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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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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Anion exchange membranes based on (3-acrylamidopropyl) trimethylammonium chloride (APTA) and phenyl Acrylate: Impact of crosslinker and crosslinker content on physiochemical properties and transport behavior of acetate and formate

CO 2 reduction cells are innovative devices that convert CO 2 into valuable chemicals, such as formate (OFm - ) and acetate (OAc - ), at the cathode. One of the key challenges in these devices is the development of ion exchange membranes that enable the transport of charge carriers between electrodes while minimizing the transfer of CO 2 reduction products. This study focuses on the preparation and characterization of crosslinked anion exchange membranes (AEMs) made of phenyl acrylate (PA) and (3-acrylamidopropyl) trimethylammonium chloride (APTA), crosslinked with either poly(ethylene glycol) diacrylate (PEGDA) or N,N’-methylenebisacrylamide (MBAA). Here, the membranes are characterized to understand their physiochemical properties and corresponding transport behavior through characterization of water volume fraction, mechanical properties, ionic conductivity, ion exchange capacity, water contact angle, glass transition temperature as well as their permeability and solubility to formate and acetate. MBAA crosslinked membranes exhibit higher Young’s modulus and lower strain at break compared to PEGDA-crosslinked membranes, which is attributed to their shorter chain length. Within a series of membranes of varied comonomer content, for either PEGDA or MBAA as crosslinker, permeabilities generally follow free volume theory (increasing permeability with increasing water content where water content increases with decreasing crosslinker content). Interestingly, for membranes with different crosslinkers but analogous water volume fraction significant differences (∼2 orders of magnitude) in permeability are observed which we attribute to differences in chain mobility as characterized through the glass transition temperature.

25 ENERGY STORAGE↗
DOE OSTI2026

Effects of cleavable comonomer structure and crosslinker chemistry on the performance and deconstructability of frontally cured pDCPD composites

Reclaiming undamaged carbon fiber from thermoset composites requires chemical recycling methods that leverage complete deconstruction of the polymer matrix. Cleavable comonomers enable chemical recycling of poly(dicyclopentadiene) (pDCPD) composites, but current systems suffer from reduced glass transition temperature (T g ), limiting application. Here, we investigate the effect of cleavable comonomer loading and cleavable crosslinker chemistry on network formation, thermomechanical properties, and fiber recovery in frontally cured pDCPD composites. All formulations fully deconstructed in acid and recovered fibers ranged from pristine to variably contaminated depending on crosslinker chemistry. Reducing backbone-cleaving comonomer content and introducing cleavable crosslinkers raised composite T g to 126–138 °C compared to 105 °C previously reported in deconstructable pDCPD composites. Although the cleavable crosslinkers increased T g in unreinforced polymers to 150–160 °C, the fiber-reinforced composite T g remained lower due to under-curing and interactions between the crosslinkers and the fiber surface. Increasing polymerization initiator loading improved comonomer conversion and yielded a deconstructable composite with T g = 151 °C, approaching the performance of non-deconstructable pDCPD composites (T g = 161 °C). This work clarifies how cleavable comonomer and crosslinker chemistry governs curing, thermomechanical performance, and reclaimed reinforcement quality, and the results highlight the need for more robust cleavable comonomers to realize multigenerational composite materials without sacrificing thermomechanical performance.

Carbon fibers↗
DOE OSTI2025

Ion Transport in Concentrated Crosslinked Solid Polymer Electrolytes

Crosslinking polymers is a common approach to create mechanically stable solid materials such as polymer electrolytes for lithium batteries. In conventional liquid electrolytes, the solvent molecules move freely to accommodate the field-induced motion of ions. However, in crosslinked polymer electrolytes, the rearrangement of polymer segments is constrained by the deformation limits of the network. Herein, we develop a new transport model that accounts for both the formation of concentration gradients and the elasticity of the electrolyte. The elasticity is incorporated by adding an additional term related to the entropy of crosslinked strands to the electrochemical potential of the salt. The resulting Crosslink Model contains two adjustable parameters: $\mathcal{N}$, the average number of monomers in a strand, and λ crit , the maximum strain the network can sustain. These solid-like constraints produce singularities in the governing transport equations, fundamentally altering the concentration profiles. Plateaus in salt concentrations emerge near the electrodes, and network elasticity introduces a strain overpotential. When compared to a Baseline Model ($\mathcal{N}$ → ∞, equivalent to concentrated solution theory), which predicts steepest gradients near the electrodes, both models yield similar current–voltage relationships. Model predictions are compared to electrochemical data for a poly(ethylene oxide)-based crosslinked polymer electrolyte.

