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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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Suppressing proximity effects during rapid serial two-photon lithography through tuning of reaction–diffusion kinetics

The ability of two-photon lithography (TPL) to print deterministic nanoporous 3D structures is highly valuable for many applications. However, it is challenging to print such structures rapidly due to the proximity effects that cause closely spaced features to enlarge and merge. A key challenge is the limited understanding of the origins and spatiotemporal dynamics of the long-range proximity effects that extend beyond the optical focal spot. Here, we empirically investigate these proximity effects in serial TPL using custom-made acrylate-based photoresists. We demonstrate that the complex spatiotemporal dynamics of the proximity effects can be explained through the kinetics of the reaction–diffusion photopolymerization mechanisms that underlie the curing process. Specifically, we show that the proximity effects arise due to comparable timescales of reaction and diffusion of oxygen. Furthermore, we demonstrate that long-range proximity effects can be suppressed by introducing phenolic inhibitors, which reduce oxygen consumption through non-inhibiting side reactions and promote faster termination of curing reactions. These insights enabled improving the linewidths from >400 to 260 nm during printing of nanoporous 3D woodpiles at scanning speeds of 50 mm s −1 . Thus, the knowledge generated here can be applied to deterministically tune the proximity effects and enable rapid printing of high-resolution nanoporous 3D structures.

36 MATERIALS SCIENCE↗
NASA NTRS2023

Ultrasonic Inspection During Autoclave Cure of Reflowable-Interface Composite Joints

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making the interface susceptible to minute quantities of contamination, which can cause weak bonds. Regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded primary-structures due to uncertainty in bond performance. To address this issue, the NASA Convergent Aeronautics Solutions (CAS): Adhesive Free Bonding of Composites (AERoBOND) project is investigating reformulated aerospace epoxy-matrix resins to enable reflow and diffusion of the resin at the joint interface during a secondary bonding and cure process that can eliminate the material discontinuity at the interface. Implementing in-situ process monitoring enables assessing the bond quality during processing rather than waiting for post-fabrication mechanical testing to be completed. In this paper, an in-situ ultrasonic inspection system is used to monitor the joining of three composite laminates assembled using the AERoBOND technique. For each panel, the amplitude of the wave reflection at the joint was measured throughout the cure cycle. The results indicate the timing and extent of reflow and cure of the epoxy resin at the joint. Factors indicating end of cure were ascertained and a metric was developed to qualitatively predict acceptable mode-II fracture toughness based on the ultrasonic amplitude at the joint line during cure. In addition, since the inspection system scans an area of the joint, high-resolution localized results can be obtained across the joint.

Tyler B Hudson↗
NASA NTRS1991

The full-scale process and design changes for elimination of insulation edge separations and voids in tang flap area

Qualification of the full-scale process and design changes for elimination of redesigned solid rocket motor tang nitrile butadiene rubber insulation edge separations and voids was performed from 24 March to 3 December 1990. The objectives of this test were: to qualify design and process changes on flight hardware using a tie ply between the redesigned solid rocket motor steel case and the nitrile butadiene rubber insulation over the tang capture features; to qualify the use of methyl ethyl ketone in the tang flap region to reduce voids; and to determine if holes in the separator film reduce voids in the tang flap region. The tie ply is intended to aid insulation flow during the insulation cure process, and thus reduce or eliminate edge unbonds. Methyl ethyl ketone is intended to reduce voids in the tang flap area by providing better tacking characteristics. The perforated film was intended to provide possible vertical breathe paths to reduce voids in the tang area. Tang tie ply testing consisted of 270 deg of the tang circumference using a new layup method and 90 deg of the tang circumference using the current layup methods. Tie ply process success was defined as a reduction of insulation unbonds. Lack of any insulation edge unbonds on the tang area where the new process was used, and the presence of 17 unbonds with the current process, proves the test to be a success. Successful completion of this test has qualified the new processes.

Danforth, Richard A.↗
NASA NTRS1982

High-temperature resins

The basic chemistry, cure processes, properties, and applications of high temperature resins known as polyimides are surveyed. Condensation aromatic polymides are prepared by reacting aromatic diamines with aromatic dianhydrides, aromatic tetracarboxylic acids, or with dialkyl esters of aromatic tetracarboxylic acids, depending on the intended end use. The first is for coatings or films while the latter two are more suitable for polyimide matrix resins. Prepreg solutions are made by dissolving reactants in an aprotic solvent, and advances in the addition of a diamine on the double bond and radical polymerization of the double bond are noted to have yielded a final cure product with void-free characteristics. Attention is given to properties of the Skybond, Pyralin, and NR-150B polyimide prepreg materials and characteristics of aging in the NP-150 polyimides. Finally, features of the NASA-developed PMR polyimides are reviewed.

