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At least 343 records · Page 19

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NASA NTRS1987

The effect of bromination of carbon fibers on the coefficient of thermal expansion of graphite fiber-epoxy composites

To examine the effect of bromination of carbon fibers on the coefficient of thermal expansion (CTE) of carbon fiber epoxy composites, several pristine and brominated carbon fiber-epoxy composite samples were subjected to thermomechanical analysis. The CTE's of these samples were measured in the uniaxial and transverse directions. The CTE was dominated by the fibers in the uniaxial direction, while it was dominated by the matrix in the transverse directions. Bromination had no effect on the CTE of any of the composites. In addition, the CTE of fiber tow was measured in the absence of a polymer matrix, using an extension probe. The results from this technique were inconclusive.

Jaworske, D. A.↗

NASA NTRS1994

The effect of Low Earth Orbit exposure on some experimental fluorine and silicon-containing polymers

Several experimental fluorine and silicon-containing polymers in film form were exposed to low Earth orbit (LEO) on a Space Shuttle flight experiment (STS-46, Evaluation of Oxygen Interaction with Materials, EOIM-3). The environmental parameters of primary concern were atomic oxygen (AO) and ultraviolet (UV) radiation. The materials were exposed to 2.3 plus or minus 0.1 x 10(exp 20) oxygen atoms/sq cm and 30.6 UV sun hours during the flight. In some cases, the samples were exposed at ambient, 120 C and 200 C. The effects of exposure on these materials were assessed utilizing a variety of characterization techniques including optical, scanning electron (SEM) and scanning tunneling (STM) microscopy, UV-visible (UV-VIS) transmission, diffuse reflectance infrared (DR-FTIR), x-ray photoelectron (XPS) spectroscopy, and in a few cases, gel permeation chromatography (GPC). In addition, weight losses of the films, presumably due to AO erosion, were measured. The fluorine-containing polymers exhibited significant AO erosion and exposed films were diffuse or 'frosted' in appearance and consequently displayed dramatic reductions in optical transmission. The silicon-containing films exhibited minimum AO erosion and the optical transmission of exposed films was essentially unchanged. The silicon near the exposed surface in the films was converted to silicate/silicon oxide upon AO exposure which subsequently provided protection for the underlying material. The silicon-containing epoxies are potentially useful as AO resistant coatings and matrix resins as they are readily processed into carbon fiber reinforced composites and cured via electron radiation.

Connell, John W.↗

NASA NTRS1979

Advanced thermoset resins for fire-resistant composites

The thermal and flammability properties of some thermoset polymers and composites are described. The processing and evaluation of composites fabricated from currently used resins and advanced fire-resistant resins are also described. Laboratory test methodology used to qualify candidate composite materials includes thermochemical characterization of the polymeric compounds and evaluation of the glass reinforced composites for flammability and smoke evolution. The use of these test methods will be discussed in comparing advanced laminating resins and composites consisting of modified epoxies, phenolics and bismaleimide, with conventional baseline materials consisting of epoxy.

Kourtides, D. A.↗

NASA NTRS2007

Protective Skins for Aerogel Monoliths

A method of imparting relatively hard protective outer skins to aerogel monoliths has been developed. Even more than aerogel beads, aerogel monoliths are attractive as thermal-insulation materials, but the commercial utilization of aerogel monoliths in thermal-insulation panels has been inhibited by their fragility and the consequent difficulty of handling them. Therefore, there is a need to afford sufficient protection to aerogel monoliths to facilitate handling, without compromising the attractive bulk properties (low density, high porosity, low thermal conductivity, high surface area, and low permittivity) of aerogel materials. The present method was devised to satisfy this need. The essence of the present method is to coat an aerogel monolith with an outer polymeric skin, by painting or spraying. Apparently, the reason spraying and painting were not attempted until now is that it is well known in the aerogel industry that aerogels collapse in contact with liquids. In the present method, one prevents such collapse through the proper choice of coating liquid and process conditions: In particular, one uses a viscous polymer precursor liquid and (a) carefully controls the amount of liquid applied and/or (b) causes the liquid to become cured to the desired hard polymeric layer rapidly enough that there is not sufficient time for the liquid to percolate into the aerogel bulk. The method has been demonstrated by use of isocyanates, which, upon exposure to atmospheric moisture, become cured to polyurethane/polyurea-type coats. The method has also been demonstrated by use of commercial epoxy resins. The method could also be implemented by use of a variety of other resins, including polyimide precursors (for forming high-temperature-resistant protective skins) or perfluorinated monomers (for forming coats that impart hydrophobicity and some increase in strength).