Patel, Vivaan [University of California, Berkeley,↗
DOE OSTI2025

Crosslinked polymeric ionic liquid stationary phases incorporating a combination of silver(I) and copper(II) ions for olefin separations by gas chromatography

The development of efficient and selective olefin separation technologies is a critical challenge within the chemical industry given the high energy demands of conventional cryogenic distillation methods. To address this, the study explores the effectiveness of polymeric ionic liquid (PIL) stationary phases in gas chromatography (GC) that incorporate both silver(I) ([Ag + ]) and copper(II) ([Cu 2+ ]) ions for enhanced olefin separation via π-complexation interactions. Further, the effects of both non-crosslinked and crosslinked PIL stationary phases containing varying ratios of [Ag⁺] and [Cu²⁺] ions were systematically investigated to evaluate their impact on the separation of olefins from paraffins and structurally similar olefins. Retention measurements using a broad range of olefinic probes revealed that [Ag⁺] ions provided stronger and more consistent π-complexation in PIL-based stationary phases, while [Cu²⁺] ions preferentially enhance olefin retention in crosslinked systems. Furthermore, thermal stability studies showed that [Ag + ]-containing PIL stationary phases maintain stable olefin separation efficiency over prolonged exposure under elevated temperatures, while crosslinked PIL stationary phases containing [Cu 2+ ] ions exhibited stronger retention due to increased surface adsorption. These findings provide insight into the tunability of metal–olefin interactions using PIL-based stationary phases and suggest design strategies for achieving thermally stable and highly selective chromatographic separations of unsaturated hydrocarbons.

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

Site-specific photo-crosslinking in a double crossover DNA tile facilitated by squaraine dye aggregates: advancing thermally stable and uniform DNA nanostructures

We investigated the role of dichloro-squaraine (SQ) dye aggregates in facilitating thymine–thymine interstrand photo-crosslinking within double crossover (DX) tiles, to develop thermally stable and structurally uniform two-dimensional (2D) DNA-based nanostructures. By strategically incorporating SQ modified thymine pairs, we enabled site-selective [2 + 2] photocycloaddition under 310 nm UV light. Strong dye–dye interactions, particularly through the formation of aggregates, facilitated covalent bond formation between proximal thymines. To evaluate the impact of dye aggregation on crosslinking efficiency, ten DX tile variants with varying SQ-modified thymine positions were tested. Our results demonstrated that SQ dye aggregates significantly enhanced crosslinking, driven by precise SQ-modified thymine dimer placement within the DNA tiles. Analytical techniques, including denaturing PAGE and UV-visible spectroscopy, validated successful crosslinking in DNA tiles with multiple SQ-modified thymine pairs. This non-phototoxic method offers a potential route for creating thermally stable, homogeneous higher-order DNA–dye assemblies with potential applications in photoactive and exciton-based fields such as optoelectronics, nanoscale computing, and quantum computing. Furthermore, the insights from this study establish a foundation for further exploration of advanced DNA–dye systems, enabling the design of next-generation DNA nanostructures with enhanced functional properties.

2D DNA template↗
DOE OSTI2025

Ultrahigh pressure compaction-resistant thin film crosslinked composite reverse osmosis membranes

In this study, we present a class of thin-film crosslinked (TFX) composite reverse osmosis (RO) membranes that resist physical compaction at ultrahigh pressures (up to 200 bar). Since RO membranes experience compaction at virtually all pressure ranges, the ability to resist compaction has widespread implications for RO membrane technology. The process described herein involves crosslinking a phase inverted porous polyimide (PI) support membrane followed by interfacial polymerization of a polyamide layer, thereby forming a fully thermoset composite membrane structure. We explore a range of phase inversion membrane formation parameters such as PI concentration, solvent-cosolvent ratios, coagulation bath composition, and crosslinking methods in addition to interfacial polymerization reaction chemistry and conditions. Overall, TFX membranes exhibit significantly less compaction compared to hand-cast and commercial high-pressure RO membranes, experiencing less than 10% decline in water permeance and maintaining salt rejection over 99% for NaCl solutions up to 180,000 mg/L with 200 bar applied pressure.

