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A high modulus polymeric fiber was evaluated as a reinforcement for filament wound pressure vessels. Winding parameters and design data were established for the fiber with two different epoxy resin systems. Comparison was made between the performance factors of the polymeric fiber and those of S-glass and high modulus graphite vessels.
A new high modulus fiber was evaluated as a reinforcement for filament wound pressure vessels. Based on preliminary data it offers significant specific strength and modulus improvements over an S-glass reinforcement. Winding parameters and design data were established for the fiber with two different epoxy resin systems. NOL composite rings were evaluated for tensile strength, modulus and interlaminar shear strength at +70 F, -320 F and -423 F. Results showed that the fiber reinforced composite exhibited a specific strength of 4,100,000 inches and a specific modulus of 290,000,000 inches compared to 3,260,000 inches and 110,000,000 inches respectively for S-glass. Utilizing this data to design small filament wound pressure vessels, a performance factor of 806,000 inches was obtained experimentally with PRD 49-1 fiber compared to values of 632,000 inches and 501,000 inches for S-glass and high modulus graphite vessels, respectively.
Twenty-four different epoxy resin systems were evaluated by a variety of test techniques to identify materials that exhibited improved impact damage tolerance in graphite/epoxy composite laminates. Forty-eight-ply composite panels of five of the material systems were able to sustain 100 m/s impact by a 1.27-cm-diameter aluminum projectile while statically loaded to strains of 0.005. Of the five materials with the highest tolerance to impact, two had elastomeric additives, two had thermoplastic additives, and one had a vinyl modifier; all the five systems used bisphenol A as the base resin. An evaluation of test results shows that the laminate damage tolerance is largely determined by the resin tensile properties, and that improvements in laminate damage tolerance are not necessarily made at the expense of room-temperature mechanical properties. The results also suggest that a resin volume fraction of 40 percent or greater may be required to permit the plastic flow between fibers necessary for improved damage tolerance.
Flight service experience and in-service inspection results are reported for DC-10 graphite composite rudders during the third year of airline service. Test results and status are also reported for ground-based and airborne graphite-epoxy specimens with three different epoxy resin systems to obtain moisture absorption data. Twenty graphite composite rudders were produced, nine of which were installed on commercial aircraft during the past three years. The rudders collectively accumulated 75,863 flight hours. The high time rudder accumulated 12,740 flight hours in slightly over 36 months. The graphite composite rudders were inspected visually at approximately 1000 flight hour intervals and ultrasonically at approximately 3000 flight hour intervals in accordance with in-service inspection plans. All rudders were judged acceptable for continued service as a result of these inspections. Composite moisture absorption data on small specimens, both ground-based and carried aboard three flight-service aircraft, are given. The specimens include Thornel 300 fibers in Narmco 5208 and 5209 resin systems, and Type AS fibers in the Hercules 3501-6 resin system.
Ballistic impact experiments were performed on triaxially braided polymer matrix composites to study the heat generated in the material due to projectile velocity and penetration damage. Quantifying the heat generation phenomenon is crucial for attaining a better understanding of composite behavior and failure under impact loading. The knowledge gained can also be used to improve physics-based models which can numerically simulate impact of composites. Triaxially braided (0/+60/-60) composite panels were manufactured with T700S standard modulus carbon fiber and two epoxy resins. The PR520 (toughened) and 3502 (untoughened) resin systems were used to make different panels to study the effects of resin properties on temperature rise. Ballistic impact tests were conducted on these composite panels using a gas gun, and different projectile velocities were applied to study the effect on the temperature results. Temperature contours were obtained from the rear surface of the panel during the test through a high speed, infrared (IR) thermal imaging system. The contours show that high temperatures were locally generated and more pronounced along the axial tows for the T700S/PR520 composite specimens; whereas, tests performed on T700S/3502 composite panels using similar impact velocities demonstrated a widespread area of lower temperature rises. Nondestructive, ultrasonic C-scan analyses were performed to observe and verify the failure patterns in the impacted panels. Overall, the impact experimentation showed temperatures exceeding 525 K (485degF) in both composites which is well above the respective glass transition temperatures for the polymer constituents. This expresses the need for further high strain rate testing and measurement of the temperature and deformation fields to fully understand the complex behavior and failure of the material in order to improve the confidence in designing aerospace components with these materials.