Serafini, T. T.↗
NASA NTRS1990

Filament winding cylinders. II - Validation of the process model

Analytical and experimental studies were performed to validate the model developed by Lee and Springer for simulating the manufacturing process of filament wound composite cylinders. First, results calculated by the Lee-Springer model were compared to results of the Calius-Springer thin cylinder model. Second, temperatures and strains calculated by the Lee-Springer model were compared to data. The data used in these comparisons were generated during the course of this investigation with cylinders made of Hercules IM-6G/HBRF-55 and Fiberite T-300/976 graphite-epoxy tows. Good agreement was found between the calculated and measured stresses and strains, indicating that the model is a useful representation of the winding and curing processes.

Calius, Emilio P.↗
NASA NTRS2004

Composite-Material Tanks with Chemically Resistant Liners

Lightweight composite-material tanks with chemically resistant liners have been developed for storage of chemically reactive and/or unstable fluids . especially hydrogen peroxide. These tanks are similar, in some respects, to the ones described in gLightweight Composite-Material Tanks for Cryogenic Liquids h (MFS-31379), NASA Tech Briefs, Vol. 25, No. 1 (January, 2001), page 58; however, the present tanks are fabricated by a different procedure and they do not incorporate insulation that would be needed to prevent boil-off of cryogenic fluids. The manufacture of a tank of this type begins with the fabrication of a reusable multisegmented aluminum mandrel in the shape and size of the desired interior volume. One or more segments of the mandrel can be aluminum bosses that will be incorporated into the tank as end fittings. The mandrel is coated with a mold-release material. The mandrel is then heated to a temperature of about 400 F (approximately equal to 200 C) and coated with a thermoplastic liner material to the desired thickness [typically approxiamtely equal to 15 mils (approximately equal to 0.38 mm)] by thermal spraying. In the thermal-spraying process, the liner material in powder form is sprayed and heated to the melting temperature by a propane torch and the molten particles land on the mandrel. The sprayed liner and mandrel are allowed to cool, then the outer surface of the liner is chemically and/or mechanically etched to enhance bonding of a composite overwrap. The etched liner is wrapped with multiple layers of an epoxy resin reinforced with graphite fibers; the wrapping can be done either by manual application of epoxy-impregnated graphite cloth or by winding of epoxy-impregnated filaments. The entire assembly is heated in an autoclave to cure the epoxy. After the curing process, the multisegmented mandrel is disassembled and removed from inside, leaving the finished tank. If the tank is to be used for storing hydrogen peroxide, then the liner material should be fluorinated ethylene/propylene (FEP), and one or more FEP O ring(s) should be used in the aluminum end fitting(s). This choice of materials is dictated by experimental observations that pure aluminum and FEP are the only materials suitable for long-term storage of hydrogen peroxide and that other materials tend to catalyze the decomposition of hydrogen peroxide to oxygen and water. Other thermoplastic liner materials that are suitable for some applications include nylon 6 and polyethylene. The processing temperatures for nylon 6 are lower than those for FEP. Nylon 6 is compatible with propane, natural gas, and other petroleum-based fuels. Polyethylene is compatible with petroleum- based products and can be used for short-term storage of hydrogen peroxide.

DeLay, Thomas K.↗
DOE OSTI2020

Tailored Graphene Micropatterns by Wafer-Scale Direct Transfer for Flexible Chemical Sensor Platform

2D materials, such as graphene, exhibit great potential as functional materials for numerous novel applications due to their excellent properties. The grafting of conventional micropatterning techniques on new types of electronic devices is required to fully utilize the unique nature of graphene. However, the conventional lithography and polymer-supported transfer methods often induce the contamination and damage of the graphene surface due to polymer residues and harsh wet-transfer conditions. In this work, a novel strategy to obtain micropatterned graphene on polymer substrates using a direct curing process is demonstrated. Employing this method, entirely flexible, transparent, well-defined self-activated graphene sensor arrays, capable of gas discrimination without external heating, are fabricated on 4 in. wafer-scale substrates. Finite element method simulations show the potential of this patterning technique to maximize the performance of the sensor devices when the active channels of the 2D material are suspended and nanoscaled. This study contributes considerably to the development of flexible functional electronic devices based on 2D materials.