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

Investigating the Crosslinking, Degradation, and Adhesion Behavior of Photovoltaic Encapsulants Under Thermal Accelerated Aging

Degradation of photovoltaic (PV) module encapsulant characteristics that lead to mechanical embrittlement and delamination remains a cause of failure in solar installations. A multiscale reliability model connecting the encapsulant mechanical and fracture properties to the degraded molecular structure and interfacial bonding to adjacent solar cell and glass substrates was previously published. The model, developed primarily for poly(ethylene-co-vinyl acetate) acetate (EVA) encapsulants, remains to be experimentally validated. Determining the degradation and crosslinking kinetics of alternative encapsulants, such as polyolefin elastomer (POE) and EVA/POE/EVA composites (EPE), can generalize the model. In this work, we subject fully cured EVA, POE, and EPE encapsulants to accelerated thermal aging to determine how high temperatures impact reaction kinetics. An increase in gel content (crosslinking) and decrease in crystallinity of the encapsulants under hot-aerobic (90 degrees C, 22% RH) and hot-anaerobic (90 degrees C, sealed in N 2 air) aging were observed, even in the absence of UV and crosslinking initiators. Fourier transform infrared spectroscopy (FTIR)-attenuated total reflectance analysis showed insignificant encapsulant degradation, demonstrating the critical role of UV and moisture in accelerating degradation. Adhesion testing performed on coupon-level specimens (cell/encapsulant/glass laminates) showed decreases in adhesion energy, Gc , from 5000 h of hot-dry (90 degrees C, ~1% RH) and hot-humid (90 degrees C, 60% RH) aging. POE coupons demonstrated the best stability, followed by EPE then EVA. For EVA and POE, hot-humid aged coupons experienced a larger decrease in Gc due to enhanced hydrolytic degradation. Hot-dry aging condition demonstrated that thermal degradation of the interface could be significant even if the encapsulant experiences negligible degradation in the absence of UV and elevated humidity.

accelerated aging↗
DOE OSTI2025

B‐Staging and Crosslinking of Polycarbosilane at Room Temperature: Cure Mechanism and Properties

The viscosity of polycarbosilane (PCS) polymers is not advantageous for free forming. Various fillers and heat are used to obtain a formable paste. Due to the low yield stress, structures and preforms tend to slump or resin will flow out, especially during the curing of the polymer. B-staging of PCS allows for a more stable structure from room temperature until the full cure of the allyl groups occurs with heat. Additionally, hydrosilation is an effective means of crosslinking at room temperature and controlling viscosity. A network structure was formed in SMP-10 using silane and a vinyl-based crosslinker to bridge each polymer chain. Pt addition catalysts were added to enhance the increase in viscosity to make a lightly crosslinked gel to aid in thickening and forming and to improve the ceramic yield at 1000°C. In conclusion, this enables several options for controlling rheology and improving the properties of preceramic polymers to avoid slumping during curing.

inorganic polymers↗
DOE OSTI2025

Isomerization kinetics of azobenzene crosslinked to a liquid crystal polymer network

