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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 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Amplifying Nanoparticle Reinforcement through Low Volume Topologically Controlled Chemical Coupling

Here, we present a streamlined method to covalently bond hydroxylated carbon nanotubes (CNOH) within a polyphenol matrix, all achieved through a direct, solvent-free process. Employing an extremely small concentration of CNOH (0.01% w/w) along with topologically contrasting linkers led to a maximum of 5-fold increase in modulus and a 25% enhancement in tensile strength compared to the unaltered matrix, an order of magnitude greater reinforcement (w/w) compared to state-of-the-art melt-processed nanocomposites. Through dynamic mechanical analysis, low field solid-state nuclear magnetic resonance spectroscopy, and molecular dynamics simulations, we uncovered the profound influence of linker’s conformational degrees of freedom on the segmental dynamics and therefore the material’s properties.

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

Enabling Industrial Re-Use of Large-Format Additive Manufacturing Molding and Tooling

Large-format additive manufacturing (LFAM) is an enabling manufacturing technology capable of producing large parts with highly complex geometries for a wide variety of applications, including automotive, infrastructure/construction, and aerospace mold and tooling. In the past decade, the LFAM industry has seen widespread use of bio-based, glass, and/or carbon fiber reinforced thermoplastic composites which, when printed, serve as a lower-cost alternative to metallic parts. One of the highest-volume materials utilized by the industry is carbon fiber (CF)-filled polycarbonate (PC), which in out-of-autoclave applications can achieve comparable mechanical performance to metal at a significantly lower cost. Previous work has shown that if this material is recovered at various points throughout the manufacturing process for both the lab and pilot scale, it can be mechanically recycled with minimal impacts on the functional performance and printability of the material while significantly reducing the feedstock costs. End-of-life (EOL) CF-PC components were processed through industrial shredding, melt compounding, and LFAM equipment, followed by evaluation of the second-life material properties. Experimental assessments included quantitative analysis of fiber length attrition, polymer molecular weight degradation using gel permeation chromatography (GPC), density changes via pycnometry, thermal performance using dynamic mechanical analysis (DMA), and mechanical performance (tensile properties) in both the X- and Z-directions. Results demonstrated a 24.6% reduction in average fiber length compared to virgin prints, accompanied by a 21% decrease in X-direction tensile strength and a 39% reduction in tensile modulus. Despite these reductions, Z-direction tensile modulus improved by 4%, density increased by 6.8%, and heat deflection temperature (HDT) under high stress retained over 97% of its original value. These findings underscore the potential for integrating mechanically recycled CF-PC into industrial LFAM applications while highlighting the need for technological innovations to mitigate fiber degradation and enhance material performance for broader adoption. This critical step toward circular material practices in LFAM offers a pathway to reducing feedstock costs and environmental impact while maintaining functional performance in industrial applications.

additive manufacturing↗
NASA NTRS1995

Chemical and Thermal Analysis

During the past six months we have conducted significant research in several domains in order to clarify and understanding the aging and chemical failure mechanism of thermoplastics (PVDF or Tefzel) for pipes. We organized numerous analytical studies with methods including Fourier Transform Infrared Spectroscopy, Dynamic Mechanical Analysis, Differential Scanning Calorimetry, and Stress Relaxation experiments. In addition we have reanalyzed previous thermogravimetric data concerning the rate of deplasticization of Coflon pipe. We investigated a number of aged samples of both Tefzel and Coflon that were forwarded from MERL. We conducted stress relaxation experiments of Coflon pipe at several temperatures and determined an activation energy. We also examined the dynamic mechanical response PVDF during deplasticization and during methanol plasticization. We performed numerous DSC analyses to research the changing crystalline morphology. We have noted significant changes in crystallinity upon aging for both PVDF and Tefzel. Little variation in elemental composition was noted for many of the aged Coflon and Tefzel samples tested.

