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DOE OSTI2023

Strategy for Nonenzymatic Harvesting of Cells via Decoupling of Adhesive and Disjoining Domains of Nanostructured Stimulus-Responsive Polymer Films

The nanostructured polymer film introduces a novel mechanism of nonenzymatic cell harvesting by decoupling solid cell-adhesive and soft stimulus-responsive cell-disjoining areas on the surface. The key characteristics of this architecture are the decoupling of adhesion from detachment and the impermeability to the integrin protein complex of the adhesive domains. This surface design eliminates inherent limitations of thermoresponsive coatings, namely, the necessity for the precise thickness of the coating, grafting or cross-linking density, and material of the basal substrate. The concept is demonstrated with nanostructured thermoresponsive films made of cell-adhesive epoxy photoresist domains and cell-disjoining poly(N-isopropylacrylamide) brush domains.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1985

Increasing Fire Safety of Epoxies

Epoxy with increased resistance to fire made by reacting any of three commercial epoxide monomers with curing agent consisting of mixture of isomers called "DCEPD". Curing agent incorporates phosphorus and chlorine directly into crosslinking part of polymer. DCEPD produced by nitrating precursor phosphonylmethyl benzene, then reducing resulting isomeric mixture of dinitro compounds.

Kourtides, D. A.↗

DOE OSTI2021

Consortium for Production of Affordable Carbon Fibers in the United States (Final Report)

Various feedstocks from coal, petroleum and bio-based acrylonitrile were investigated for their ability to produce carbon fiber within DOE strength (250 ksi), modulus (25 Msi), elongation (>1%) and cost (≤$5/lb) goals for wider utilization in light-weight vehicles for the automotive industry. The overarching approach was to chemically identify and map the various feedstocks, understand the molecular transformation to produce carbon fiber precursors (mesophase for pitch materials of polyacrylonitrile polymer) and how these impact carbon fiber quality. Predictive models were built to relate the feedstocks and precursors to carbon fiber properties using atomistic and micro-scale modeling within ±15%. Using tow-level carbon fiber epoxy composites, carbon fibers tow-level predictions of elastic components of the carbon fibers were also successfully modeled within ±15%, using finite element analysis to confirm single filament carbon fiber properties. These models were validated with tow-level epoxy composite experiments from carbon fibers produced in this study.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2023

Fluorescent aggregate structure revealed in bisphenol F epoxy thermoset

Bisphenol F (BPF) epoxy resin is a prepolymer component of thermosets used in construction of reinforced carbon fiber composites (RCFC). The fluorescence of this resin can provide information about chemical and structural alterations of the thermoset from thermal or mechanical damage. While some work has investigated the fluorescence spectra of bisphenol A epoxy resin, a structural analog of BPF, none have studied BPF. The purpose of this study is to investigate the baseline fluorescence spectra of the BPF epoxy resin for features that could be utilized for monitoring damage and structural alterations. Bisphenol F epoxy resin was found to have two emission peaks with a broad peak centered at 410 nm and a sharp peak centered at 550 nm. The broad emission peak was identified as the fluorescence from BPF epoxy monomer while the sharp emission peak was found to be from an aggregate structure present in the epoxy resin. It is hypothesized that this structure is an H-aggregate based on the emission features and structural stability of the aggregate compared to the alternative J-aggregate which was determined via density functional theory calculations. The H-aggregate was found to persist into one of the cured thermoset formulations evaluated but was lost when exposed to elevated temperatures below thermal degradation of the thermoset. This loss of aggregate structure was due to polymer network rearrangement. This new fluorescence signature can be used as an indicator of polymer network rearrangement from thermal exposure which may alter the expected material performance and precede thermal degradation.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Carbon Additive Manufacturing with a Near-Replica “Green-to-Brown” Transformation

