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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Hierarchically Structured Vitrimer Biocomposites for Sustainable Manufacturing

Polymers containing dynamic covalent bonds (DCBs) exhibit thermoplastic-like flow above their topology freezing temperature (T v ) while maintaining thermoset-like properties below it, making them promising for sustainable manufacturing. However, their large-scale adoption remains limited due to challenges in accurately determining T v and achieving efficient fiber-matrix bonding in composite applications. Here, hierarchically structured epoxy-anhydride-based polyester vitrimer composites reinforced with cellulosic filaments is demonstrated, where hydroxyl groups on fiber surfaces participate directly in transesterification with the matrix. Further, this dynamic interfacial bonding delivers exceptional mechanical properties, including ≈70 MPa shear strength and >10% strain-to-failure, while enabling thermal malleability. Using a combination of nuclear magnetic resonance and nano-infrared spectroscopies, direct evidence is provided that chemical bond exchange begins well below the conventionally measured T v , supporting the hypothesis that rheologically determined T v reflects a combination of chemical exchange and frictional dynamics rather than a discrete transition. The composites demonstrate excellent processability through vacuum-assisted resin transfer molding and maintain >90% of their mechanical properties after multiple thermal reforming cycles. These findings advance both the fundamental understanding of vitrimeric transitions and the practical development of sustainable, high-performance composite materials.

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

Strength characterization of solar-synthesized cylindrical graphite carbon–carbon composites

The present work describes a new morphology of cylindrical graphite synthesized in a unique manner by direct solar decomposition of methane and reports the mechanical properties of its manifestation in woven carbon–carbon composites. Whereas traditional carbon–carbon composites are formed via epoxy impregnation, the deposited material in the process presented here conformally follows the existing shape and orientation of individual carbon fibers. Through this process, cylindrical graphite fibers are synthesized that possess superior strength due to their graphitic layers that amalgamate into interlocked pathways between disparate fibers. Here, strength measurements, taken in tandem with Raman, XRD, and SEM, paint a picture of the shift from cloth to composite behavior via graphitization of the original substrate combined with sheets of graphene coalescing into a unified composite, with a notable improvement in elastic modulus from 0.19 to 2.66 GPa.

Carbon–carbon composite↗
DOE OSTI2024

Empirical Characterization and Modeling of Cohesive – to – Adhesive Shear Fracture Mode Transition due to Increased Adhesive Layer Thicknesses of Fiber Reinforced Composite Single – Lap Joints

Here, to ensure a strong adhesive bond, most standards and adhesive manufacturers specify a maximum adhesive gap of 1 mm when bonding fiber reinforced composite structures. In manufacturing large components, such as joining two halves of wind turbine blades, meeting this gap tolerance specification is impractical; gaps larger than 10 mm are common in large adhesively bonded composite structures using state-of-the-art manufacturing techniques. Currently, there is a lack of fundamental understanding of the failure mechanics of adhesive gaps larger than 3 mm. To create such understanding, glass fiber - acrylic thermoplastic composite panels bonded using different epoxy adhesives within single-lap joint samples with adhesive thicknesses of 0.1 mm, 0.3 mm, 1 mm, 3 mm, 5 mm, and 10 mm were sheared to failure. A transition from cohesive to adhesive failure was observed to occur about 1 mm to 3 mm joint thicknesses. Plotting the shear stress normalized by the ratio of the joint width to thickness as a function of the joint thickness normalized by the joint length is shown to result in the ability to fit simple empirically derived models of the cohesive-to-adhesive failure transition, regardless of the adhesive. Furthermore, using these normalized variables, all the observed cohesively failed specimens collapse to a single master curve, as do the adhesively failed specimens.