Azobenzene is an important chromophore having numerous applications that are a direct implication of its ability to change shape upon irradiation with a suitable wavelength. Here, in this study, photoisomerization kinetics of a diacrylate azobenzene molecule (A3MA) cross-linked to a liquid crystal polymer network (LCN) is investigated. Isomerization experiments were conducted on planar LCN thin films with varying cross-linking densities for a fixed azobenzene concentration. The experiments were conducted at approximately 26 °C, which is significantly below each film’s glass transition temperature. The forward trans-cis and reverse cis-trans isomerization slows down in crosslinked azobenzene liquid crystal polymer networks (ALCNs) as compared to a solution and an uncrosslinked polymer mixture. The observed slowdown is due to the reduction in the free volume and increased steric hindrances with an increase in crosslinking. A single-term first-order kinetics rate equation is known to describe the isomerization kinetics in solutions or uncrosslinked mixtures while the same form fails to represent the reaction kinetics in moderate to highly cross-linked ALCNs. Our results for the first time indicate that a two-term first-order reaction rate is an accurate way to describe the forward trans-cis and reverse thermal cis-trans isomerization in crosslinked azobenzene liquid crystal polymer networks. In addition, the effect of film thickness and incident intensities on the reaction kinetics is investigated. Finally, the two-term isomerization kinetics is incorporated into a finite element photo-chemo-mechanical model to reveal the consequent slowdown in the actuation response of ALCN films. The current findings will be of particular interest to theoreticians and experimentalists alike, for it will help predict and understand accurately the responses of azobenzene-based coatings, and actuators and may have potential applications in underwater soft robotics.

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

Polyolefin blends with co-continuous architectures enabled by dynamic covalent crosslinking

Blending polymers produces brittle materials due to macrophase separation and poor interfacial adhesion, which is exemplified by mixtures of polyolefins. This presents a formidable challenge for the mechanical recycling of mixed plastic waste. Here, we demonstrate that dynamic covalent crosslinking of immiscible polyolefin blends creates macrophase separated co-continuous architectures, yet they display excellent mechanical properties, which challenges the conventional wisdom regarding morphology-property relationships in polymer blend compatibilization. We find that the position and orientation of dynamic crosslinks and their influence on crystallinity are key to understanding the structure-morphology-property relationships. In particular, high-resolution microscopy imaging reveals alignment of crystallite planes with strong orientational preference, particularly at polymer-polymer interfaces, which contribute to material performance. We further demonstrate that changes in crosslinker density and valency allow the properties of binary and ternary polyolefin blends to be tuned in a modular fashion.

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

Dynamic Diketoenamine Crosslinking Unlocks Vinyl Polymer Vitrimers From β ‐Triketone Chemistry

Covalent adaptable networks (CANs) offer a compelling strategy to unite the mechanical robustness of thermosets with the reprocessability of thermoplastics, yet achieving simultaneous durability, processability, and true recyclability remains challenging. We introduce diketoenamine (DKE) vitrimers derived from β-triketone methacrylate monomers and demonstrate how rational monomer design dictates network processability, viscoelasticity, and recyclability. By systematically varying the spacer length between the β-triketone (TK) moiety and the polymer backbone, we identify a key structure–property relationship that dictates vitrimer behavior. Networks bearing TK pendants minimally displaced from the backbone suppress creep but exhibit limited stress relaxation, whereas extended spacers yield lower glass transition temperatures, higher effective crosslink densities, and efficient stress dissipation, enabling optical transparency and reprocessability. Extending this platform to ultra-high molecular-weight prepolymers introduces physical entanglements as secondary crosslinks, further enhancing dimensional stability without compromising processability. Both mechanical and chemical recycling validate the closed-loop circularity of these materials. Furthermore, these results establish TK methacrylates as a versatile platform for designing high-performance vitrimers that integrate durability, reprocessability, and true closed-loop recyclability.

closed-loop recyclability↗
DOE OSTI2026

Tuning the Mechanical Properties of Crosslinked Copolymers via Sequence and Solvent‐Selective Swelling for Vat Photopolymerization

Block copolymers (BCPs) offer distinct advantages for vat photopolymerization by enabling mechanically programmable network structures through microphase-separated morphologies that can be kinetically trapped during curing, yielding properties unattainable in homogeneous resins. However, the respective roles of repeat-unit sequence and solvent environment, together with their interplay in directing network formation and mechanical performance, remain unclear. Here, we synthesize a series of CO 2 -based polycarbonate copolymers comprising a crosslinkable glassy poly(vinyl cyclohexene carbonate) (PVCHC, A block) and a non-crosslinkable soft poly(propylene carbonate) (PPC, B block). The polymer sequence is systematically varied (ABA, BAB, and statistical), and solvent choice controls block-selective swelling to jointly control gelation behavior, microphase morphology, and mechanical response through changes in the accessibility and local environment of photocrosslinkable vinyl groups during network formation, as revealed by photorheology and small angle x-ray scattering. By tuning polymer sequence and curing solvent, we transform nominally identical formulations from brittle to highly ductile materials, achieving a three-orders-of-magnitude range in toughness (0.003 to 9.1 MJ m −3 ). These results establish clear structure–processing–property relationships and identify polymer sequence and selective solvation as powerful strategies for programming both printability and performance of block copolymer resins for additive manufacturing.

