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DOE OSTI2025

Material Extrusion Printing of Poly(Acrylonitrile‐Styrene‐Acrylate) and Poly(Acrylonitrile‐Butadiene‐Styrene) Structures Reinforced with Poly(Phenylene Oxide) Additives for Improved Thermomechanical Properties and their Surface Analysis by Time‐of‐Flight Secondary Ion Mass Spectrometry

Fused filament fabrication offers the ability to 3D print complex geometries made from plastic filament materials; however, these parts are mechanically outperformed by parts created by traditional fabrication methods. To overcome this challenge, a high-performance polymer poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) is incorporated as an additive into two common engineering thermoplastics, poly(acrylonitrile-styrene-acrylate) (ASA) and poly(acrylonitrile-butadiene-styrene) (ABS). Structures printed from these polymer blends are more mechanically robust compared to those prepared from the parent polymers, with low loading levels (1–5 wt%) of PPO improving the elastic strength by up to ≈30% relative to the parent terpolymers. Even at higher loading levels (10 and 20 wt% PPO), there is no evidence of additive aggregation in the model thin films, which is supported by compositional analysis of the copolymers and chemical analysis via time-of-flight secondary ion mass spectrometry. The enhancements in mechanical properties of ASA and ABS blends appear to be a consequence of homogeneous incorporation of the PPO additive. In conclusion, this work explores expanding materials-property space using miscible blends of engineering thermoplastics to improve mechanical performance as a general approach to overcoming challenges with parts created by melt-based material extrusion printing.

additive manufacturing↗

NASA NTRS1982

Polymer research at NASA Langley Research Center

Polymer synthesis programs involve the development of Novel thermoplastics, pseudothermoplastics, and thermosets. These systems are prepared to elucidate structure-property relationships involving thermal capabilities, toughness, processability and environmental stability. Easily processable polyimides, solvent-resistant polysulfones and polyphenylquinoxalines, and tougher high and intermediate temperature polymers were developed. Characterization efforts included high pressure liquid chromatography methodology, the development of toughness tests for fiber reinforced composites, a study of electrical properties of metal ion filled polyimides, and a study of the mutagenicity of aromatic diamines. Also the mechanism of cure/degradation of experimental polymers was studied by rheology, mechanical behavior, separation techniques and spectroscopy. The degradative crosslinking of alkyl-containing polyimides, the separation and identification of crosslinked phenylquinoxalines, the rheological behavior of hot-melt polyimides, and the elucidation of the cure of norbornene endcapped imides were also studied.

Terry L. St. Clair↗

DOE OSTI2025

Pultrusion and Vitrimer Composites: Emerging Pathways for Sustainable Structural Materials

Pultrusion is a manufacturing process used to produce fiber-reinforced polymer composites with excellent mechanical, thermal, and chemical properties. The resulting materials are lightweight, durable, and corrosion-resistant, making them valuable in aerospace, automotive, construction, and energy sectors. However, conventional thermoset composites remain difficult to recycle due to their infusible and insoluble cross-linked structure. This review explores integrating vitrimer technology a novel class of recyclable thermosets with dynamic covalent adaptive networks into the pultrusion process. As only limited studies have directly reported vitrimer pultrusion to date, this review provides a forward-looking perspective, highlighting fundamental principles, challenges, and opportunities that can guide future development of recyclable high-performance composites. Vitrimers combine the mechanical strength (tensile strength and modulus) of thermosets with the reprocessability and reshaping of thermoplastics through dynamic bond exchange mechanisms. These polymers offer high-temperature reprocessability, self-healing, and closed-loop recyclability, where recycling efficiency can be evaluated by the recovery yield retention of mechanical properties and reuse cycles meeting the demand for sustainable manufacturing. Key aspects discussed include resin formulation, fiber impregnation, curing cycles, and die design for vitrimer systems. The temperature-dependent bond exchange reactions present challenges in achieving optimal curing and strong fiber–matrix adhesion. Recent studies indicate that vitrimer-based composites can maintain structural integrity while enabling recycling and repair, with mechanical performance such as flexural and tensile strength comparable to conventional composites. Incorporating vitrimer materials into pultrusion could enable high-performance, lightweight products for a circular economy. The remaining challenges include optimizing curing kinetics, improving interfacial adhesion, and scaling production for widespread industrial adoption.