36 MATERIALS SCIENCE↗
DOE OSTI2025

The Triple Catalytic Action of Tertiary Nitrogen Catalysts in Recyclable Epoxy-Anhydride Thermosets

The thermosetting polymer matrix in fiber reinforced composites is an important component for energy related applications, such as the lightweighting of vehicles or their use in wind and waterpower turbine blades, due to their ability to provide superior adhesion, stiffness, and applicability to a wide range of manufacturing processes. Despite these benefits, today's thermosets are widely considered to be unrecyclable; thus, there is a large interest in redesigning these materials to be inherently recyclable so that energy intensive production of fibers and monomers can be circumvented, bolstering composite manufacture supply chains. Polyester covalent adaptable networks (PECANs) are one such promising alternative to the incumbent, nonrecyclable epoxy-amine thermosets. PECANs can be formed from the ring-opening co-polymerization (ROCOP) of epoxy-anhydride monomer mixtures and subsequent curing at mild temperatures to exhibit similar performance to conventional epoxies while also possessing unique dynamic chemistries along the ester-hydroxyl backbone that are capable of transesterification and thus reprocessability. While significant advancements have been made in formulating these materials for improved mechanical properties or optimizing solvolysis and reprocessing strategies, less attention has been placed on the impact of the residing amine catalyst used to generate the polyester network. In this work, we evaluated the triple-catalytic efficacy of 12 tertiary amines that act as a curing (bulk ROCOP), a transesterification (internal bond exchange), and a deconstruction (methanolysis) catalyst for PECAN thermosets. Specifically, we first distinguish between chain-growth and step-growth polymerization mechanisms for epoxy-amine and epoxy-anhydride mechanisms. We also utilized density functional theory (DFT) to estimate the basicity (pKb) of each catalyst. Of the tested catalysts, the ROCOP of the studied PECAN network can be completed between 95 and 247 min (at 80 degrees C), with variable gelation phenomena. Additionally, the stress relaxation (transesterification metric) efficiency of the tested PECAN networks with alternative embedded catalysts ranged from 95% to 15% reduction in stress after 5 h at 200 degrees C, and the depolymerization efficacy ranged from 2.5% to 9.8% deconstruction after 36 h at 130 degrees C. Overall, the nitrogen-based moieties were demonstrated to influence polymerization kinetics, catalyze the dynamic transesterification exchange mechanism, and aid in the solvolysis of the thermosets at end-of-life.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Electroplated Polymer‐Modified Carbon Fiber for Performance‐Enhancing Composite Interfaces

Carbon fiber composite performance relies on the fiber-matrix interface for effective load transfer. To enhance interfacial properties between the fiber and matrix, often carbon fiber surfaces are oxidatively and covalently modified to incorporate chemical functional groups. By contrast, here, noncovalent electrodeposition of functional polyelectrolyte is applied onto conducting carbon fibers from aqueous solutions. A natural polymer, chitosan (CS), is electro-deposited onto the fiber surface, which undergoes multi-scale physical interactions. The bound CS layer with abundant amine functionalities reacts with epoxy moieties within the matrix to improve the interfacial properties. The scalable and energy-efficient electrodeposition eliminates traditional functionalization and sizing requirements of carbon fiber while delivering significantly higher mechanical performance with enhanced consistency. For continuous fiber reinforced composites, compared to conventional fibers, apparent interlaminar shear strength increases by 27%, reaching ≈86 MPa. The short fiber composites with only 2–11 wt.% fibers exhibit ≈20% increase in tensile strength with a peak performance of 120 MPa. Unlike traditionally treated and sized carbon fiber, this approach delivers coated fibers with long shelf-life and allows recovery of both CS in electrolyte form and carbon fiber by continuous electrochemical processing of the modified fibers with inverse polarity; thus, it promotes overall fiber recyclability.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Impact of DMP-30 catalyst concentration on the degradation and kinetics of bisphenol A epoxy thermosets cured with linear amine hardener

Epoxy thermosets are a crucial component in carbon-fiber composites, serving as the organic binding matrix. Catalysts are commonly used in prepolymer formulations to accelerate curing of the thermosets. However, the impact of catalysts on the thermal stability, degradation pathways, and kinetics of the final thermoset is poorly understood. Here, in this work, Product-Specific Kinetics (PSK) analysis was utilized with isoconversional kinetics to provide a first look into the degradation kinetics of major pyrolysis pathways in bisphenol A (BPA) epoxy resins and determine the impact of altering catalysis concentrations on these kinetic pathways. Results revealed new insights into previously identified degradation pathways, provided evidence of multiple degradation pathways for some products, and showed that use of excess catalyst results in polymer network alterations and reduced thermal stability of the thermosets.

