higher energy densities and improved safety over conventional cells. Hybrid polymer–ceramic electrolytes are a promising solution, combining the processability of polymers with the high ionic conductivity and mechanical strength of inorganic fillers. In this work, we demonstrate a solventless, UV-curing method to produce hybrid solid electrolytes using a poly(ethylene glycol) dimethyl ether (PEGDME)-based photocurable matrix incorporating Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 (LAGP) or Li 7 La 3 Zr 2 O 12 (LLZO) ceramic electrolyte. Inorganic filler loadings up to ∼55 wt.% could be successfully incorporated via this process which was the highest inorganic content at which the slurry remains processable and cured into a uniform film. The resulting UV-cured composite electrolytes remain flexible and exhibit room-temperature ionic conductivities on the order of 10 −4 S·cm −1 , along with notably improved lithium-ion transference numbers compared to conventional polymer electrolytes. Similar performance and processing limits were observed for both LAGP and LLZO, indicating that ceramic filler chemistry does not significantly affect the UV-curing process or the electrolyte's ion transport properties in this regime. Eliminating solvents from fabrication not only simplifies processing and mitigates environmental concerns but also enables higher solid contents that enhance mechanical strength and help suppress lithium dendrite formation. In conclusion, this scalable approach thus paves the way for manufacturing robust composite solid electrolytes for next-generation solid-state batteries (SSBs).

Batteries↗

NASA NTRS1998

Development of a Convergent Spray Technologies(tm) Spray Process for a Solventless Sprayable Coating, MCC-1

This paper discusses the application of Convergent Spray Technologies (TM) Spray Process to the development and successful implementation of Marshall Convergent Coating (MCC-1) as a primary Thermal Protection System (TPS) for the Space Shuttle Solid Rocket Boosters (SRBs). This paper discusses the environmental and process benefits of the MCC-1 technology, shows the systematic steps taken in developing the technology, including statistical sensitivity studies of about 35 variables. Based on the process and post-flight successes on the SRB, it will be seen that the technology is "field-proven". Application of this technology to other aerospace and commercial programs is summarized to illustrate the wide range of possibilities.

Patel, Anil K.↗

NASA NTRS2000

Marshall Convergent Coating Development Team: An Aerospace Success Story

The external thermal insulation systems for the Space Shuttle solid rocket boosters and the Air Force Titan IV payload fairings were in jeopardy due to EPA regulatory problems, endangering the flight status of both vehicles. The Marshall Convergent Coating (MCC-1) Development Team was formed in February 1994 to develop and implement an EPA-compliant external thermal insulation system for both systems. MCC-1 made use of a process known as Convergent Spray Technology (CST), a solventless, sprayable process that eliminated the environmentally hazardous chemicals involved with the old methods. Implemented in record time, the new insulation was so successful that it was selected for two additional flight vehicles, Boeing's Sea Launch and Delta TV. The activity also led to commercial spin-off pilot projects. The team continues today to share data between the various production sites, resolve production issues, expand the material's use, and consider potential improvements for the future.

Lester, Carl N.↗

DOE OSTI2026

Accelerating Laboratory-Based, All-Solid-State Battery Research and Development: Industrially Relevant Small-Batch Dry-Processing, Small and Low-Cost Test Fixtures, and Short-Tolerant Separators

This work presents improvements to mixing (for dry-processed electrodes), separator robustness, and cell testing jigs for all-solid-state batteries (ASSBs). These developments combine synergistically to enable rapid research and development of ASSB catholytes. A mechanical "kneader" is designed and built which emulates the mixing and fibrillation of poly-tetrafluoroethylene binder that occurs in industrially relevant twin-screw extruders. A modest improvement in the mixing and dispersion catholyte materials is observed using micro-resolution X-ray computed tomography (X-ray CT). Catholytes are paired with an In-metal anode and separated by a novel, dual-layer, polyaramid-fiber-supported, sulfide-solid electrolyte (Li6 PS5 Cl) separator. This separator achieves high short tolerance which enabled a 95% success rate across 20 attempted cells and to date over 100 successful cells have been built. ASSBs were tested in a 2032 coin-cell format. Simultaneous cycling of a large number of cells is further enabled by a compact and low cost (~ 38 USD per jig) pressure application jig of which 100 have been constructed to date. The utility of these advances is demonstrated through a brief study on the effect cathode-side conductive carbon and current collector type has on capacity and rate performance.