additive manufacturing↗
DOE OSTI2025

Understanding the impact of SPMAK and PEGPEA in crosslinked PEGDA membranes: Methanol-carboxylate co-transport behavior and correlating structure-physicochemical-transport properties

Investigating multicomponent transport in dense, hydrated polymer membranes is necessary in applications such as fuel cells, electrolyzers, and desalination systems. Of particular interest are photoelectrochemical CO 2 reduction cells (PEC-CRC) which produce liquid products such as alcohols (methanol) and carboxylates (formate, acetate). Flux coupling and competitive sorption behavior of these products (solutes) have been found to affect permselectivity, thereby motivating us to investigate fundamental membrane structure-physicochemical-transport relationships. Past research has shown that systematic tuning of crosslinked cation exchange membranes (CEMs) with charge-neutral monoacrylate monomers containing alkyl and phenyl groups (i.e., poly(ethylene glycol) methacrylate (PEGMA), and poly(ethylene glycol) phenyl ether acrylate (PEGPEA)) can suppress acetate transport (permeability) in co-permeation with methanol. To further investigate this transport behavior and to enhance membrane ionic conductivities, 3-sulfopropyl methacrylate potassium (SPMAK), a sulfonated monoacrylate monomer is incorporated here. SPMAK content is varied with neutral PEGPEA and diacrylate crosslinker, poly (ethylene glycol) diacrylate (PEGDA) of two different chain lengths (n = 10 and 13) to prepare membranes of various compositions. Electrochemical and physicochemical properties including ionic conductivity, ion exchange capacity, and water uptake increase with increasing charged SPMAK content. Different states of water within hydrated membranes are probed using differential scanning calorimetry (DSC), where increasing intermediate (loosely bound) water is observed with increasing hydrophilic SPMAK content. The transport behavior of methanol and carboxylates (formate, acetate, propionate) are investigated, where permeabilities vary as methanol > formate > acetate ≈ propionate. Interestingly, permeabilities decrease with increasing PEGPEA content and are more dependent on solute diffusion than sorption. Permeabilities and diffusivities decrease while permselectivities increase with decreasing PEGDA chain length.

25 ENERGY STORAGE↗
DOE OSTI2026

Plasticizer-Free Gradient-Crosslinked Polyurethane Electrolyte for Room-Temperature Solid-State Lithium Batteries

Polymer-based solid-state electrolytes are promising for next-generation lithium metal batteries, yet their limited ionic conductivity and mechanical stability at ambient conditions remain key challenges. Herein, we report a novel gradient crosslinked polymer electrolyte (PU/PUA/PU) synthesized via a sequential in situ UV-curing process that integrates a mechanically robust polyurethane acrylate (PUA) core with soft linear polyurethane (PU) interfaces. This all-solid membrane operates without any liquid plasticizer and the interfacial PU layers ensure low interfacial resistance and intimate electrode contact, while the PUA core provides enhanced dimensional stability and dendrite suppression. As a result, the gradient electrolyte delivers an impressive ∼2.6 × 10 −4 S cm −1 ionic conductivity at 25 °C (two orders of magnitude higher than conventional PEO) and remains electrochemically stable >5 V (vs Li + /Li). Structural analysis confirms the formation of a well-defined crosslinked network with suppressed crystallinity and expanded interchain spacing. Electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV) further validate these properties. When applied in a Li||NMC811 cell, the PU/PUA/PU electrolyte delivers stable cycling with high capacity at both 60 °C and 25 °C, demonstrating its potential for room-temperature solid-state battery applications without reliance on plasticizers or heating. In conclusion, this gradient design offers a practical path toward ambient-condition operation of solid-state lithium batteries, providing a paradigm for overcoming the traditional trade-off between ionic conductivity and mechanical robustness.