Bisphenol A↗
DOE OSTI2025

Sustainable, degradable and malleable low-dielectric-constant thermosets derived from biomass for recyclable green electronics

In view of their excellent thermal and chemical resistance, favorable adhesion properties, high tensile strength, and other advantages, epoxy thermosets have numerous industrial applications such as coating, adhesive, and composite material production. However, bisphenol A (BPA)-based resins, which account for a significant fraction of the above thermosets, adversely affect human health by interfering with the normal functioning of the endocrine system and cannot be easily decomposed and recycled. Herein, degradable and sustainable bio-based epoxy thermosets with crosslinked network structures are prepared by the epoxidation of isosorbide with epichlorohydrin and the curing of the produced isosorbide diglycidyl ether (ISDGE) with cyclic lactones through a cationic ring-opening reaction. The ISDGE thermosets fully decompose into soluble and recyclable products under mildly basic conditions within three days, which is ascribed to the presence of ester moieties within the polymer network structure. Compared to a representative BPA-based epoxy, ISDGE-based thermosets exhibit lower dielectric constants and are more flexible. Moreover, the glass fibers in ISDGE-based prepregs can be fully recovered after on-demand degradation. Furthermore, our work provides promising eco-friendly alternatives to conventional epoxy thermosets and paves the way for the reduction of plastic waste generation and the development of recyclable green electronics.

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

Ambient-Pressure Chemical Recycling of Thermoset Carbon Fiber-Reinforced Polymers via Low-Temperature Solvolysis: Techno-Economic and Life-Cycle Assessment

Carbon fiber-reinforced polymer (CFRP) waste is rapidly accumulating, with global volumes projected to exceed 500,000 tons annually by 2050. Virgin carbon fiber production is extremely energy- and cost-intensive, and growing demand has intensified supply-chain vulnerabilities associated with precursor availability and reliance on critical materials. Scalable recycling technologies therefore offer not only environmental benefits but also opportunities to reduce material costs and strengthen domestic composite supply chains. This study introduces an efficient, mild chemical recycling method for epoxy-amine CFRPs, utilizing acetic acid (80 wt%) and zinc acetate (1 wt%) at atmospheric pressure and low temperature (~110 °C). The solvolysis process preserves residual resin (~40%) on recycled carbon fibers (rCF), enhancing interfacial bonding in remanufactured composite materials. Recycled fibers retain ~90% of their mechanical properties, and recovered oligomers show potential for reuse in epoxy formulations, supporting material circularity. Techno-economic analysis (TEA) and life-cycle assessment (LCA) confirm the scalability and sustainability of this process.

Recycling CFRP↗
DOE OSTI2024

Hierarchical Composites Patterned via 3D Printed Cellular Fluidics

Additive manufacturing of freeform structures containing multiple materials with deterministic spatial arrangement and interactions remains a challenge for most 3D printing processes, due to complex fabrication tool requirements and limitations in printability of some material classes. Here, in this paper, a versatile method is reported to produce architected composites using the concept of cellular fluidics, in which lattices of unit cells are used as templating scaffolds to guide flowable infill materials in a programmed spatial pattern, upon which they are cured in place to produce a deterministically ordered multimaterial solid. The lattice design relies on the unit cell size, type, strut diameter, surface wetting, and distribution of cellular structures to control liquid flow and retention. Individual unit cells are tuned to achieve reliable infilling and combined into higher-order architectures to achieve multiscale composite materials with disparate mechanical properties, including those considered non-printable. Lattice design considerations for leveraging capillary phenomena and demonstrate several methods of patterning polymers in 3D-printed cellular fluidic structures are presented. The concept of tuning the compressive response of an architected composite using a flexible-elastomer as the lattice and a stiff-epoxy as the infill material is illustrated.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Harnessing biomass-derived reinforcements for sustainable flame-resistant composite