2D materials, Graphene, Microscale patterning, Che↗
DOE OSTI2022

Bio‐Based Piezo‐ and Thermoresistive Photocurable Sensing Materials from Acrylated Epoxidized Soybean Oil

Abstract Bio‐based photocurable polymers are increasingly in demand as environmentally friendly materials for advanced applications. Together with functional fillers, these represent a next step for the generation of functional and active smart materials, compatible with additive manufacturing technologies. Herein, acrylated epoxidized soybean oil (AESO) mixed with different amounts of reduced graphene oxide (rGO) up to 6 wt% in order to obtain UV‐curable piezoresistive and thermoresistive materials, is reported. It is shown that the addition of rGO to AESO hinders the curing process, but always maintains double bond conversions higher than 50%. Composites are characterized by a good dispersion of micrometric filler clusters. Further, the thermal stabilities are close to 300 °C and crosslinking degrees are above 1.75 mmol cm –3 . The Young modulus of the composites decreases with the addition of the rGO fillers, in particular for the higher filler contents, and electrical conductivities up to 0.13 S m –1 are obtained for the composites with the highest rGO content. UV‐curable composites with piezoresistive and thermoresistive responses suitable for applications are thus obtained, characterized by gauge factors around 26 for deformations up to 2% and maximum thermoresistive sensitivity of S = 0.43, values similar to the values obtained for petroleum‐based materials.

Mendes‐Felipe, Cristian↗
DOE OSTI2020

An in-situ crosslinking binder for binder jet additive manufacturing

Additive Manufacturing (AM) of metals is a potentially disruptive technology that could significantly change the industrial supply chain. There are a limited number of AM methods capable of creating metal parts, and one method showing significant potential is Binder Jet AM (Binder Jetting). Binder Jetting utilizes an inkjet print head to deposit a binder fluid onto a powder bed and bind together powder particles into a desired geometry. This study investigates a new binder system consisting of a difunctional monomer, triethylene glycol dimethacrylate (TEG-DMA). TEG-DMA exhibits excellent printability with an Ohnesorge’s number of .258 making the Z number 3.876. During the thermal curing process, the difunctional monomer polymerizes and crosslinks at the onset temperature of 138 °C, becoming a solid dimethacrylate network. When the binder is utilized within the stainless-steel powder bed at 200 °C, it forms a network incorporating the stainless-steel particles, binding the powder into any specified geometry. Crosslinking the monomer within the stainless-steel 420 powder bed imparts a flexural strength of 1.0–3.3 MPa to the green part depending on the volume of monomer in the part. After sintering, the final stainless-steel parts results in a void fraction close to 60 % and carbon content below 0.4 %.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Structural stability of thin overhanging walls during material extrusion additive manufacturing of thermoset-based ink

Recent developments have enabled material extrusion additive manufacturing of thermoset-based composite inks on the large scale. In addition, printing out-of-plane components is of broad interest to the polymer material extrusion community. Here, we address some of the challenges associated with both large-scale and out-of-plane thermoset material extrusion additive manufacturing by studying the height at which thin overhanging walls collapse. Walls at a range of overhang angles were printed until they collapsed. An optical camera captured the profile of each wall throughout the print, allowing the collapse height to be identified and the geometric fidelity to the programmed angle to be evaluated. Using previously measured rheological properties, predictive models were generated to approximate the collapse height and profile of the deflected walls. First, an analytical model was created to predict the height at which the walls would yield. The analytical model assumes the walls exhibit a perfectly linear profile; however, experiments proved this assumption to be false. Therefore, a finite element simulation was developed to account for the elastic deflection that occurs during printing. The finite element simulation predicts both the yield height and the deflected profile after the deposition of each layer. For the properties of the thermoset ink used here, the yield height predicted by the analytical model and finite element simulation are virtually identical. These predictions match experimental data reasonably well, but minor errors are observed. Accounting for the fully plastic moment appears to explain the small mismatch between experimental data and predictions. Additionally, the finite element simulation provides an excellent prediction of the deflected profile before the wall begins to collapse. Finally, by demonstrating that the collapse height and deflected profile of thin overhanging walls can be predicted, this work illustrates how the soft viscoelastic properties of thermoset-based composite inks limit the scale of a key feature required to print some nonplanar components. It also provides a basis to tailor in-process curing systems to suppress deflection and collapse of thin overhanging walls.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Stimuli-responsive petroleum cement composite with giant expansion and enhanced mechanical properties

Shrinkage, as an inherent property of cement during the curing process, has been a concern in the oil & gas industry for centuries. Therefore, expansive cement has been studied for many decades, primarily through incorporation of expansive additives. Nevertheless, traditional expansive additives are not able to achieve the required expansive ratio or maintain a good mechanical property for the cement composite at extreme underground condition. Accordingly, a new generation of expansive additive, which not only has the required expansion, but also work at the downhole high temperature and high pressure environment, and maintain or even enhance the mechanical property, is highly desired. In this work, a high enthalpy storage shape memory polymer (SMP) as a new class of expansive additive is investigated. It is found that the cement composite achieves 1.4% circumferential expansion by only 6% by weight of SMP additives. The compressive strength and flexural strength are also enhanced at the same time, which is hardly achievable by other expansive additives with the same concertation. Good pumpability is also proved by rheological study. The mechanism controlling the enhanced properties is reveled through morphological study and element mapping analysis at the SMP/cement interface.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Network stability of FKM rubber compounds under hydrogen pressure