Bulluck, J. W.↗
DOE OSTI2021

Wood-reinforced composites by stereolithography with the stress whitening behavior

In this study, poplar wood flour at various concentrations (1–10 wt%) is incorporated into a methacrylate-based resin via solution blending to fabricate wood-reinforced composites using stereolithography apparatus (SLA) 3D printing. Differential scanning calorimetry (DSC) along with Fourier transform infrared spectroscopy (FTIR) analysis shows the presence of a small amount of residual monomer in the printed samples. For the printed composites, the glass transition temperature (T g ) from dynamic mechanical analysis (DMA) decreases as more wood flour is incorporated, which indicates an increase in free volume occupied by polymer chains. The tensile strength is improved up to 17.3% from 21.1 MPa (no wood flour) to 24.7 MPa (1.0 wt% wood flour). The highest Young’s modulus reaches 323.8 MPa (2.0 wt% wood flour), which is 1.9-fold of that of the sample without wood flour. Moreover, the composites show “stress whitening” with the addition of wood flour during the uniaxial drawing. Morphology analysis of the tested samples show that the formation of microcraze and microvoids likely causing the stress whitening. This is the first study that demonstrates wood flour can be utilized in SLA 3D printed wood plastic composites (WPC) which can reinforce the printed products with a modest loading amount.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microscopic Origins of the Nonlinear Behavior of Particle-Filled Rubber Probed with Dynamic Strain XPCS

The underlying microscopic response of filler networks in reinforced rubber to dynamic strain is not well understood due to the experimental difficulty of directly measuring filler network behavior in samples undergoing dynamic strain. This difficulty can be overcome with in situ X-ray photon correlation spectroscopy (XPCS) measurements. The contrast between the silica filler and the rubber matrix for X-ray scattering allows us to isolate the filler network behavior from the overall response of the rubber. This in situ XPCS technique probes the microscopic breakdown and reforming of the filler network structure, which are responsible for the nonlinear dependence of modulus on strain, known in the rubber science community as the Payne effect. These microscopic changes in the filler network structure have consequences for the macroscopic material performance, especially for the fuel efficiency of tire tread compounds. In this work, we elucidate the behavior with in situ dynamic strain XPCS experiments on industrially relevant, vulcanized rubbers filled (13 vol %) with novel air-milled silica of ultrahigh-surface area (UHSA) (250 m 2 /g). The addition of a silane coupling agent to rubber containing this silica causes an unexpected and counterintuitive increase in the Payne effect and decrease in energy dissipation. For this rubber, we observe a nearly two-fold enhancement of the storage modulus and virtually equivalent loss tangent compared to a rubber containing a coupling agent and conventional silica. Interpretation of our in situ XPCS results simultaneously with interpretation of traditional dynamic mechanical analysis (DMA) strain sweep experiments reveals that the debonding or yielding of bridged bound rubber layers is key to understanding the behavior of rubber formulations containing the silane coupling agent and high-surface area silica. These results demonstrate that the combination of XPCS and DMA is a powerful method for unraveling the microscale filler response to strain which dictates the dynamic mechanical properties of reinforced soft matter composites. With this combination of techniques, we have elucidated the great promise of UHSA silica when used in concert with a silane coupling agent in filled rubber. Such composites simultaneously exhibit large moduli and low hysteresis under dynamic strain.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Novel application of the modal strain energy technique for state-of-the-art damping predictions

Structural damping, which measures the energy dissipation of a vibrating structure, is a key modeling input for lightweight structures but is notoriously hard to predict. This work utilizes vibration-based measurements of centimeter-scale coupons and the modal strain energy approach to predict structural damping of a lightly damped structure. The approach was originally validated with panels shorter than a meter in length. This work extends the validation to a 2.75 m beam made of unidirectional and biaxial glass fiber laminates bonded by adhesive. The comparison between three-dimensional finite element model predictions and full-scale experimental measurements of damping show an average error of 5.2% for the first five modes. Additionally, the modal strain energy approach is newly applied with a one-dimensional geometrically exact beam theory model and a two-dimensional sectional analysis solver. This beam approach accurately predicts the damping behavior of the first bending modes but loses accuracy for higher order modes that are dominated by three-dimensional effects. This novel approach provides faster simulations while allowing arbitrary beam cross sections. The paper also investigates traditional and high-force dynamic mechanical analysis to measure structural damping of coupons. Both alternatives show significant errors in attempted validation against the theoretical thermoelastic damping of aluminum coupons.