Bio-based composites containing natural fiber reinforcements have been integral to developing innovative, low-cost, and low-energy technologies for transportation applications in marine, automotive, and other industries. The low density of natural fibers gives these materials a high specific stiffness and strength, which can lead to significant weight savings in composites. This study focused on a specialty type of wood fiber treated with boric acid (≤ 7%) sourced from Northern White Pine in the USA, marketed as TimberFill. TimberFill is a high aspect ratio, fibrillated wood fiber that is produced commercially for wood fiber insulation; it is chemically treated to improve both its flame retardance and water resistance. In the present study, TimberFill was processed into non-woven mats using a process akin to papermaking and then infiltrated with epoxy resin. Biochar from wood waste was also incorporated into the epoxy resin as a low-cost filler and functional additive. The effects of biochar concentration on composites’ flame retardance (17% improvement in burn rate), thermal conductivity (improved by 9%), and mechanical performance (33% improvement in modulus) are herein presented. Additionally, it explores the plasticizing effect of the boric acid used in the treatment of TimberFill on the thermal and mechanical properties of the resulting composites, specifically on the thermal expansion coefficient.

Joshy, Joslin [ORNL]↗
DOE OSTI2024

Understanding interfacial crystallization dynamics on carbon fiber reinforced polypropylene composite manufacturing

Reinforcing polymers with discontinuous fibers improves mechanical properties, such as strength and stiffness, and in some cases achieve isotropic properties, rendering them suitable for various engineering applications. Matrix materials are generally highly engineered thermosets (e.g. crosslinked epoxies), bonded to the fiber periphery by proprietary surface and sizing chemistries. Semicrystalline thermoplastic matrices are less utilized due to poor fiber-matrix bonding resulting in inefficient interfacial load-transfer in reinforced composites. However, flexibility with melt-processing or molding conditions can be leveraged to promote non-covalent interfacial bonding between matrix and fiber via crystallization of the matrix onto fiber surface. In the present study, we utilize a co-mingle chopped carbon and isotactic polypropylene fibers to form isotropic composites, tailoring interfacial immobilized matrix or interphase morphology to optimize performance through precise control of thermal processing/molding windows. Calorimetry and optical microscopy were employed to investigate the impact of carbon fiber at various volume fractions (10, 20, and 30 %) on isotactic polypropylene crystallization and mechanical performance. Variations in mechanical properties correspond to the structural evolution of the interfacial region and are correlated to underlying microstructural attributes using wide-angle X-ray scattering, thermal analysis, and low-field nuclear magnetic resonance spectroscopy. These results provide a practical framework for the manufacturing of thermoplastic matrix composites. In conclusion, the results presented provide a guide for the strategic optimization of interphase design, showcasing tailorable tensile strengths which outperform any isotactic polypropylene carbon fiber composites previously reported in literature.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Predicting multi-nodal in-nozzle particle interactions in high-viscosity fluid mediums for acoustophoretic direct-ink writing of line-patterned composites

Patterned functional materials offer improved properties (electrical, thermal, etc.) over their bulk counterparts in many applications, including energy storage, flexible electronics, and sensors. However, manufacturing approaches for patterning materials over large areas with features on the order of hundreds of microns or less are limited. Acoustophoresis, which uses acoustic forces to control particle arrangement in a fluid medium, is a pathway to address this challenge. This process is dependent on particle and fluid properties and enables patterning of a broad range of materials. Herein, a model with experimental validation is presented to demonstrate that acoustophoresis can be combined with direct-ink writing (DIW) to fabricate line patterns over large cm-scale areas. An in-nozzle particle interaction model was developed to investigate the impact of processing conditions on multi-nodal acoustophoretic DIW. The model predicts patterned line widths within a factor of two relative to experimental results for a high viscosity case study. Here, the model was used to investigate the impact of frequency, particle loading, particle radius, and acoustic pressure on line width and patterning time, providing critical feedback regarding the processing conditions suitable for a target application. Model results illustrate that frequency has the greatest impact on line patterns: increasing from 1 to 3 MHz resulted in a greater than 65% reduction in line width and a greater than 85% reduction in patterning time. Additionally, experiments were conducted with an alumina-epoxy ink and a ~21 cm 2 area pattern was rastered in ~5.5 minutes, demonstrating a path towards large-area line-patterned composite fabrication.