Fluorocarbon-based rubber (FKM) compounds are typically utilized in the aeronautical industry due to its exceptional chemical and thermal resistance and recently has drawn significant interest from the hydrogen community for various hydrogen applications, but there exists little data evaluating its hydrogen compatibility. In this paper, a formulated FKM compound was exposed to ultrahigh hydrogen pressure (90 MPa) and analyzed by attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and crosslinking densities by solvent swelling measurement. ATR-FTIR spectroscopic data demonstrated that high-pressure hydrogen not only caused cleavages in polymer backbone and cross linkages, but also induced additional degradation of FKM compounds by breaking intermolecular hydrogen bonding between carboxylic acids, which were produced during rubber molding and post curing processes. This hydrogen pressure-driven degradation was significantly higher towards the core of the material than at the surface due to its weaker bonding between polymers and fillers.

Polymers, hydrogen, stability, degradation, Charac↗
DOE OSTI2025

Shock-induced chemistry and high strain-rate viscoelastic behavior of a phenolic polymer

We use impact experiments and a finite element model (up to 1.2 GPa), and molecular dynamics simulations (up to 60 GPa), to examine the behavior of a phenolic polymer under shock compression, spanning both nonreactive and reactive regimes. In the nonreactive regime, relaxation following compression at strain rates of ∼105 s−1 can be explained by viscoelasticity observed at ordinary laboratory rates (≲1 s−1) by accounting for the temperature dependence of the phenolic β-transition. Reasonable agreement is found between the measured shock Hugoniot up to 1.2 GPa and molecular dynamics simulation for cross-linked structures of comparable density. We also observed a first-order mechanical transition near 0.36 GPa shock stress and estimated a spall strength of 0.102 GPa and Hugoniot elastic limit of 1–2 GPa. The shock stress is found to vary up to 24% among phenolics made with different resin and/or cure processes. Finally, molecular dynamics simulations are used to identify a reactive regime at shock pressures ≳20 GPa that is characterized by chemically driven, rate-dependent relaxation processes, including dehydrogenation and dehydration reactions that promote the formation of a dense, highly cross-linked carbonaceous solid and the release of light volatiles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Encapsulation Residual Stress and Ferrite Loss in Inductive Coil Assemblies

As inductive wireless charging reaches higher power levels, thermal management and mechanical durability become more critical. To address these concerns, past works have demonstrated the benefit of encapsulating coil assemblies in thermally conductive materials. However, due to the sensitivity of the MnZn ferrites commonly used in coil assemblies to mechanical stress, care must be taken to avoid creating large stresses in the ferrite that cause higher hysteresis loss. The stress formation in the encapsulant curing process is overviewed and modeled and an experiment is performed to demonstrate the effect in a small-scale coil assembly. Finally, the effect is shown in the reduced coil-coil efficiency of a first generation high power inductive power transfer prototype using a stiff epoxy compared to better performance in a second prototype using a softer thermally-conductive silicone encapsulant.

Foote, Andrew↗
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 OSTI2022

Low-Temperature Architected Cementation Agents (LAMINAE)

The cement industry contributes 5-9% of all anthropogenic CO 2 . At the same time, current concrete curing processes are passive, with little-to-no control over microstructure. The LAMINAE process offers the potential for a low-temperature pathway for producing cementitious aluminosilicate hydrate (zeolite) structures which: (a) reduces the energy burden of cement production by 30%, (b) reduces CO 2 emissions by 60%, and (c) offers microstructure control as was implicitly ensured in Roman concrete. This project generated data and engineering correlations to support further scale up and design of initial commercial processes.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Porous Polymeric Materials FY24 PDRD Final Report

Fillers and pore formers are used in many materials at Kansas City National Security Campus (KCNSC) to fine tune density and stiffness. Current off-the-shelf options such as urea and Expancel do not always provide the desired properties. This project investigated several methods for introducing porosity in rigid polymers such as epoxy and polyurethane. This work was done at partnering universities to identify a variety of methods to create porous polymeric materials. The University of Oklahoma (OU) investigated emulsion templating of epoxy, where the epoxy is mixed with a surfactant and water to form an emulsion. The emulsion is then molded and cured. During the cure process, water droplets evaporate to form porous structures. Total porosity can be tuned by changing the concentration of water added to the polymer. The University of Kansas (KU) investigated the synthesis of phenolic microballoons by spray drying, as well as methods of incorporating removable porogens into epoxy and polyurethane materials to create polymeric foams.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