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NASA NTRS2005

High-Performance Polymers Having Low Melt Viscosities

High-performance polymers that have improved processing characteristics, and a method of making them, have been invented. One of the improved characteristics is low (relative to corresponding prior polymers) melt viscosities at given temperatures. This characteristic makes it possible to utilize such processes as resin-transfer molding and resin-film infusion and to perform autoclave processing at lower temperatures and/or pressures. Another improved characteristic is larger processing windows that is, longer times at low viscosities. Other improved characteristics include increased solubility of uncured polymer precursors that contain reactive groups, greater densities of cross-links in cured polymers, improved mechanical properties of the cured polymers, and greater resistance of the cured polymers to chemical attack. The invention is particularly applicable to poly(arylene ether)s [PAEs] and polyimides [PIs] that are useful as adhesives, matrices of composite materials, moldings, films, and coatings. PAEs and PIs synthesized according to the invention comprise mixtures of branched, linear, and star-shaped molecules. The monomers of these polymers can be capped with either reactive end groups to obtain thermosets or nonreactive end groups to obtain thermoplastics. The synthesis of a polymeric mixture according to the invention involves the use of a small amount of a trifunctional monomer. In the case of a PAE, the trifunctional monomer is a trihydroxy- containing compound for example, 1,3,5-trihydroxybenzene (THB). In the case of a PI, the trifunctional monomer is a triamine for example, triamino pyrimidine or melamine. In addition to the aforementioned trifunctional monomer, one uses the difunctional monomers of the conventional formulation of the polymer in question (see figure). In cases of nonreactive end caps, the polymeric mixtures of the invention have melt viscosities and melting temperatures lower than those of the corresponding linear polymers of equal molecular weights. The lower melting temperatures and melt viscosities provide larger processing windows. In cases of reactive end caps, the polymeric mixtures of the invention have lower melt viscosities before curing and the higher cross-link densities after curing (where branching in the uncured systems would become cross-links in the cured systems), relative to the corresponding linear polymers of equal molecular weights. The greater cross-link densities afford increased resistance to chemical attack and improved mechanical properties.

Jensen, Brian J.↗

DOE OSTI2020

Printing polymer blends through in situ active mixing during fused filament fabrication

Fused filament fabrication (FFF) enables production of 3D objects over a range of material compositions at low-cost relative to traditional manufacturing approaches. To date, a limited but growing number of materials are able to be used with FFF, however many applications exist where specific mechanical, thermal, or chemical properties are needed that cannot currently be met with the available feedstock selection. Therefore, a need exists to tune these materials for specific chemical or mechanical properties. One common formulation strategy to address these demanding design parameters is to develop composites or polymer blend filaments. Typically, this is a time-consuming and costly optimization process. Here, we have developed hardware for reproducibly mixing two filaments of similar or dissimilar compositions at the time of printing within individual printed layers. This mixing occurs via software-controlled rotating hardware in the chamber of an extruder’s hot-end. The efficiency of mixing within the printed layers has been characterized in detail as a function of the rotational speed and geometry of the blending hardware. These parameters were exploited to program the ratio and distribution of thermoplastic-based filaments blended within printed extrudate. Example printed specimens were produced with thermoplastic polyurethane (TPU) elastomer blended with rigid polylactic acid (PLA) and Nylon blended with PLA. In addition, a conductive carbon nanotube (CNT)-PLA composite was blended as a function of mixer geometry and input feed ratios with non-conductive PLA and resistance values were measured across the resulting printed specimens.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Matrix resin development at NASA Langley Research Center

The polymer program at NASA Langley Research Center involves exploratory studies in polymer science. These include the synthesis of novel polymers and their characterization. Polymer synthesis programs involve the development of novel thermoplastics, pseudothermoplastics, and thermosets. Recent investigations have led to the development of more easily processable polyimides, solvent-resistant polysulfones and polyphenylquinoxalines, and tougher high and intermediate-temperature polymers. Characterization efforts have 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 has been studied by rheology, mechanical behavior, separation techniques and spectroscopy. Some of these programs have involved the degradation 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.