25 ENERGY STORAGE↗
DOE OSTI2025

Comparison of interlaminar damage modeling strategies for hybrid composite/aluminum laminates subjected to low-velocity impact

Low-velocity impact of hybrid metal-composite structures was investigated experimentally and computationally. Composite laminates consisting of 2D woven glass fiber reinforced polymer (GFRP) and carbon fiber reinforced polymer (CFRP) were joined with a 6061-T6 aluminum plate using an epoxy adhesive. Two variations of the structure were studied; one consisting of all plies oriented at 0° and one consisting of all plies oriented at 45°. A drop tower was used to impact structures at a range of energies, including energies above and below the threshold at which the aluminum layer was perforated. Numerical simulations were implemented using Sierra/SM, an in-house transient dynamics finite element code developed at Sandia National Laboratories. A Hosford plasticity model was used to describe the response of the aluminum layer. A newly implemented orthotropic continuum damage mechanics (CDM) constitutive model was used to represent the composite laminate. This 3D-CDM model was compared to a cohesive zone model (2D-CDM/CZM) to investigate efficacy of aluminum perforation energy prediction, delamination prediction, and computational cost. Accuracy of each model was evaluated using the experimental results. Each showed good agreement with the tests for both the force and velocity histories, as well as the observed damage mechanisms. The 2D-CDM/CZM model was marginally more accurate in capturing both the composite and aluminum behavior — this model averaged error percentages of -11.2% and 10.8% for residual velocity and peak force, respectively. Meanwhile, the 3D-CDM model predictions yielded average error percentages of -35.5% (velocity) and 22.6% (force). However, the 3D-CDM model generally resulted in a decreased computational cost; the average run time was 14% shorter than the 2D-CDM/CZM model and 3x as many timesteps per hour were computed using the same computational resources. In conclusion, new experimental data on the impact and perforation resistance of metal-composite laminates is presented in addition to numerical predictions of the impact behavior.

Carbon fiber↗
DOE OSTI2024

Rational design of semi-interpenetrating network based on hyperbranched polyglycerol grafted MXene/polyurethane–epoxy for compressed hydrogen storage

Here, hydrogen (H 2 ) energy has emerged as a promising alternative in the automotive sector to replace fossil fuel; however, its storage with volumetric efficiency remains a challenge. The latest type IV storage vessel featuring a polymeric liner with composite overwrap incurs hydrogen saturation, which eventually causes failure. To prevent the H 2 dissolution in the liner, we have developed a barrier coating comprised of polyurethane/epoxy semi-interpenetrating network (S-IPN) combined with hyperbranched polyglycerol grafted MXene (h-MXene). The hyperbranched structure facilitated the dispersion of MXene in the coating solution by enhancing the exfoliation and improved the polymer filler interaction by forming covalent and H-bonding through end-terminal hydroxyl groups. Leveraging the dense network of S-IPN combined with the dispersed layer structured h-MXene significantly increased the tortuosity of the spray-coated barrier film applied to the nylon 6 liner. The coating exhibited a 90 % reduction in the H 2 gas permeability at only 2 wt% h-MXene concentration, which further improved to above 98 % at 10 wt% loading. Additionally, the h-MXene considerably improved the adhesion with the liner even in a highly stretched condition, signifying the durability of the coating under cyclic pressurization and depressurization of the storage vessel.