Nanocomposites containing nanoscale materials offer exciting opportunities to encode nanoscale features into macroscale dimensions, which produces unprecedented impact in material design and application. However, conventional methods cannot process nanocomposites with a high particle loading, as well as nanocomposites with the ability to be tailored at multiple scales. A composite architected mesoscale process strategy that brings particle loading nanoscale materials combined with multiscale features including nanoscale manipulation, mesoscale architecture, and macroscale formation to create spatially programmed nanocomposites with high particle loading and multiscale tailorability is reported. The process features a low-shrinking (<10%) “green-to-brown” transformation, making a near-geometric replica of the 3D design to produce a “brown” part with full nanomaterials to allow further matrix infill. Here, this demonstration includes additively manufactured carbon nanocomposites containing carbon nanotubes (CNTs) and thermoset epoxy, leading to multiscale CNTs tailorability, performance improvement, and 3D complex geometry feasibility. The process can produce nanomaterial-assembled architectures with 3D geometry and multiscale features and can incorporate a wide range of matrix materials, such as polymers, metals, and ceramics, to fabricate nanocomposites for new device structures and applications.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Closed‐Loop Recyclable Vitrimer Plastics from PET Waste: A Design for Circularity

Plastics are essential to modern society, but their low recycling rates and inefficient end-of-life management pose a significant environmental challenge. Herein, the efficient strategy for upcycling postconsumer poly(ethylene terephthalate) (PET) waste into robust, closed-loop recyclable vitrimer plastics and composites is presented to address this issue. The catalyst-free aminolysis utilizes readily available amines to deconstruct diverse PET wastes into macromonomers, which are upcycled into vitrimers, exhibiting superior mechanical properties and exceeding the ultimate tensile stress and Young's Modulus of virgin PET by 80% and 150% respectively. These vitrimers exhibit excellent healability, shape memory, thermal reprocessability, and closed-loop chemical recyclability, enabling quantitative macromonomer recovery even from mixed plastic waste streams and glass/carbon fiber reinforced vitrimer (G/CFRV) composites. Furthermore, the vitrimer resin yields robust GFRV and CFRV composites with tensile strengths exceeding those of traditional epoxy composites by 100% and 80%, respectively, while maintaining complete chemical recyclability of both constituent materials. A preliminary technoeconomic analysis confirms the costeffectiveness and competitiveness of the facile PET deconstruction approach, which is potentially adaptable to other condensation polymers. Further, this study presents a facile approach to upcycling plastic waste into circular plastics and composites, offering a sustainable solution to global plastic waste management and fostering a circular economy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1987

Interfacial adhesion of carbon fibers

Relative adhesion strengths between AS4, AS1, and XAS carbon fibers and thermoplastic polymers were determined using the embedded single filament test. Polymers studied included polycarbonate, polyphenylene oxide, polyetherimide, polysulfone, polyphenylene oxide blends with polystyrene, and polycarbonate blends with a polycarbonate polysiloxane block copolymer. Fiber surface treatments and sizings improved adhesion somewhat, but adhesion remained well below levels obtained with epoxy matrices. An explanation for the differences between the Hercules and Grafil fibers was sought using X ray photon spectroscopy, wetting, scanning electron microscopy and thermal desorption analysis.

Bascom, Willard D.↗

DOE OSTI2022

Diamond formation in double-shocked epoxy to 150 GPa

We present measurements of diamond formation in doubly shocked Stycast 1266 epoxy (comprising C, H, Cl, N, and O) using in situ x-ray diffraction. Epoxy samples were reshocked against a LiF window to pressures between 80 and 148 GPa in experiments at the Omega Laser Facility. Furthermore, the pressure and temperature conditions were diagnosed in situ using velocimetry and optical pyrometry, respectively. X-ray diffraction patterns of the compressed epoxy are consistent with cubic diamond (Fd3¯m), indicating that diamond can precipitate not only from twice-shocked CH polystyrene [Kraus et al. Nat. Astron. 1, 606 (2017)] at these conditions but also from twice-shocked CH polymers with the addition of oxygen, nitrogen, and chlorine. These results, in combination with previous works on CH, CH 2 , CH 4 , and methane hydrate, support that diamond often, but not always, forms from CH-based compounds at extreme pressures and temperatures, indicating that the chemical composition, thermodynamic compression path, and kinetics play an important role.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effect of the Segmental Structure of Thermoplastic Polyurethane (Hardness) on the Interfacial Adhesion of Textile-Grade Carbon Fiber Composites