Fiber composites↗

DOE OSTI2023

Multiphysics Modeling Framework for Soft PVC Gel Sensors with Experimental Comparisons

Polyvinyl chloride (PVC) gels have recently been found to exhibit mechanoelectrical transduction or sensing capabilities under compressive loading applications. This phenomenon is not wholly understood but has been characterized as an adsorption-like phenomena under varying amounts and types of plasticizers. A different polymer lattice structure has also been tested, thermoplastic polyurethane, which showed similar sensing characteristics. This study examines mechanical and electrical properties of these gel sensors and proposes a mathematical framework of the underlying mechanisms of mechanoelectrical transduction. COMSOL Multiphysics is used to show solid mechanics characteristics, electrostatic properties, and transport of interstitial plasticizer under compressive loading applications. The solid mechanics takes a continuum mechanics approach and includes a highly compressive Storakers material model for compressive loading applications. The electrostatics and transport properties include charge conservation and a Langmuir adsorption migration model with variable diffusion properties based on plasticizer properties. Results show both plasticizer concentration gradient as well as expected voltage response under varying amounts and types of plasticizers. Experimental work is also completed to show agreeance with the modeling results.

42 ENGINEERING↗

DOE OSTI2022

High Bio-Content Thermoplastic Polyurethanes from Azelaic Acid

To realize the commercialization of sustainable materials, new polymers must be generated and systematically evaluated for material characteristics and end-of-life treatment. Polyester polyols made from renewable monomers have found limited adoption in thermoplastic polyurethane (TPU) applications, and their broad adoption in manufacturing may be possible with a more detailed understanding of their structure and properties. To this end, we prepared a series of bio-based crystalline and amorphous polyester polyols utilizing azelaic acid and varying branched or non-branched diols. The prepared polyols showed viscosities in the range of 504–781 cP at 70 °C, with resulting TPUs that displayed excellent thermal and mechanical properties. TPUs prepared from crystalline azelate polyester polyol exhibited excellent mechanical properties compared to TPUs prepared from amorphous polyols. These were used to demonstrate prototype products, such as watch bands and cup-shaped forms. Importantly, the prepared TPUs had up to 85% bio-carbon content. Studies such as these will be important for the development of renewable materials that display mechanical properties suitable for commercially viable, sustainable products.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS1984

Liquid crystal polyester-carbon fiber composites

Liquid crystal polymers (LCP) have been developed as a thermoplastic matrix for high performance composites. A successful melt impregnation method has been developed which results in the production of continuous carbon fiber (CF) reinforced LCP prepreg tape. Subsequent layup and molding of prepreg into laminates has yielded composites of good quality. Tensile and flexural properties of LCP/CF composites are comparable to those of epoxy/CF composites. The LCP/CF composites have better impact resistance than the latter, although epoxy/CF composites possess superior compression and shear strength. The LCP/CF composites have good property retention until 200 F (67 % of room temperature value). Above 200 F, mechanical properties decrease significantly. Experimental results indicate that the poor compression and shear strength may be due to the poor interfacial adhesion between the matrix and carbon fiber as adequate toughness of the LCP matrix. Low mechanical property retention at high temperatures may be attributable to the low beta-transition temperature (around 80 C) of the LCP matrix material.

Chung, T. S.↗

NASA NTRS2003

Using Diffusion Bonding in Making Piezoelectric Actuators

A technique for the fabrication of piezoelectric actuators that generate acceptably large forces and deflections at relatively low applied voltages involves the stacking and diffusion bonding of multiple thin piezoelectric layers coated with film electrodes. The present technique stands in contrast to an older technique in which the layers are bonded chemically, by use of urethane or epoxy agents. The older chemical-bonding technique entails several disadvantages, including the following: It is difficult to apply the bonding agents to the piezoelectric layers. It is difficult to position the layers accurately and without making mistakes. There is a problem of disposal of hazardous urethane and epoxy wastes. The urethane and epoxy agents are nonpiezoelectric materials. As such, they contribute to the thickness of a piezoelectric laminate without contributing to its performance; conversely, for a given total thickness, the performance of the laminate is below that of a unitary piezoelectric plate of the same thickness. The figure depicts some aspects of the fabrication of a laminated piezoelectric actuator by the present diffusion- bonding technique. First, stock sheets of the piezoelectric material are inspected and tested. Next, the hole pattern shown in the figure is punched into the sheets. Alternatively, if the piezoelectric material is not a polymer, then the holes are punched in thermoplastic films. Then both faces of each punched piezoelectric sheet or thermoplastic film are coated with a silver-ink electrode material by use of a silkscreen printer. The electrode and hole patterns are designed for minimal complexity and minimal waste of material. After a final electrical test, all the coated piezoelectric layers (or piezoelectric layers and coated thermoplastic films) are stacked in an alignment jig, which, in turn, is placed in a curved press for the diffusion-bonding process. In this process, the stack is pressed and heated at a specified curing temperature and pressure for a specified curing time. The pressure, temperature, and time depend on the piezoelectric material selected. At the end of the diffusion-bonding process, the resulting laminated piezoelectric actuator is tested to verify the adequacy of the mechanical output as a function of an applied DC voltage.