17 WIND ENERGY↗
NASA NTRS1991

Study of balloon and thermal control material degradation aboard LDEF

The initial results of analysis performed on a number of polymeric materials which were exposed aboard the Long Duration Exposure Facility (LDEF) are discussed. These materials include two typical high altitude balloon films (a polyester and a polyethylene) and silver-backed Teflon from thermal control blanket samples. The techniques used for characterizing changes in mechanical properties, chemical structure and surface morphology include Fourier Transform Infrared (FTIR) spectroscopy, scanning electron microscopy, and dynamic mechanical analysis.

Letton, Alan↗
DOE OSTI2026

Formulation and Performance Evaluation of Epoxy Sealant Systems for Double-Shell Tank Bottom Refurbishment

The performance of epoxy sealants used in the refurbishment of double-shell tank (DST) systems requires balancing processability, thermomechanical stability, and adhesion to cementitious substrates. This study incorporates Heloxy 8 as a reactive diluent into Westlake 862 epoxy to tailor workability and cured-state properties. Rheological time-sweep analysis demonstrates that increasing the diluent content significantly reduces complex viscosity and extends workability, thereby improving pumpability and flow for large-area applications. However, the targeted 2-hour processing window is not fully achieved. Differential scanning calorimetry (DSC) confirms that all formulations cure at room temperature to glass transition temperatures ( T g ) at least 20 °C above the maximum DST operating temperature (27 °C), thereby ensuring service in the glassy regime. Dynamic mechanical analysis (DMA) reveals formulation-dependent reductions in tan delta and increases in storage modulus, indicating increasingly elastic and mechanically stable networks with diluent incorporation. Pull-off adhesion testing shows that modified formulations (70–90% Westlake epoxy) exhibit significantly higher adhesion strengths than the unmodified system. Grout cohesive failure indicates that interfacial bonding exceeds substrate strength. Collectively, these results demonstrate that controlled reactive diluent incorporation enables optimization of processing behavior, interfacial adhesion, and thermomechanical performance, supporting the suitability of the modified epoxy systems as durable sealant layers for cementitious barrier applications in hazardous waste containment infrastructure.

Differential scanning calorimetry↗
DOE OSTI2020

Addition of Short Polymer Chains Mechanically Reinforces Glassy Poly(2-vinylpyridine)–Silica Nanoparticle Nanocomposites

The addition of hard fillers to a polymer matrix is a well-known process for achieving mechanical reinforcement. With a decrease in the size of the fillers, the contribution from polymer–particle nanometer-sized interfaces become significant, and these interfaces affect the mechanical performance of polymer nanocomposites (PNCs) beyond the limits established for conventional composites. However, the molecular mechanisms underlying the improvement in the mechanical performance of glassy PNCs remain unresolved, necessitating a deeper understanding of the structure–property relationships in these intrinsically heterogeneous systems. In this effort, by using Brillouin light scattering (BLS) and dynamic mechanical analysis (DMA), we demonstrated that adding shorter chains to a PNC prepared with high molecular weight polymers significantly improved the mechanical properties of the PNC in the glassy state. The strongest enhancement of mechanical properties occurred at an optimum concentration of short chains. This is in contrast to behavior of the glass transition temperature of PNCs which shows a monotonic decrease with an increase in the concentration of shorter chains. Using experimental data and coarse-grained molecular dynamics (MD) simulations, we have identified the molecular mechanism leading to the observed non-monotonic changes in mechanical reinforcement. Here, this mechanism includes changes in the nanoscale organization at the interface, combined with chain stretching amplified by the addition of the short chains. Overall, our approach paves a simple, cost-effective pathway to fabricating glassy PNCs with significantly improved mechanical properties that will fill various practical needs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2005

High Temperature Thermosetting Polyimide Nanocomposites Prepared with Reduced Charge Organoclay