In polymer composites, the fiber–matrix interface is primarily influenced by the surface treatment of the fibers and polymer morphology. Previous studies have investigated the effect of surface treatment of carbon fiber on the mechanical properties of the resulting composites. However, very few studies have explored the chemical structural modification of polymer effect on the fiber–matrix adhesion. In this work, the interfaces of soft thermoplastic polyurethane (S-TPU) and hard-segmented TPU (H-TPU) were investigated through surface, thermal, and mechanical characterization. A textile-grade carbon fiber (TCF) with 1% concentration of epoxy sizing (an emerging material for nonaerospace applications with 450 K filament tows) was used as a reinforcement to investigate the structure–property relationship at the interface. Atomic force microscopy results showed 39% higher surface roughness for S-TPU than for H-TPU. X-ray photoelectron spectroscopy results revealed a 550% increase in C=O content, which can provide multiple hydrogen bonding networks in H-TPU, and these C=O bonds can produce a strong chemical bond at the fiber–matrix interface. Additionally, dynamic mechanical analysis and differential scanning calorimetry results confirmed the presence of hydrogen bonding that enhances the cross-linked density by 232% in H-TPU compared to S-TPU. The improved mechanical properties of H-TPU composites, such as flexural, impact and tensile by 30, 50, and 130% compared to S-TPU composites, prove that the crystallinity and hydrogen bonding significantly increase the load bearing capacity due to the strong interface. The mechanical properties of TCF–TPU composites validate the formation of chemical bonds through a nucleophilic addition reaction at the interface and improve the bond strength of the composites. Thus, tailoring the polyurethane structure broadens the performance of segmented TPU in conjunction with TCF reinforcement, which has implications for cost-effective, high-strength composites.

36 MATERIALS SCIENCE↗

NASA NTRS1984

Status and New Directions for Solid Lubricant Coatings and Composite Materials

At one time, solid lubricants were used almost entirely in aerospace applications. Today there is a pronounced trend to use them over a much broader range of applications. For example, self-lubricating polymer-based composites have displaced traditional oil-lubricated, metallic composites for many journal bearings and thrust, washers in applications as diverse as earthmoving machinery and snow blowers to aircraft applications. For moderate temperatures below 200° C, glass filament-wound epoxy bearings with PTFE lubricating liners are useful; for temperatures up to 350° C, graphite fiber reinforced polyimide bearing materials are finding applications. Molybdenum disulfide, graphite, and PTFE are the most widely known and used solid lubricants, and there is increasing interest in the relatively new solid lubricant graphite fluoride. Advanced technology engines such as the adiabatic diesel and the small, efficient gas turbine have severe lubrication and wear problems at temperatures beyond the capabilities of any of these lubricants. Here, self-lubricating ceramics and inorganic composites for use at I000° C or higher are of interest. However, perhaps the most significant new direction for solid lubricant coatings and self-lubricating composites is their steadily increasing use in dry bearings for large volume, moderate temperature applications. This can be attributed to their simplicity of use (no supporting lubricant system needed), light weight, convenience, and general cost effectiveness.

Harold E Sliney↗

DOE OSTI2024

Designing a Dynamic Material via Interlocking Kraft Lignin with Ultrahigh Molecular Weight Poly(ethylene oxide)

The environmental issues stemming from plastic waste and the excessive use of petroleum-based chemicals are both concerning and urgent. To effectively address this problem, we need to adopt a comprehensive approach involving developing more sustainable and renewable materials. These materials should be capable of demonstrating similar or even better performance than functional polymers synthesized from petroleum-based chemicals. Our research aims to develop more sustainable materials by leveraging the intrinsic characteristics of a natural polymer, lignin, a byproduct of the biorefinery industries. We utilized the three-dimensional branching structure of lignin as a material framework. We employed an approach to co-reactive melt processing of kraft lignin with aliphatic flexible chains of soft cross-linkers through the reaction of the cross-linker epoxy chain ends with lignin functional groups. Our study demonstrates that the interlocked structure formed from the co-blending of kraft lignin with ultrahigh molecular weight poly(ethylene oxide) and the cross-linking of lignin chains through a solvent-free process can manipulate the macromolecular interactions and relaxation. This manipulation results in materials that exhibit a wide range of thermomechanical properties and self-healing and shape memory effects, with drastically improved stiffness in a single material. We have explored the fundamental understanding of the macromolecular chain relaxation dynamics originating from the interlocking structure formation. In conclusion, this investigation utilized various techniques, including thermal, mechanical, rheology, and quasi-elastic neutron scattering.