St.clair, T. L.↗

DOE OSTI2022

Characterization of anisotropic mechanical properties of polymer composites from a hybrid additive manufacturing-compression molding process using x-ray computer tomography

In this study, anisotropic stiffness tensors were reconstructed based on fiber orientation distributions obtained from X-ray computer tomography (xCT). A preform was manufactured via a big area additive manufacturing (BAAM) system with carbon fiber (CF) filled acrylonitrile butadiene styrene (ABS). The tailored preform from additive manufacturing (AM) was used in the compression molding (CM) process to produce a low-void high-performance thermoplastic composite panel. An xCT technique was employed to detect the fiber orientations in CF/ABS composites manufactured via three different methods: AM from BAAM, extrusion compression molding (ECM), and AM-CM. The anisotropic stiffness tensor was obtained from the composite panel manufactured via the three manufacturing methods (AM, ECM, and AMCM). A micromechanics theory was used to obtain the orthotropic stiffness tensors of the composite panels and compared with the experimental values. The predicted stiffness tensors of AM and AM-CM composite panels were used to study the deformation characteristics of a steering wheel during airbag deployment by performing finite element analysis (FEA). The approach developed in this study can be utilized for evaluating high-performance composites.

Pokkalla, Deepak↗

DOE OSTI2021

Mica filled polyetherketoneketones for material extrusion 3D printing

Polyetherketoneketone (PEKK) has superior physical properties to most available thermoplastics compatible with material extrusion-based 3D printing, including analogs in the polyaryletherketone (PAEK) family. To date, the performance of fused filament fabrication (FFF) compatible PEKK has been detailed primarily as a function of varying the isomer ratios composing the co-polymer structure. The strategy to form blends or composites with PEKK for FFF is attractive for further tailoring of performance in application, yet has received limited attention. Here, we report the integration of three grades of mica platelets into PEKK at 10% and 30% mass loadings to generate an array of filament feedstocks that were then used to print objects with a simple FFF machine. The effects of mica coating chemistry and surface treatment on the compatibility with PEKK and resulting properties are described. Mica fillers at both loadings have only subtle influence on the FFF relevant melt rheological properties inherent to PEKK. Pigment micas at high loadings can lower the melting temperature of PEKK (up to 19 ºC) without shifting its glass transition temperature and inhibit much of the undesirable crystallization occurring during processing with unfilled PEKK. The printed composites were effectively cold crystallized post-printing, affording crystalline fractions up to 90% relative to unfilled PEKK with increased dimensional stabilities. All micas, when used as fillers in low and high relative PEKK crystallinities, significantly increased the tensile modulus (as high as 126% or to 7.31 GPa) of parts in correlation to the loading. Furthermore, the underlying microstructural features of a printed composite were compared to unfilled PEKK by use of a high-resolution helical micro-computed tomography instrument. Practically, pigment micas can confer a wide range of rich colors to 3D-printed PEKK.

36 MATERIALS SCIENCE↗

NASA NTRS1992

New materials drive high-performance aircraft

This report shows how advanced composite materials and new processing methods are enabling lighter, lower cost aircraft structures. High-temperature polymers research will focus on systems capable of 50,000 to 100,000 hours of operation in the 212-400 F temperature range. Prospective materials being evaluated include high-temperature epoxies, toughened bismaleimides, cyanates, thermoplastics, polyimides and other polymers.

Ruhmann, Douglas C.↗

NASA NTRS1984

Thermoplastic-carbon fiber hybrid yarn

Efforts were directed to develop processing methods to make carbon fiber/thermoplastic fiber preforms that are easy to handle and drapeable, and to consolidate them into low void content laminates. The objectives were attained with the development of the hybrid yarn concept; whereby, thermoplastic fiber can be intimately intermixed with carbon fiber into a hybrid yarn. This was demonstrated with the intermixing of Celion 3000 with a Celanese liquid crystal polymer fiber, polybutylene terepthalate fiber, or polyetheretherketone fiber. The intermixing of the thermoplastic matrix fiber and the reinforcing carbon fiber gives a preform that can be easily fabricated into laminates with low void content. Mechanical properties of the laminates were not optimized; however, initial results indicated properties typical of a thermoplastic/carbon fiber composites prepared by more conventional methods.

Ketterer, M. E.↗

NASA NTRS1994

Tough, processable semi-interpenetrating polymer networks from monomer reactants

A high temperature semi-interpenetrating polymer network (semi-IPN) was developed which had significantly improved processability, damage tolerance, and mechanical performance, when compared to the commercial Thermid materials. This simultaneous semi-IPN was prepared by mixing the monomer precursors of Thermid AL-600 (a thermoset) and NR-150B2 (a thermoplastic) and allowing the monomers to react randomly upon heating. This reaction occurs at a rate which decreases the flow and broadens the processing window. Upon heating at a higher temperature, there is an increase in flow. Because of the improved flow properties, broadened processing window and enhanced toughness, high strength polymer matrix composites, adhesives and molded articles can now be prepared from the acetylene end-capped polyimides which were previously inherently brittle and difficult to process.