25 ENERGY STORAGE↗

NASA NTRS1998

The Successful Transfer of Space Derived Convergent Spray: An Application for Industrial Roof Coatings and Interstate Bridge Repair

A partnership was formed between the National Aeronautics and Space Administration (NASA), the Environmental Protection Agency (EPA), and United Technologies USBI Company to develop, demonstrate, and evaluate a technology that uses a solventless spray process for depositing a lightweight, highly filled roof coating on low-sloped commercial roofs. Although the levels of volatile organic compound (VOC) emissions from industrial roof coating's and paint operations have been reduced in recent years, this partnership,was an effort to further reduce VOC emission levels and to also demonstrate the use of reclaimed automobile tire rubber as a filler material in roof coating systems. Different materials and coatings were evaluated and tested before the final selection used to coat the roofs of two small buildings at NASA's Marshall Space Flight Center during fiscal year 1997. The project successfully leveraged the investment of EPA, NASA and private sector resources to demonstrate a pre-commercial roofing coating process. This process utilizes the Convergent Spray Technologies process, which was initially developed by USBI to apply highly-filled, thermal protection coatings to the Space Shuttle Solid Rocket Boosters. A second partnership between the NASA, Federal Highway Administration, Alabama Department of Transportation and USBI Company was formed to develop and demonstrate the Convergent Spray Technology as a method of applying a skid resistant coating to interstate roads and concrete bridge decking's. Again, different materials and coatings were evaluated and tested before the final selection of ground flint and resin. Two field demonstrations were performed during fiscal year 1997 for the purpose of evaluating the coating system under actual highway conditions. These coatings were applied on Interstate 65 near Huntsville Alabama, and in the Mobile Bankhead tunnel. The system performed this task without the use of harmful solvents, and accomplished the process in a single application. This project successfully leveraged the investment of NASA, Federal Highway Administration, the Alabama Department of Transportation, and private sector funding.

McMillan, Vernotto C.↗

NASA NTRS1980

Tackifier for addition polyimides

A modification to the addition polyimide, LaRC-160, was prepared to improve tack and drape and increase prepeg out-time. The essentially solventless, high viscosity laminating resin is synthesized from low cost liquid monomers. The modified version takes advantage of a reactive, liquid plasticizer which is used in place of solvent and helps solve a major problem of maintaining good prepeg tack and drape, or the ability of the prepeg to adhere to adjacent plies and conform to a desired shape during the lay up process. This alternate solventless approach allows both longer life of the polymer prepeg and the processing of low void laminates. This approach appears to be applicable to all addition polyimide systems.

Butler, J. M.↗

NASA NTRS1998

Development of CST(registered) for a Solventless Sprayable Coating, MCC-1

This paper discusses an innovative process called convergent spray technology (CST), as applied to the development and successful implementation of MCC-1 coating for the Shuttle/SRB as a primary Thermal Protection System (TPS). The session will illustrate the environmental and the process benefits of the MCC-1 technology, show the systematic steps taken for the development of the technology that included statistically conducted sensitivity studies of about 34 variables, and illustrate that the technology is "Field-proven" based on the process and post-flight successes on the Shuttle/SRB. The application of this technology to other aerospace and commercial programs will be introduced to illustrate the wide range of possibilities.

Patel, A. K.↗

NASA NTRS1978

Solventless LARC-160 Polyimide Matrix Resin

The addition polyimide, LARC-160, which was originally synthesized from low cost liquid monomers as a laminating resin in ethanol, was prepared as a solventless, high viscosity, neat liquid resin. The resin was processed by hot-melt coating techniques into graphite prepreg with excellent tack and drape. Comparable data on graphite reinforced laminates made from solvent-coated and various hot-melt coated prepreg were generated. LARC-160, because of its liquid nature, can be easily autoclave processed to produce low void laminates. Liquid chromatographic fingerprints indicate good reaction control on resin scale ups. Minor changes in monomer ratios were also made to improve the thermal aging performance of graphite laminates.