08 HYDROGEN↗
DOE OSTI2025

Comparison of Nb 3 Sn Insulation Systems With as Received and De-Sized Glass

Epoxy cracking has been the main suspected contributor to training in Nb 3 Sn magnets for some time, as it leads to energy release and magnet quenching. Cracking in a superconducting composite can occur from several modes, and the likelihood of these modes is not well understood. Failure has been observed between insulation systems and the superconducting cable itself rather than within the cable or insulation. To target the behavior at the interface, samples have been fabricated and tested for Mode I fracture toughness in an adapted version of ASTM D5528. This work seeks to better characterize the fracture toughness of this interface to better understand how to model and design insulation systems.

Krave, Steven T. [Fermilab] (ORCID:000000021752145↗
DOE OSTI2024

Tough and circular glass fiber composites via a tailored dynamic boronic ester interface

Glass fiber reinforced polymer (GFRP) composites are valued for their strength and cost-effectiveness. However, traditional GFRPs often face challenges for end-of-life recycling due to their non-depolymerizable thermoset matrices, and long-term performance due to inadequate interfacial adhesion, which can lead to fiber–matrix delamination. Here, in this work, we have designed dynamic fiber–matrix interfaces to allow tough and closed-loop recyclable GFRPs by utilizing a vitrimer, derived from upcycled polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene (SEBS) with boronic ester (S-Bpin) and amine-based diol crosslinker. The boronic ester groups in S-Bpin form dynamic covalent bonds with the naturally present hydroxyl groups on the unsized GF surface, which eliminates the need for fiber sizing and enables facile closed-loop recyclability of both the fibers and the vitrimer matrix. The resulting strong fiber–matrix interface, depicted by the Raman mapping, leads to a 552% increase in-plane shear toughness (6.2 ± 0.3 MJ m -3 ) and 27% ultimate tensile strength (361 ± 89.2 MPa) compared to those of the conventional epoxy-based matrix (0.95 ± 0.05 MJ m -3 and 264 ± 59.7 MPa, respectively). The network rearrangement through dynamic boronic ester exchange enables fast thermoformability and repairability of micro-cracks at elevated temperatures. Additionally, both the matrix and composite demonstrate strong adhesion to various surfaces including steel and glasses exhibiting ≥6 MPa lap shear strength, which expands their suitability for diverse industrial applications. The readily created dynamic interface between boronic ester functionalized vitrimer and neat GFs presents a promising strategy for developing closed-loop recyclable, multifunctional structural materials, offering a sustainable alternative to non-recyclable thermoset GFRPs and contributes to a circular economy in composite materials.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Epoxy Coating of Biofiber: An Effective Modifier of Biofiber Physical and Flow Properties for Improved Tensile Behavior of Biofiber-Reinforced Biocomposite

Biocomposites combine renewable, plant-based fibers with degradable polymers and are an attractive option for sustainable, lightweight, and cost-effective materials with a low carbon footprint, especially for large-scale additive manufacturing. One of the major challenges in the widespread adoption of biocomposites is that their mechanical performance is significantly inferior to that of synthetic composites. Surface treatment is a common and effective technique to improve the mechanical properties of the biofibers used in biocomposites. This study aims to investigate the physical and flow properties of surface-treated biofibers, as well as the tensile properties of their PLA-based biocomposite, to gain insights into how surface treatment changes the fiber‘s characteristics and biocomposite‘s mechanical properties. Surface treatment was created using a two-component epoxy system by reacting poly(bisphenol A-co-epichlorohydrin) glycidyl end-capped (PBG) and dicyandiamide (DICY). The treatment was tested on two different biofibers (loblolly pine and corn stover fibers) with three different PBG/DICY molar ratios (0.25, 0.5, and 2). Results showed that surface-treated fibers improved the tensile strength and Young‘s modulus of the biocomposites. Loblolly pine biocomposites from fibers treated with a PBG/DICY ratio of 0.25 exhibited the best tensile properties. The surface treatment resulted in a more loosely dispersed fiber bulk structure, as evidenced by less fiber agglomeration into smaller particle sizes, higher fiber sphericity, and lower loose bulk density. This can enhance stress distribution and the overall mechanical performance of the biocomposites. Additionally, surface-treated fibers exhibited better dynamic flow properties.

36 MATERIALS SCIENCE↗