Pater, Ruth H.↗

NASA NTRS1994

Chemical recycling of scrap composites

There are no well-developed technologies for recycling composite materials other than grinding to produce fillers. New approaches are needed to reclaim these valuable resources. Chemical or tertiary recycling, conversion of polymers into low molecular weight hydrocarbons for reuse as chemicals or fuels, is emerging as the most practical means for obtaining value from waste plastics and composites. Adherent Technologies is exploring a low-temperature catalytic process for recycling plastics and composites. Laboratory results show that all types of plastics, thermosets as well as thermoplastics, can be converted in high yields to valuable hydrocarbon products. This novel catalytic process runs at 200 C, conversion times are rapid, the process is closed and, thus, nonpolluting, and no highly toxic gas or liquid products have been observed so no negative environmental impact will result from its implementation. Tests on reclamation of composite materials show that epoxy, imide, and engineering thermoplastic matrices can be converted to low molecular weight hydrocarbons leaving behind the reinforcing fibers for reuse as composite reinforcements in secondary, lower-performance applications. Chemical recycling is also a means to dispose of sensitive or classified organic materials without incineration and provides a means to eliminate or reduce mixed hazardous wastes containing organic materials.

Allred, Ronald E.↗

NASA NTRS2000

A Damage Resistance Comparison Between Candidate Polymer Matrix Composite Feedline Materials

As part of NASAs focused technology programs for future reusable launch vehicles, a task is underway to study the feasibility of using the polymer matrix composite feedlines instead of metal ones on propulsion systems. This is desirable to reduce weight and manufacturing costs. The task consists of comparing several prototype composite feedlines made by various methods. These methods are electron-beam curing, standard hand lay-up and autoclave cure, solvent assisted resin transfer molding, and thermoplastic tape laying. One of the critical technology drivers for composite components is resistance to foreign objects damage. This paper presents results of an experimental study of the damage resistance of the candidate materials that the prototype feedlines are manufactured from. The materials examined all have a 5-harness weave of IM7 as the fiber constituent (except for the thermoplastic, which is unidirectional tape laid up in a bidirectional configuration). The resin tested were 977-6, PR 520, SE-SA-1, RS-E3 (e-beam curable), Cycom 823 and PEEK. The results showed that the 977-6 and PEEK were the most damage resistant in all tested cases.

Nettles, A. T↗

NASA NTRS2000

Dry Ribbon for Heated Head Automated Fiber Placement

Ply-by-ply in situ processes involving automated heated head deposition are being developed for fabrication of high performance, high temperature composite structures from low volatile content polymer matrices. This technology requires (1) dry carbon fiber towpreg, (2) consolidation of towpreg to quality, placement-grade unidirectional ribbon or tape, and (3) rapid, in situ, accurate, ply-by-ply robotic placement and consolidation of this material to fabricate a composite structure. In this study, the physical properties of a candidate thermoplastic ribbon, PIXA/IM7, were evaluated and screened for suitability in robotic placement. Specifically, towpreg was prepared from PIXA powder. Various conditions (temperatures) were used to convert the powder-coated towpreg to ribbons with varying degrees of processability. Ribbon within preset specifications was fabricated at 3 temperatures: 390, 400 and 410 C. Ribbon was also produced out-of-spec by purposely overheating the material to a processing temperature of 450 C. Automated placement equipment at Cincinnati Milacron and NASA Langley was used to fabricate laminates from these experimental ribbons. Ribbons were placed at 405 and 450 C by both sets of equipment. Double cantilever beam and wedge peel tests were used to determine the quality of the laminates and, especially, the interlaminar bond formed during the placement process. Ribbon made under conditions expected to be non-optimal (overheated) resulted in poor placeability and composites with weak interlaminar bond strengths, regardless of placement conditions. Ribbon made under conditions expected to be ideal showed good processability and produced well-consolidated laminates. Results were consistent from machine to machine and demonstrated the importance of ribbon quality in heated-head placement of dry material forms. Preliminary screening criteria for the development and evaluation of ribbon from new matrix materials were validated.

Hulcher, A. Bruce↗

NASA NTRS1997

Automated Fabrication of High Performance Composites: An Overview of Research at the Langley Research Center

Automated heated placement of consolidated fiber reinforced polymer ribbon/tape is a rapid, cost effective technique for net shape fabrication of high performance composites. Several research efforts in the United States are developing the heated head robotic hardware and associated software needed to bring this technology into widespread use for building aircraft parts. These efforts emphasize the use of pre-consolidated thermoplastic ribbon or tape which is thermally welded on-the-fly . The approach provides in-situ consolidation and obviates the need for autoclave processing and massive debulking, thereby reducing costs. Addressed in this paper are some key issues being pursued at NASA Langley related to this technology. These include: (a) preparation of high quality intermediate materials forms such as thermoplastic powders, powder-coated towpreg and consolidated ribbon/tape and (b) achievement of precise control of the following: robot head positioning on the tool; material placement; heat delivery to the lay-down zone; and cut/add, start/stop capability. Heated head development has dealt with the use of hot gases alone and in combination with focused infrared radiation as heat sources.