36 MATERIALS SCIENCE↗

NASA NTRS2019

Observations of Non-Spherical, Graphite-Epoxy Projectiles Impacting a Thermally-Insulated, Double-Wall Shield

The DebriSat hypervelocity impact experiment, performed at the Arnold Engineering Development Center (U.S.A.F. Arnold Air Force Base), is intended to update the catastrophic break-up models for modern satellites. To this end, the DebrisSat was built with many modern materials including structural panels of carbon-fiber, reinforced polymer (CFRP). Subsequent to the experiment, fragments of the DebrisSat have been extracted from porous, catcher panels used to gather the debris from the impact event. Thus far, one of the key observations from the collected fragments is that CFRP represents a large fraction of the fragments and that these fragments tend to be thin, flake-like structures or long, needle-like structures; whereas, debris with nearly equal dimensions is less prevalent. As current ballistic-limit models are all developed based upon spherical impacting particles, the experiment has pointed to a missing component in the current approach that must be considered. To begin to understand the implications of this observation, simulations like those shown in Fig. 1 have been performed using cylindrical structures at a representative orbital speed into an externally-insulated, double-wall shield that is representative of shielding of International-Space-Station-visiting vehicles. These simulations have been performed for normal impacts to the surface with three different angles-of-attack (AOA) to capture the effect on the shield performance. This paper documents the simulated shield and the models developed to study the effect of non-spherical fragments, as well as, derives the critical characteristics of CFRP impacting particles for the selected shield as shown in Fig. 2. To assist with the design of the updated debris models, this work summarizes the simulated results into a deployable form for evaluating the relative importance of fragment structures.

Miller, Joshua E.↗

DOE OSTI2022

ELASTOMERIC MICROVASCULAR SELF-HEALING MATERIALS

Damaged elastomeric diaphragms within pneumatic controllers used in the oil and gas industry lead to an unintended release of methane. Self-healing microvascular materials capable of healing various types of damage have been fabricated. These microvascular materials are designed to replace currently available commercial diaphragms found in pneumatic controllers and provide a solution to reduce unintended methane leaks. Poly(dimethylsiloxane) (PDMS) was used as the main matrix material, with additional testing conducted on polyurethane and flexibilised epoxy materials. Microvascular networks were implemented into the elastomeric membranes to act as ves- sels to deliver healing agents to the damaged areas. The complex, interdigitated channel networks were created using a 3D printed custom compounded filament composed of polylactic acid (PLA) and tin(II) oxalate. Two-part liquid casting polymers were poured around the channels into a mould to create samples with the scaffolding of the microvascular channels intact. Hollow microvascular networks were created by placing the samples within a vacuum oven at 250◦C which causes the thermal depolymerisation of PLA into its gaseous monomers. The manufactured materials were placed in test stands and pressurized using nitrogen gas to determine their healing and mechanical behaviour. Self-healing behaviour was demonstrated using PDMS matrix materials and healing chemistries within a pressure test cell. This test cell was designed to detect any damage to a sample by record- ing an outlet pressure. Damages including puncture holes, diagonal cuts and star-shaped central iv cuts were applied to the samples and a reduction in the outlet pressure was recorded for all sam- ples. A variation in channel spacing and diameter was studied to determine the optimal design of the microvascular network for self-healing performance. The mechanical performance of elastomeric membrane materials within a diaphragmatic pressurised stand was observed. Deformations and strains around the channels and channel inter- sections at the midplane of the materials were recorded using digital image correlation. Normal stresses were calculated using Hooke’s law and the material properties of the PDMS matrix. A reduction in leak rate, implying the success of self-healing, was recorded within manu- factured diaphragm samples tested within a commercial valve. PDMS is the favourable material when compared to polyurethane and flexibilised epoxy for creating

03 NATURAL GAS↗

NASA NTRS1990

Ethynyl-Terminated Imidothioethers And Derived Resins

New toughened epoxies exhibit excellent properties, but temperatures at which used limited. Bismaleimide resins some of base materials being formulated to develop materials used at moderate temperatures. Work conducted on use of acetylenic (ethynyl) group to cross-link and extend chains of oligomers and polymers to obtain materials that perform at high temperatures. Work extended to ethynyl-terminated imidothioethers (ETI's). Tested primarily as adhesives and composite matrices and found to have useful properties in terms of processing, resistance to high temperature, fracture toughness, and resistance to solvents. Also have desirable mechanical properties. Potentially useful for aerospace and nonaerospace applications.