The naturally occurring sodium and calcium cations found in bentonite clay galleries were exchanged with lithium cations. Following the cation exchange, a series of reduced charge clays were prepared by heat treatment of the lithium bentonite at 130 C, 150 C, or 170 C. Inductively coupled plasma (ICP) analysis showed that heating the lithium clay at elevated temperatures reduced its cation exchange capacity. Ion exchange of heat-treated clays with either a protonated alkyl amine or a protonated aromatic diamine resulted in decreasing amounts of the organic modifier incorporated into the lithium clay. The level of silicate dispersion in a thermosetting polyimide matrix was dependent upon the temperature of Li-clay heat treatment as well as the organic modification. In general, clays treated at 150 C or 170 C, and exchanged with protonated octadcylamine or protonated 2,2'-dimethlybenzidine (DMBZ) showed a higher degree of dispersion than clays treated at 130 C, or exchanged with protonated dodecylamine. Dynamic mechanical analysis showed little change in the storage modulus or T(sub g) of the nanocomposites compared to the base resin. However, long term isothermal aging of the samples showed a significant decrease in the resin oxidative weight loss. Nanocomposite samples aged in air for 1000 hours at 288 C showed of to a decrease in weight loss compared to that of the base resin. This again was dependent on the temperature at which the Li-clay was heated and the choice of organic modification.

Campbell, Sandi↗
DOE OSTI2025

Sustainable Shape Memory Elastomers with Reduced Melt Viscosity and Enhanced Stiffness

Melt reactive processing of lignin with nitrile rubber is a promising approach to synthesizing shape memory materials. The strong intramolecular interactions in lignin macromolecular structures, caused by π–π stacking in aromatic rings and hydrogen bonding, often result in large phase separation or low miscibility with rubbers. In this study, we investigated the chemical and molecular characteristics, as well as the stiffness and complex viscosity, of modified kraft lignin melt-reacted with an acrylonitrile/butadiene copolymer containing 41% acrylonitrile (NBR41). To enhance the macromolecular compatibility of kraft lignin with NBR41, kraft lignin was cross-linked with poly(propylene glycol) diglycidyl ether (PPDE) and trimethylolpropane triglycidyl ether (TTE), both rich in epoxy reactive groups capable of forming chemical bonds with hydroxyl and carboxyl groups. Here, our findings demonstrate that the modification of kraft lignin with PPDE and TTE resulted in significantly increased stiffness of the composites. The elastic modulus of NBR41-Kraft lignin-PPDE and NBR41-Kraft lignin-TTE increased by 82 and 162%, respectively. Both the yield strength and Young’s modulus of these two samples showed dramatic improvements. Specifically, the yield strength and Young’s modulus of NBR41-Kraft lignin-TTE increased nearly 4 and 3-fold, respectively, compared to the control sample. Interestingly, despite significant improvements in mechanical properties, the viscosity of NBR41-Kraft lignin-PPDE was substantially lower than that of the control sample. At 210 °C and an angular frequency of 1 rad/s, the complex viscosity of NBR41-Kraft lignin was approximately 100.25 ± 4.77 kPa·s, while that of NBR41-Kraft lignin-PPDE was significantly lower at 56 ± 0.93 kPa·s. These findings were validated through Fourier transform infrared spectroscopy, scanning electron microscopy, dynamic mechanical analysis, thermal characterization, rheological tests, and quasi-elastic neutron scattering techniques.

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

Exceptional Alignment in a Donor–Acceptor Conjugated Polymer via a Previously Unobserved Liquid Crystal Mesophase