Sager, Frank E.↗

NASA NTRS1988

Reinforcing of thermoplastic polycarbonate and polysulfone with carbon fibers: Production and characteristics of UD-compound objects

The production and characteristics of the carbon fiber reinforced thermoplastics polycarbonate and polysulfone are described. The production of prepregs from defined polymer solutions is emphasized along with methods of optimizing the production of compounds. The characteristics of unidirectionally reinforced thermoplastics, such as shear strength, bending strength, and impact resistance are compared with regard to fracture behavior, the influence of intermediate layers, and the behavior under cryogenic conditions and under slightly elevated temperatures. The problem of adhesion between high strength carbon fibers and thermoplastics is examined, taking into account the effect of moisture on the shear strength and the impact resistance.

Fitzer, E.↗

DOE OSTI2022

Post polymerization cure shape memory polymers

This invention relates to chemical polymer compositions, methods of synthesis, and fabrication methods for devices regarding polymers capable of displaying shape memory behavior (SMPs) and which can first be polymerized to a linear or branched polymeric structure, having thermoplastic properties, subsequently processed into a device through processes typical of polymer melts, solutions, and dispersions and then crossed linked to a shape memory thermoset polymer retaining the processed shape.

Wilson, Thomas S.↗

DOE OSTI2024

Post polymerization cure shape memory polymers

Wilson, Thomas S.↗

NASA NTRS1989

Morphological control of inter-penetrating polymer networks

Synthetic organic polymer chemistry has been successful in producing composition of matter with thermal oxidation stability and progressively higher glass transition temperatures. In part, this was done by increasing the steric-hindrance of moieties in the chain of a macromolecule. The resulting polymers are usually quite insoluble and produce molten polymers of very high viscosities. These types of polymers are not easily processed into graphite fiber prepregs by melt or solution impregnation methods. Hence, a technological need exists to produce new knowledge of how to produce polymer-fiber composites from this class of polymers. The concept of freeze drying amic-acid prepolymers with reactive thermoplastic was proposed as a research topic for the ASEE/NASA Summer Faculty Program of 1989 as a means of producing polymer-fiber composites. This process scheme has the thermodynamic attribute that the magnitude of phase separation due to differences in solubility of two organic constituents in solution will be greatly reduced by removing a solvent not by evaporation but by sublimation. Progress to date on evaluating this polymer processing concept is briefly outlined.

Hansen, Marion↗

NASA NTRS1981

Flow properties of a series of experimental thermoplastic polymides

The softening temperature to degradation temperature range of the polymers was about 440 to 650 K. All of the polymers retained small amounts of solvent as indicated by an increase in T(sub g) as the polymers were dried. The flow properties showed that all three polymers had very high apparent viscosities and would require high pressures and/or high temperatures and/or long times to obtain adequate flow in prepregging and molding. Although none was intended for such application, two of the polymers were combined with carbon fibers by solution prepregging. The prepregs were molded into laminates at temperatures and times, the selection of which was guided by the results from the flow measurements. These laminates had room temperature short beam shear strength similar to that of carbon fiber laminates with a thermosetting polyimide matrix. However, the strength had considerable scatter, and given the difficult processing, these polymides probably would not be suitable for continuous fiber composites.