Johnston, N. J.↗

DOE OSTI2025

Simulation-driven design optimization of reaction injection molding (RIM) process for polydicyclopentadiene (pDCPD): Minimizing cycle time, defects, and warpage

Replacing metal components in trucks, trailers, and buses with lightweight polymer composites is challenging due to high temperatures and complex manufacturing. The Reaction Injection Molding (RIM) process using Dicyclopentadiene (DCPD) resin offers a solution by producing robust parts with excellent stiffness, impact strength, and resistance properties. Simulations are essential for optimizing this process, predicting defects, and improving quality. However, most commercial software is tailored for thermoplastics, requiring thermoset users to generate their own datasets. In this study, a material data card for DCPD was developed to perform RIM simulations. Design of Experiments (DOE) was used to identify key factors affecting filling, curing, and warpage, aiming to minimize cycle time and defects. The simulations explored varying injection gate parameters (size, location, number) and process conditions (mold/resin temperature, injection/curing pressure). Results showed that gate design significantly impacts filling behavior and defects. A single central gate provided balanced flow with fewer defects, while two corner gates led to more defects. Additionally, lower injection pressure increased filling time, while higher mold temperature accelerated curing but led to more warpage. In conclusion, this optimization framework aims to enhance DCPD part performance and promote sustainable manufacturing by reducing waste and energy consumption.

42 ENGINEERING↗

DOE OSTI2025

Enabling Next Generation Reaction Injection Molding (RIM) for Lightweight Structures

Replacing metal components in trucks, trailers, and buses with lightweight polymer composites is challenging due to high temperatures and complex manufacturing. The Reaction Injection Molding (RIM) process using Dicyclopentadiene (DCPD) resin offers a solution by producing robust parts with excellent stiffness, impact strength, and resistance properties. Simulations are essential for optimizing this process, predicting defects, and improving quality. However, most commercial software is tailored for thermoplastics, requiring thermoset users to generate their own datasets. In this project, a material data card for DCPD was developed to perform RIM simulations. Design of Experiments (DOE) was used to identify key factors affecting filling, curing, and warpage, aiming to minimize cycle time and defects. The simulations explored varying injection gate parameters (size, location, number) and process conditions (mold/resin temperature, injection/curing pressure). Results showed that gate design significantly impacts filling behavior and defects. A single central gate provided balanced flow with fewer defects, while two corner gates led to more defects. Additionally, lower injection pressure increased filling time, while higher mold temperature accelerated curing but led to more warpage. This optimization framework aims to enhance DCPD part performance and promote sustainable manufacturing by reducing waste and energy consumption. This research has been performed in collaborations with McClarin Composites. The research outcome has been submitted to the Journal of Manufacturing Processes.

36 MATERIALS SCIENCE↗

NASA NTRS1994

Tough, processable simultaneous semi-interpenetrating polyimides

A high temperature semi-interpenetrating polymer network (semi-IPN) was developed which had significantly improved processability, damage tolerance, and mechanical performance when compared to the commercial Thermid materials. This simultaneous semi-IPN was prepared by mixing a thermosetting polyimide with a thermoplastic monomer precursor solution (NR150B2) and allowing them to react upon heating. This reaction occurs at a rate which decreases the flow and broadens the processing window. Upon heating at a higher temperature, there is an increase in flow. Because of the improved flow properties, broadened processing window and enhanced toughness, high strength polymer matrix composites, adhesives and molded articles can now be prepared from the acetylene endcapped polyimides which were previously inherently brittle and difficult to process.

Pater, Ruth H.↗

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↗

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↗

NASA NTRS1996

Tough, processable simultaneous semi-interpenetrating polyimides

A high temperature semi-interpenetrating polymer network (semi-IPN) was developed which had significantly improved processability, damage tolerance and mechanical performance, when compared to the commercial Thermid.RTM. materials. This simultaneous semi-IPN was prepared by mixing a thermosetting polyimide with a thermoplastic monomer precursor solution (NR-15082) and allowing them to react upon heating. This reaction occurs at a rate which decreases the flow and broadens the processing window. Upon heating at a higher temperature, there is an increase in flow. Because of the improved flow properties, broadened processing window and enhanced toughness, high strength polymer matrix composites, adhesives and molded articles can now be prepared from the acetylene endcapped polyimides which were previously inherently brittle and difficult to process.

Pater, Ruth H.↗