Abstract Orienting polymer semiconductors is desirable to optimize device characteristics, provide insight into microstructure, and magnify subtle phase behavior. Here, a combination of uniaxial strain and subsequent heating of the donor–acceptor (DA) polymer PBnDT‐FTAZ is discovered to lead to exceptional optical dichroic ratios of up to 38 (and close to 50 near the polymer's absorption edge). This alignment is achieved due to the existence of a previously undetected thermotropic liquid crystal (LC) mesophase. The LC transition, not discernable through calorimetry, is uncovered through a combination of in situ UV–vis spectroscopy, X‐ray scattering, and dynamic mechanical analysis (DMA). Comparing PBnDT‐FTAZ to the non‐fluorinated PBnDT‐HTAZ and the homo polymer PBnDT, all of which show similar thermal transitions, reveals that exceptional alignment is only found in PBnDT‐FTAZ. This is attributed to the PBnDT‐FTAZ film having two distinct liquid crystal populations, and the polymer templating to a highly aligned, high‐clearing temperature population when heated. The DMA thermal relaxation behavior observed here is also seen in other DA conjugated polymers suggesting that such thermotropic LC mesophases may be common in these materials. These findings demonstrate a polymer semiconductor with remarkable alignment and uncover phase behavior with broad implications for process‐structure‐property relationships in polymer semiconductors.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Multimorphic Materials: Spatially Tailoring Mechanical Properties via Selective Initiation of Interpenetrating Polymer Networks

Access to multimaterial polymers with spatially localized properties and robust interfaces is anticipated to enable new capabilities in soft robotics, such as smooth actuation for advanced medical and manufacturing technologies. Here, orthogonal initiation is used to create interpenetrating polymer networks (IPNs) with spatial control over morphology and mechanical properties. Base catalyzes the formation of a stiff and strong polyurethane, while blue LEDs initiate the formation of a soft and elastic polyacrylate. IPN morphology is controlled by when the LED is turned “on”, with large phase separation occurring for short time delays (≈1–2 min) and a mixed morphology for longer time delays (>5 min), which is supported by dynamic mechanical analysis, small angle X-ray scattering, and atomic force microscopy. Through tailoring morphology, tensile moduli and fracture toughness can be tuned across ≈1–2 orders of magnitude. Furthermore, a simple spring model is used to explain the observed mechanical behavior. Photopatterning produces “multimorphic” materials, where morphology is spatially localized with fine precision (<100 µm), while maintaining a uniform chemical composition throughout to mitigate interfacial failure. As a final demonstration, the fabrication of hinges represents a possible use case for multimorphic materials in soft robotics.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Hygrothermal aging and recycling effects on mechanical and thermal properties of recyclable thermoplastic glass fiber composites

Abstract Glass fiber‐reinforced polymer composites are widely used in marine applications, including renewable energy devices and submarines, due to their strength‐to‐weight ratios and corrosion resistance. As sustainability becomes more important, recyclable thermoplastic composites are gaining attention in marine energy applications. These materials face harsh conditions such as high chloride water, UV radiation, pressurization, and thermal cycling, which can affect their durability and recyclability. This study examines the impact of hygrothermal aging on the recyclability of an Elium glass fiber (GF) composite. Samples were mechanically ground for recycling, and mechanical and thermal properties were compared between aged and unaged samples. After seawater aging, the tensile strength and modulus of the unaged composite dropped by 25% and 13% respectively, due to water ingress along the fiber‐matrix interface. The recycled composite showed reduced flexural strength as the long fiber composite was converted into short fibers during the process. Differential scanning calorimetry (DSC) revealed no change in glass transition temperature after aging. Weight loss (25%) was attributed to the thermal stability of the glass fibers. Dynamic mechanical analysis (DMA) showed that the storage modulus increased with aging, and fracture analysis confirmed a mixed mode of failure for aged composites. Highlights Hygrothermal aging lowers mechanical performance of Elium® GF composites. Failure mechanism tends to be matrix cracking and interface bonding. Glass transition temperature is not reduced by hygrothermal aging. Fractured composite was successfully recycled via thermoforming. Flexural strength of the recycled composite is lower.