Composite cryotanks, or composite overwrapped pressure vessels (COPVs), offer advantages over currently used aluminum-lithium cryotanks, particularly with respect to weight savings. Future NASA missions are expected to use COPVs in spaceflight propellant tanks to store fuels, oxidizers, and other liquids for launch and space exploration vehicles. However, reliability, reparability, and reusability of the COPVs are still being addressed, especially in cryogenic temperature applications; this has limited the adoption of COPVs in reusable vehicle designs. The major problem with composites is the inherent brittleness of the epoxy matrix, which is prone to microcrack formation, either from exposure to cryogenic conditions or from impact from different sources. If not prevented, the microcracks increase gas permeation and leakage. Accordingly, materials innovations are needed to mitigate microcrack damage, and prevent damage in the first place, in composite cryotanks. The self-healing technology being developed is capable of healing the microcracks through the use of a novel engineered nanocomposite, where a uniquely designed nanoparticle additive is incorporated into the epoxy matrix. In particular, this results in an enhancement in the burst pressure after cryogenic cycling of the nanocomposite COPVs, relative to the control COPVs. Incorporating a novel, self-healing, epoxy-based resin into the manufacture of COPVs allows repeatable self-healing of microcracks to be performed through the simple application of a low-temperature heat source. This permits COPVs to be reparable and reusable with a high degree of reliability, as microcracks will be remediated. The unique phase-separated morphology that was imparted during COPV manufacture allows for multiple self-healing cycles. Unlike single-target approaches where one material property is often improved at the expense of another, robustness has been introduced to a COPV by a combination of a modified resin and nanoparticle additives. Unique nanoparticles were used that have been surface-functionalized to be compatible with the resin. Both organic and inorganic components toughen the matrix and result in a more impact-resistant COPV. In one resin system containing an inorganic nanomaterial additive, a significant improvement in burst performance was observed after the COPV was cryo-impact-damaged and then self-healed, with a greater than 10% improvement in burst pressure after the self-healing process was performed. Initial cross-sectional analysis via microscopy showed good resin infiltration of the carbon fibers and without voids. To further enhance the capability between the nanomaterial additives and the resin, a surface modification was successfully performed. A second specialty epoxy resin was prepared using a surface modified nanomaterial additive, and COPVs were fabricated. Steps were taken to improve the mechanical properties of the COPVs by using a low-viscosity resin system that contained a different curing agent. This lower viscosity improves the processing of the COPV, and preliminary results show that the burst pressure of these new vessels is 20 to 25% higher than that of the original. The self-healing concept demonstrated in this research and development effort represents a platform technology, and the self-healing property is neither restricted to the particular epoxy system used here, nor to the COPV application. Self-healing is a direct result of a unique phase separated morphology created via the resin and is aided by the nanoparticles. The self-healing function can be introduced to other customer-specific resin systems in coating, bulk, or composite applications provided that the unique phase separated morphology can be enabled in those systems.
A study was carried out to select a state-of-the-art epoxy for wet filament winding. Ten epoxy systems were used to filament wind pressure vessels with a high-modulus, high-strength organic fiber. Data are reported on vessel performance, fiber strand strengths, and shear strengths for the different systems. Using our criteria (processibility, neat resin properties, and vessel performance), we find that an epoxy system based on the rubber-modified bis-phenol-F resin, diluted with vinyl cyclohexane dioxide and cured with mixed aromatic amines, can easily replace bis-phenol-A epoxies diluted with bis-(2, 3-epoxycyclopentyl) ether (such as ERL 2256 epoxy of Union Carbide) with comparable overall performance.
Research was conducted to improve the impact strength and toughness of fiber/resin composites by means of a fiber coating interphase. Graphite fiber/epoxy resin composites were fabricated with four different fiber coating systems introduced in a matrix-fiber interphase. Two graphite fibers, a high strength and a high modulus type, were studied with the following coating systems: chemical vapor deposited boron, electroless nickel, a polyamide-imide resin and a thermoplastic polysulfone resin. Evaluation methods included the following tests: Izod, flexure, shear fracture toughness, longitudinal and transverse tensile, and transverse and longitudinal compression. No desirable changes could be effected with the high strength fiber, but significant improvements in impact performance were observed with the polyamide-imide resin coated high modulus fiber with no loss in composite modulus.
The blending of LARC-TPI polyimide with the thermotropic liquid crystal polymer designated Xydar and with four different oligomeric imide materials has facilitated the resulting resin systems' processing into films while enhancing their mechanical properties and lowering their coefficient of thermal expansion to virtually zero. Two film-formation processes have been evaluated: (1) the casting of polyamic acid films followed by thermal imidization and biaxial stretching, and (2) the blown-film melt-extrusion of fully imidized LARC-TPI polymer. The best results have been obtained through the use of Xydar as a processing aid at levels in the 10-30 percent range.
A second generation polymerization monomeric reactants (PMR) polyimdes matrix system (PMR 2) was characterized in both neat resin and composite form with two different graphite fiber reinforcements. Three different formulated molecular weight levels of laboratory prepared PMR 2 were examined, in addition to a purchased experimental fully formulated PMR 2 precurser solution. Isothermal aging of graphite fibers, neat resin samples and composite specimens in air at 316 C were investigated. Humidity exposures at 65 C and 97 percent relative humidity were conducted for both neat resin and composites for eight day periods. Anaerobic char of neat resin and fire testing of composites were conducted with PMR 15, PMR 2, and an epoxy system. Composites were fire tested on a burner rig developed for this program. Results indicate that neat PMR 2 resins exhibit excellent isothermal resistance and that PMR 2 composite properties appear to be influenced by the thermo-oxidative stability of the reinforcing fiber.