Burks, H. D.↗

DOE OSTI2025

Mechanical and Thermal Characterization of Additively Manufactured Carbon/Nylon 12 and Carbon/PEEK Composites

This study explores additive manufacturing of carbon fiber-reinforced thermoplastic composites using the Composite-Based Additive Manufacturing (CBAM) process. Carbon/Nylon 12 and Carbon/PEEK composites were fabricated and evaluated through mechanical (compression, tensile, flexural, and impact) and thermal (DSC and TGA) tests. Carbon/PEEK exhibited superior mechanical performance, with 97.5% higher tensile strength, 79.8% higher elastic modulus, and 59.6% higher flexural strength compared to Carbon/Nylon 12. Thermal testing showed that Carbon/PEEK had higher thermal stability, beginning degradation at 350 °C versus 298 °C for Carbon/Nylon. These results indicate that CBAM-fabricated Carbon/PEEK composites are suitable for applications requiring high strength and temperature resistance.

Additive manufacturing↗

DOE OSTI2021

Morphological Studies of Solution-Crystallized Thermoplastic Elastomers with Polyethylene Endblocks and a Random-Copolymer Midblock

Styrenic thermoplastic elastomers (TPEs) in the form of triblock copolymers possessing glassy endblocks and a rubbery midblock account for the largest global market of TPEs worldwide, and typically rely on microphase separation of the endblocks and the subsequent formation of rigid microdomains to ensure satisfactory network stabilization. In this work, the morphological characteristics of a relatively new family of crystallizable TPEs that instead consist of polyethylene endblocks and a random-copolymer midblock composed of styrene and (ethylene-co-butylene) moieties are investigated. Copolymer solutions prepared at logarithmic concentrations in a slightly endblock-selective solvent are subjected to crystallization under different time and temperature conditions to ascertain if copolymer self-assembly is directed by endblock crystallization or vice versa. According to transmission electron microscopy, semicrystalline aggregates develop at the lowest solution concentration examined (0.01 wt%), and the size and population of crystals, which dominate the copolymer morphologies, are observed to increase with increasing aging time. Real-space results are correlated with small- and wide-angle X-ray scattering to elucidate the concurrent roles of endblock crystallization and self-assembly of these unique TPEs in solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Improving the Recyclability of Polymer Composites With Cellulose Nanofibrils

Cellulose nanofibers (CNFs) have been widely studied for their reinforcing potential in high-performance composites. While there are numerous publications on CNF-reinforced composites in a variety of polymer matrices, few have considered the recyclability of such thermoplastic composites and whether the incorporation of CNFs deteriorates or improves their performance upon reprocessing. In this study, two thermoplastic resins, poly(lactic acid) (PLA), and glycol-modified polyethylene terephthalate (PETg), were prepared with CNF reinforcement and thermomechanically recycled to investigate the effect of CNF inclusion on the composite properties after reprocessing as well as their effect on the composites’ number of useful life cycles. Additionally, changes in mechanical, thermal, rheological, molecular, and microstructural properties of the composites and/or base resins were monitored as a function of cycle numbers. As is typical, the polymers’ molecular weight and mechanical performance deteriorated with continued processing. However, the addition of spray dried CNF was found to better maintain the mechanical performance of both polymers throughout multiple recycling steps as compared to neat samples. For example, the tensile strength of PETg with 20 wt% CNF after 6 processing cycles was found to exceed that of virgin neat PETg, and higher loadings of CNF were found to preserve a higher yield strength during multiple rounds of reprocessing compared to PETg composites with lower CNF loadings. Ultimately this study indicates that the addition of CNF to some thermoplastic materials can increase both their sustainability by offsetting the use of high-embodied energy resins and their circularity by enabling performance retention over more use cycles.

42 ENGINEERING↗

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 OSTI2021

PEKK-10pct mica content unheated

CT data on PEKK with 10pct mica unheated sample

36 MATERIALS SCIENCE↗

NASA NTRS1993

The effects of stress and physical aging on the creep compliance of a polymeric composite

An experimental study was performed to determine the effects of stress and physical aging on the matrix dominated viscoelastic properties of IM7/8320, a high temperature fiber reinforced thermoplastic composite. Established creep/aging test techniques developed for polymers were adapted for testing of the composite material. The transverse and shear compliance for an orthotropic plate were found from creep compliance measurements at constant, sub-Tg temperatures. These compliance terms were shown to be effected by physical aging. Aging time shift factors and shift rates were found to be a function of applied stress.

Gates, Thomas E.↗