25 ENERGY STORAGE↗
DOE OSTI2025

Solution‐Like Water Transport Across Molecular to Macroscopic Length Scales in Crosslinked Poly(Ethylene Glycol Diacrylate) Networks With Tailored Sidechains

Poly(ethylene glycol) (PEG)‐based materials, like PEG‐diacrylate (PEGDA), are prized for their hydrophilic, inert properties, and leveraged in hydrogels and as membrane mimics. While network chemistry is often tuned for selective transport and antifouling, fundamental understanding of water dynamics at the network surface and the impact on bulk transport is limited. We utilize Overhauser dynamic nuclear polarization (ODNP) to measure nanoscale water diffusivity near a tethered spin label at the water‐polymer surface and compare it to bulk water diffusivity from pulsed field gradient (PFG) NMR. Via active ester chemistry, spin labels and varied sidechain chemistries are introduced, modulating network hydrophilicity. Tuning network hydration through crosslinker content and functional groups further impacts water diffusivity. Results show rapid nanoscale water transport at the polymer surface, reflecting network volumetric water content, with further modulation by sidechain functionality. These findings demonstrate PEGDA's utility as a membrane mimic and the critical impact of network chemistry on water transport.

hydrogels↗
DOE OSTI2025

Tunable Crosslinked Ether Polymer Network Electrolytes for High‐Performance All‐Solid‐State Sodium Batteries

All-solid-state batteries (ASSBs) are critical for achieving high energy density and enhanced safety. Solid polymer electrolytes (SPEs) offer key advantages over other electrolytes, including improved safety, flexibility, and interfacial contact. Among the SPEs, ether-based polymers are widely studied due to their ease of processing and high ionic conductivity (σi) in the amorphous state. In this work, the introduction of poly(ethylene glycol) methyl ether methacrylate (PEGMEMA) into an SPE matrix composed of poly(ethylene glycol) diacrylate (PEGDA), poly(ethylene glycol) (PEG2k), and sodium bis(fluorosulfonyl)imide (NaFSI) salt is investigated to facilitate the formation of amorphous, high σ i SPEs through end-group engineering and polymer ratio optimization. PEGMEMA enhances structural integrity via crosslinking with PEGDA through its methacrylate group, while its methyl end group aids ion conduction. A 2:1:7 ratio of PEGDA:PEGMEMA:PEG2k exhibits a σi of 1.16 x 10 -4 S cm -1 and oxidative stability up to 4.4 V at 60 °C. A solid-state cell incorporating this SPE, a Na 2/3 Ni 1/3 Mn 2/3 O 2 (NM12) cathode, and a sodium-metal anode demonstrates excellent cycling stability, retaining over 80 % of its initial capacity for 150 cycles at 60 °C. The findings highlight the potential of end-group engineering in improving the electrochemical performance of SPEs.

25 ENERGY STORAGE↗
DOE OSTI2025

Cohesive instability in elastomers: insights from a crosslinked Van der Waals fluid model

Abstract The resistance to volumetric deformations displayed by polymer networks is largely due to secondary and tertiary interactions between neighboring polymer chains. These interactions are both entropic and enthalpic in nature but are fundamentally different from the entropic forces that resist shearing in these networks. In this paper, we introduce a new depiction of elastomers as a crosslinked Van der Waals fluid. Starting from first principles, we develop constitutive equations that are implemented in a continuum model as well as a discrete network model. Our models predict that the failure of polymer networks may be driven by an instability in the underlying polymer bulk ‘fluid’ or by the breaking of polymer chains, depending on the loading path taken. The results of this study indicate that material failure in elastomers exposed to a purely triaxial state, such as in a poker chip experiment, may be driven by an entirely different mode of instability than those deformed in pure shear, such as in a uniaxial tension experiment.

Lamont, Samuel C.↗
DOE OSTI2026

Functional silicon crosslinks in conjugated polymer networks

The first conjugated polymers with functional Si–Si crosslinks are reported. In addition to complete structural characterization using solid-state NMR techniques, the electronic structure of the polymers are supported by electrochemical studies.

Wentz, Kelsie E. [Department of Chemistry, Johns H↗