The results are presented of mechanical and physical properties characterization testing for the fiber glass prepreg system used to fabricate 15 of the replacement set of 25 fan blades for the National Transonic Facility. The fan blades were fabricated to be identical to the original blade set with the exception that the 7576 style E glass cloth used for the replacement set has a different surface finish than the original 7576 cloth. The 7781 E glass cloth and resin system were unchanged. The data are presented for elevated, room, and cryogenic temperatures. The results are compared with data from the original blade set and evaluated against selected structural design criteria. Test experience is described along with recommendations for future testing of these materials if required.
Additive manufacturing (AM) enables the fabrication of complex geometries, yet its application to thermosets remains limited by post-processing requirements. Frontal ring-opening metathesis polymerization (FROMP) offers a promising alternative, enabling energy-efficient, in situ curing of freestanding thermoset structures. This study presents a real-time process monitoring and automated control system for direct ink writing (DIW) of FROMP thermosets. By integrating thermochromic leuco dyes and computer vision, we enable real-time polymerization front tracking, allowing autonomous printing parameter adjustments for consistent geometries across resin formulations. The system’s accuracy was validated against manual tracking, demonstrating precise front velocity detection. Its adaptability was confirmed by printing freestanding mechanical springs with different resins, achieving consistent geometries and mechanical properties despite front velocity variations. These findings highlight the potential of automated DIW control for scalable, repeatable, and material-agnostic 3D printing of thermosets.
High temperature stable adhesive systems were evaluated for potential Supersonic Cruise Research (SCR) vehicle applications. The program was divided into two major phases: Phase I 'Adhesive Screening' evaluated eleven selected polyimide (PI) and polyphenylquinoxaline (PPQ) adhesive resins using eight different titanium (6Al-4V) adherend surface preparations; Phase II 'Adhesive Optimization and Characterization' extensively evaluated two adhesive systems, selected from Phase I studies, for chemical characterization and environmental durability. The adhesive systems which exhibited superior thermal and environmental bond properties were LARC-TPI polyimide and polyphenylquinoxaline both developed at NASA Langley. The latter adhesive system did develop bond failures at extended thermal aging due primarily to incompatibility between the surface preparation and the polymer. However, this study did demonstrate that suitable adhesive systems are available for extended supersonic cruise vehicle design applications.
Long Duration Exposure Facility (LDEF) Experiment A0175 involved the non-instrumented exposure of seven carbon-fiber reinforced resin-matrix advanced composite panels contained in two trays - A7 and A1. These two trays were located, respectively, on the leading and trailing faces of LDEF, obliquely oriented to the RAM (Row 9) and WAKE (Row 3) directions. The identity and location of the seven panels, which consisted of six flat laminates of the following material systems are shown: carbon/epoxy (T300/934), carbon/bismaleimide (T300/F178), and carbon/polyimide (C6000/LARC-160 and C6000/PMR-15), plus one bonded honeycomb sandwich panel (T300/934 face sheets and Nomex core) patterned after the Space Shuttle payload bay door construction. These material systems were selected to represent a range of then-available matrix resins which, by virtue of their differing polymer chemistry, could conceivably exhibit differing susceptibility to the low-earth orbit (LEO) environment. The principal exposure conditions of the LDEF environment at these tray locations are shown. Noteworthy to some of the observations discussed is the four-orders-of magnitude difference in the atomic oxygen (AO) fluence, which made a shallow incidence angle (approximately 22 deg) to Tray A7, while Tray A1 on the trailing face was essentially shielded from AO exposure. This evaluation focused on determining the individual and relative suitability of a variety of resin-matrix composite systems for long-term space structural applications. This was accomplished primarily by measuring and comparing a range of engineering mechanical properties on over 300 test coupons sectioned from the flight panels and from identical control panels, and tested at ambient and elevated temperatures. This testing was supported by limited physical characterization, involving visual examination of flight panel surface features, measurements of weight loss and warpage, and examination for changes in internal integrity (micro cracking, delamination) by ultrasonic c-scan and polished cross-sections.