Hergenrother, Paul M.↗

NASA NTRS1981

Hybridized polymer matrix composite

Under certain conditions of combined fire and impact, graphite fibers are released to the atmosphere by graphite fiber composites. The retention of graphite fibers in these situations is investigated. Hybrid combinations of graphite tape and cloth, glass cloth, and resin additives are studied with resin systems. Polyimide resins form the most resistant composites and resins based on simple novolac epoxies the least resistant of those tested. Great improvement in the containment of the fibers is obtained in using graphite/glass hybrids, and nearly complete prevention of individual fiber release is made possible by the use of resin additives.

Stern, B. A.↗

NASA NTRS2006

Micromechanics Modeling of Functionally Graded Interphase Regions in Carbon Nanotube-Polymer Composites

The effective elastic properties of a unidirectional carbon fiber/epoxy lamina in which the carbon fibers are coated with single-walled carbon nanotubes are modeled herein through the use of a multi-scale method involving the molecular dynamics/equivalent continuum and micromechanics methods. The specific lamina representative volume element studied consists of a carbon fiber surrounded by a region of epoxy containing a radially varying concentration of carbon nanotubes which is then embedded in the pure epoxy matrix. The variable concentration of carbon nanotubes surrounding the carbon fiber results in a functionally graded interphase region as the properties of the interphase region vary according to the carbon nanotube volume fraction. Molecular dynamics and equivalent continuum methods are used to assess the local effective properties of the carbon nanotube/epoxy comprising the interphase region. Micromechanics in the form of the Mori-Tanaka method are then applied to obtain the global effective properties of the graded interphase region wherein the carbon nanotubes are randomly oriented. Finally, the multi-layer composite cylinders micromechanics approach is used to obtain the effective lamina properties from the lamina representative volume element. It was found that even very small quantities of carbon nanotubes (0.36% of lamina by volume) coating the surface of the carbon fibers in the lamina can have a significant effect (8% increase) on the transverse properties of the lamina (E22, k23, G23 and G12) with almost no affect on the lamina properties in the fiber direction (E11 and v12).

Seidel, Gary D.↗

NASA NTRS2006

Clay Nanocomposite/Aerogel Sandwich Structures for Cryotanks

GRC research has led to the development of epoxy-clay nanocomposites with 60-70% lower gas permeability than the base epoxy resin. Filament wound carbon fiber reinforced tanks made with this nanocomposite had a five-fold lower helium leak rate than the corresponding tanks made without clay. More recent work has produced new composites with more than a 100-fold reduction in helium permeability. Use of these advanced, high barrier composites would eliminate the need for a liner in composite cryotanks, thereby simplifying construction and reducing propellant leakage. Aerogels are attractive materials for use as cryotank insulation because of their low density and low thermal conductivity. However, aerogels are fragile and have poor environmental stability, which have limited their use to certain applications in specialized environments (e.g., in certain types of nuclear reactors as Cerenkov radiation detectors, and as thermal insulators aboard space rovers on Mars). New GRC developed polymer crosslinked aerogels (X-Aerogels) retain the low density of conventional aerogels, but they demonstrate a 300-fold increase in their mechanical strength. Currently, our strongest materials combine a density of approx. 0.45 g/cc, a thermal conductivity of approx. 0.04 W/mK and a compressive strength of ~185 MPa. Use of these novel aerogels as insulation materials/structural components in combination with the low permeability of epoxy-clay nanocomposites could significantly reduce cryotank weight and improve durability.

Miller, Sandi↗

NASA NTRS1993

Thermal stress analysis of composites in the space environment

A finite element micromechanics approach was utilized to investigate the thermally induced stress fields in continuous fiber reinforced polymer matrix composites at temperatures typical of spacecraft operating environments. The influence of laminate orientation was investigated with a simple global/local formulation. Thermal stress calculations were used to predict probable damage initiation locations, and the results were compared to experimentally observed damage in several epoxy matrix composites. The influence of an interphase region on the interfacial stress states was investigated.

Bowles, David E.↗