17 WIND ENERGY↗
DOE OSTI2025

Initiator‐Driven Tailoring of Reactivity and Inhibition in Frontally Polymerized Dicyclopentadiene‐Co‐Dihydrofuran Thermosets

Incorporating 2,3‐dihydrofuran (DHF) into dicyclopentadiene (DCPD) enables frontally polymerizable, deconstructible thermosets via acid hydrolysis. At 5–20 mol% DHF and low initiator concentration (~100 ppm), DHF inhibits front propagation, lowers the glass transition temperature ( T g ) by up to 20°C, and quenches the front, especially at 20% DHF. This paper demonstrates that increasing the initiator concentration to 250–1000 ppm overcomes inhibition, enhances front speeds by ~50%, and suppresses quenching at the expense of pot‐life. Above 5 mol% DHF, an emergence of a second exotherm is observed, attributed to increased rate dependence on the inhibition of the initiator by DHF. Void formation from volatile DHF is suppressed by applying 110 kPa nitrogen, though at the cost of reduced front speed. Dynamic mechanical analysis shows that higher initiator concentration produced more highly cross‐linked polymers, with a ~20% increase in storage modulus at 25°C and a 20°C increase in T g .

deconstructible thermosets↗
DOE OSTI2026

Design, characterization and shape recovery behavior of 3D/4D printed shape memory polymers (SMPs)

Shape memory polymers (SMPs) represent a paradigm shift in material science, uniquely capable of undergoing reversible shape transformations triggered by external stimuli, positioning them as pivotal in developing next-generation biomedical devices, aerospace components, and adaptive structures. Extensive research has been done on SMPs with a major focus on high-temperature programming methods, which can limit energy efficiency and applicability with temperature-sensitive materials. Additionally, while various SMP blends have demonstrated great potential, limited work has been done on the suitability for 3D printing these materials, particularly under high-strain and ambient temperature programming conditions. In this study, a three-component optimized SMP composition was evaluated by 3D printing via the Material Extrusion (MEX) technique and investigating its ambient temperature-programming behavior at high strains. The SMP formulation studied was a tailored blend of thermoplastic polyurethane (TPU), polycaprolactone (PCL), and an octadecane diol-based copolymer (OBC) that exhibits robust shape memory behavior, high strain tolerance, and efficient force generation. Rigorous thermal, mechanical, and shape recovery analyses, along with optimized printing parameters and consistent shape recovery rates of up to 90%, were achieved under dynamic mechanical analysis (DMA), even under ambient programming conditions. This work demonstrates the SMP composition’s potential for adaptive, self-deployable systems with 4D printing characteristics ideal for bio-inspired structures and artificial muscle fibers.

Sudan, Kavish [University of Louisville, KY]↗
DOE OSTI2021

Compositional effects on cure kinetics, mechanical properties and printability of dual-cure epoxy/acrylate resins for DIW additive manufacturing

Interest in 3D printing of thermoset resins has increased significantly in recent years. One approach to additive manufacturing of thermoset resins is printing dual-cure resins with direct ink write (DIW). Dual-cure resins are multi-component resins which employ an in situ curable constituent to enable net-shape fabrication while a second constituent and cure mechanism contribute to the final mechanical properties of the printed materials. In this work, the cure kinetics, green strength, printability, and print fidelity of dual-cure epoxy/acrylate thermoset resins are investigated. Resin properties are evaluated as a function of acrylate concentration and in situ UV exposure conditions. The acrylate cure kinetics are probed using photo-differential scanning calorimetry and the impacts of resin composition and UV cure profile on the acrylate extent of conversion are presented. Continuous and pulsed UV cure profiles are shown to affect total conversion due to variances in radical efficiency at different UV intensities and acrylate concentrations. The effects of acrylate concentration on the kinetics of the epoxy thermal cure and the final mechanical properties are also investigated using dynamic mechanical analysis and three-point bend measurements. The glass transition temperature is dependent on formulation, with increasing acrylate content decreasing the T g . However, the room temperature shear moduli, flexural moduli, strength, strain-to-failure, and toughness values are relatively independent of resin composition. The similarity of the final properties allows for greater flexibility in resin formulation and in situ cure parameters, which can enable the printing of complex parts that require high green strength. We found that the in situ UV print intensities and exposure profiles that are necessary to achieve the best print quality are not, in most cases, the conditions that maximize conversion of the acrylate network. Lastly, this highlights the importance of developing optimized resin compositions which enable complete cure of the acrylate network by promoting acrylate dark cure or thermal cure.

36 MATERIALS SCIENCE↗