High energy dynamic impact tests were conducted on AS4/PEKK and TC1225 LMPAEK T700G thermoplastic quasi-isotropic laminated tape composite panels. The primary objective was to provide data for evaluation of computational composite impact models. Measurements include transient deformations, pre- and post-test characterization of delamination and energy threshold for onset of delamination and onset of penetration. Empirical results indicate an approximately 50% increase in penetration threshold velocity and over 100% increase in penetration energy threshold for the TC1225 LMPAEK T700G composite compared to the AS4/PEKK composite. The velocity required to produce NDE-detectable delamination in the TC1225 LMPAEK T700G composite was roughly twice that for the AS4/PEKK composite. Results will be compared with those from a thermoset composite system with a similar architecture. Because of differences in the chemical structure of the two resins, differences in the impact response are to be expected.
Bisphenol A-based epoxies are much used in a wide range of composite and coating applications due to their excellent thermomechanical properties. However, their 3D printability remains a challenge with most reported materials suffering from high brittleness and low toughness. In this work, we have described especially modified epoxy resins that enable 3D printing with both fast and slow curing rates. These materials exhibit greatly enhanced toughness, tunable thermomechanical properties, and excellent shape memory behavior. Two different printing systems, including a two-part static mixing printhead and a single extrusion printhead, were developed for fast- and slow-curing epoxies, respectively. The rheology of inks in both systems has been modified into printable thixotropic fluids with the aid of silica nanoparticles and other additives. Epoxide-functionalized telechelic polybutadiene was added into the resins, which are then introduced inside the epoxy network after cross-linking. The addition of polybutadiene rubber significantly improves the toughness (over 135%), fracture strain (over 200%), and shape memory behavior. By adding different amounts of the rubber telechelic, thermomechanical properties, including modulus, elongation, and Tg of epoxy, can be well controlled in a wide range to satisfy different applications.
This paper introduces an Ensemble Cure Kinetics Network (ECK-Net), a neural network (NN)–based framework for modeling the cure kinetics of thermosetting resins within a phenomenological context. ECK-Net replaces traditional analytic models, which require extensive chemical insight and multiple isothermal/non-isothermal experiments, with a data-driven surrogate that maps nonlinear relationships between temperature, degree of cure, and reaction rate from differential scanning calorimetry data. The proposed approach predicts input-dependent kinetic coefficients of a generalized nth-order reaction equation rather than reaction rates directly, enabling a single unified model to represent various epoxy systems without relying on iso-conversional analysis or predefined functional forms. To ensure robustness, multiple independently trained networks under different random initializations are blended through an ensemble strategy, effectively mitigating the stochastic variability inherent to neural networks. The framework is validated using experimental datasets from multiple resin systems, including aerospace-grade materials (Toray 3900-2, Cycom 5320-1, and Hexcel 8552) and a windmill-grade resin (RIMR 035c). The model accurately reproduces the temporal evolution of the degree of cure under manufacturers’ recommended cure cycles across all tested resins systems, yielding Pearson’s correlation coefficients of 0.992, 0.994, 0.993, 0.997, respectively. To demonstrate process-level applicability, the trained network was implemented within the Abaqus environment to simulate out-of-autoclave (OOA) curing process of the CFRP panel composed of Toray T830H-6K/3900-2D prepreg. The simulation results showed excellent agreement with experimental temperature response (maximum peak temperature, simulation: 189.6 °C, experiment: 188.5 °C) and the final degree of cure (simulation: 0.948, experiment: 0.960 ± 0.013), confirming ECK-Net’s capability as a reliable alternative to conventional cure kinetics modeling methods.
Engineers today are presented with the opportunity to design and build the next generation of space vehicles out of the lightest, strongest, and most durable materials available. Composites offer excellent structural characteristics and outstanding reliability in many forms that will be utilized in future aerospace applications including the Commercial Crew and Cargo Program and the Orion space capsule. NASA's Composites for Exploration (CoEx) project researches the various methods of manufacturing composite materials of different fiber characteristics while using proven infusion methods of different resin compositions. Development and testing on these different material combinations will provide engineers the opportunity to produce optimal material compounds for multidisciplinary applications. Through the CoEx project, engineers pursue the opportunity to research and develop repair patch procedures for damaged spacecraft. Working in conjunction with Raptor Resins Inc., NASA engineers are utilizing high flow liquid infusion molding practices to manufacture high-temperature composite parts comprised of intermediate modulus 7 (IM7) carbon fiber material. IM7 is a continuous, high-tensile strength composite with outstanding structural qualities such as high shear strength, tensile strength and modulus as well as excellent corrosion, creep, and fatigue resistance. IM7 carbon fiber, combined with existing thermoset and thermoplastic resin systems, can provide improvements in material strength reinforcement and deformation-resistant properties for high-temperature applications. Void analysis of the different layups of the IM7 material discovered the largest total void composition within the [ +45 , 90 , 90 , -45 ] composite panel. Tensile and compressional testing proved the highest mechanical strength was found in the [0 4] layup. This paper further investigates the infusion procedure of a low-cost/high-performance BMI resin into an IM7 carbon fiber material and the optical, chemical, and mechanical analyses performed.