Stclair, T. L.↗

NASA NTRS1981

Tackifier for addition polyimides containing monoethylphthalate

An improvement of addition polyimides wherein an essentially solventless, high viscosity laminating resin is synthesized from low cost liquid monomers is disclosed. The improved process takes advantage of a reactive, liquid plasticizer such as monoethylphthalate (MEP) which is used in lieu of an alcohol solvent, and helps solve a major problem of maintaining good prepreg tack and drape, or the ability of the prepreg to adhere to adjacent plies and conform to a desired shape during the layup process. This improvement results in both longer life of the polymer prepreg and the processing of low void laminate and appears to be applicable to all addition polyimide systems.

St.clair, T. L.↗

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 OSTI2025

Thermodynamically leveraged solventless aerobic deconstruction of polyethylene-terephthalate plastics over a single-site molybdenum-dioxo catalyst

Here, we describe the solventless catalytic deconstruction of polyethylene-terephthalate (PET) under an aerobic atmosphere, mediated by an earth-abundant, low-cost activated carbon (AC)-supported single-site molybdenum-dioxo catalyst (AC/MoO 2 ). Catalytic amounts of AC/MoO 2 selectively convert waste PET into its monomer, terephthalic acid (TPA), within 4 h at 265 °C with yields as high as 94% under 1 atm air. Pure crystalline TPA product sublimes from the reaction hot zone, crystallizing on the reactor cold zone, thus avoiding the need for separation and purification steps. This process does not employ any hazardous/toxic reducing agents or solvents, and the catalyst can be recycled multiple times without loss of activity, rendering this process highly atom-efficient. According to computational and experimental mechanistic studies, the AC/MoO 2 catalyst mediates a thermoneutral metal-catalyzed β-scission step, followed by an exothermic step that converts the vinyl benzoate intermediate to TPA and acetaldehyde using trace amounts of moisture in the air. The formation of gaseous acetaldehyde makes the isolation of TPA from the reaction mixture facile and industrially favorable, especially since solvents are unnecessary. The present methodology is also extended to the deconstruction of other frequently used polyester plastics, polybutylene terephthalate (PBT), polyethylene naphthalate (PEN), and polyethylene furanoate (PEF), and operates equally well with post-consumer waste products. Notably, this process is also compatible with plastic mixtures of polyesters with polyolefins, polyamides, and polycarbonates, leading to the selective conversion of each polyester to the corresponding monomer, leaving the residual polymer unchanged and polyester-free.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Solventless Dual‐Cure Liquid Resins Via Circular Use of Phthalic Anhydride for Recyclable Composite Applications

Abstract Fiber‐reinforced composites (FRCs) possess a remarkable strength‐to‐weight ratio, making them ideal light‐weighing alternative materials of metals used in automotive, aerospace, and outdoor equipment applications, but their recycling is challenging. Chemically recyclable thermoset polymers can enable fiber recovery and reuse; however, challenges remain in the separation and purification of depolymerized small molecules for efficient polymer recycling. To this end, a series of liquid resins for chemically recyclable polymer networks is designed based on phthalic anhydride, a widely produced and inexpensive chemical. The straightforward sublimation of phthalic anhydride is leveraged to enable a simple and efficient separation process for polymer recycling. To liquefy phthalic anhydride, five mono‐acryloyl‐phthalates are synthesized to obtain stable liquid resins together with phthalic diglycidyl ester. These liquid resins undergo dual‐cure reactions that comprise photopolymerization of acrylate and, subsequently, heat‐mediated epoxy‐acid polymerization reactions. These liquid resins exhibit moderate viscosities (2600–6400 cP @ 22 °C), fast curing, and robust thermomechanical properties (T g s from 71 to 116 °C). It is demonstrated that hydrolysis of the dual‐cured polymers completes within 2 h at 80 °C, and direct sublimation produces phthalic anhydride with 82% yield. This resin system is expected to provide a cost‐competitive, highly efficient platform for recyclable FRCs.

Polymer Science↗