Leventis, Nicholas↗

NASA NTRS2013

The Effect of Fiber Strength Stochastics and Local Fiber Volume Fraction on Multiscale Progressive Failure of Composites

Continuous fiber unidirectional polymer matrix composites (PMCs) can exhibit significant local variations in fiber volume fraction as a result of processing conditions that can lead to further local differences in material properties and failure behavior. In this work, the coupled effects of both local variations in fiber volume fraction and the empirically-based statistical distribution of fiber strengths on the predicted longitudinal modulus and local tensile strength of a unidirectional AS4 carbon fiber/ Hercules 3502 epoxy composite were investigated using the special purpose NASA Micromechanics Analysis Code with Generalized Method of Cells (MAC/GMC); local effective composite properties were obtained by homogenizing the material behavior over repeating units cells (RUCs). The predicted effective longitudinal modulus was relatively insensitive to small (~8%) variations in local fiber volume fraction. The composite tensile strength, however, was highly dependent on the local distribution in fiber strengths. The RUC-averaged constitutive response can be used to characterize lower length scale material behavior within a multiscale analysis framework that couples the NASA code FEAMAC and the ABAQUS finite element solver. Such an approach can be effectively used to analyze the progressive failure of PMC structures whose failure initiates at the RUC level. Consideration of the effect of local variations in constituent properties and morphologies on progressive failure of PMCs is a central aspect of the application of Integrated Computational Materials Engineering (ICME) principles for composite materials.

multiscale analysis↗

NASA NTRSDate not supplied

Fracture Prediction of Epoxy Resin using Morse Bond Potential Embedded in GAFF using Molecular Dynamics Simulations

A generic method is developed to investigate the fracture behavior of an epoxy resin using atomistic molecular (MD) dynamics simulations. The epoxy system consisted of the stoichiometric mixture of tetra-/tri-functional epoxies and di-functional hardener molecules and was cured with a step-growth crosslinking algorithm. A hybrid force field (hFF) in which Morse bond function were added in second generation-general Amber Force Field (GAFF2) was used to capture bond breaking of the crosslinked epoxy system under uniaxial deformation. The Morse bond parameters for covalent bonds in the crosslinked backbone were fit to dissociation curves computed by CASPT2/6-311+G**. After the systems in various crosslink densities were obtained and equilibrated, the full length of stress-strain (𝜎-𝜀) curve was produced including initial elastic regime, yielding, plastic flow, strain hardening, and progressive failure. We found that the hFF was effective in studying the dissociation of crosslinked polymers and understanding the failure mechanism. In the results, the hFF delivered the same elastic property obtained from the unmodified force field GAFF. The stress-strain curve, however, began to be distinct in the plastic regime due to broken covalent bonds capable of altering the tensile behavior. Once the stress reached maximum, it progressively decreased until the ultimate failure (𝜎=0). Since hFF employed the existing GAFF functions with including a minimal change of its bond potential, this approach is easier to perform and computationally more efficient for unveiling the fracture behavior of polymer materials at the molecular level than other approaches with reactive force fields. We expect this approach will be utilized to accelerate the material-by-design process for thermosets by incorporate data from molecular models.

Changwoon Jang↗

DOE OSTI2024

Rational design of semi-interpenetrating network based on hyperbranched polyglycerol grafted MXene/polyurethane–epoxy for compressed hydrogen storage

Here, hydrogen (H 2 ) energy has emerged as a promising alternative in the automotive sector to replace fossil fuel; however, its storage with volumetric efficiency remains a challenge. The latest type IV storage vessel featuring a polymeric liner with composite overwrap incurs hydrogen saturation, which eventually causes failure. To prevent the H 2 dissolution in the liner, we have developed a barrier coating comprised of polyurethane/epoxy semi-interpenetrating network (S-IPN) combined with hyperbranched polyglycerol grafted MXene (h-MXene). The hyperbranched structure facilitated the dispersion of MXene in the coating solution by enhancing the exfoliation and improved the polymer filler interaction by forming covalent and H-bonding through end-terminal hydroxyl groups. Leveraging the dense network of S-IPN combined with the dispersed layer structured h-MXene significantly increased the tortuosity of the spray-coated barrier film applied to the nylon 6 liner. The coating exhibited a 90 % reduction in the H 2 gas permeability at only 2 wt% h-MXene concentration, which further improved to above 98 % at 10 wt% loading. Additionally, the h-MXene considerably improved the adhesion with the liner even in a highly stretched condition, signifying the durability of the coating under cyclic pressurization and depressurization of the storage vessel.

08 HYDROGEN↗

NASA NTRS2001

High T(g) Polyimides

The use of high temperature polymer matrix composites in aerospace applications has expanded steadily over the past 30 years, due to the increasing demand of replacing metal parts with light weight composite materials for fuel efficiency and bigger payloads in the aircraft and the space transportation vehicles. Polyimide/carbon fiber composites, especially, have been regarded as major high temperature matrix materials, based on their outstanding performance in terms of heat resistance, high strength-to-weight ratio and property retention compared with epoxies (177 C/350 F) and bismaleimides (232 C/450 F). Traditional, then-neoplastic polyimides were prepared from dianhydrides and diamines in N-methyl-2-pyrrolidinone (NMP) at room temperature to form the polyamic acids, which were then imidized at 150 C to yield polyimides. However, the high-boiling solvent (NMP, BP= 202 C) is very difficult to remove, leading to the formation of voids during composite fabrication. In the early 1970's, PMR addition curing polyimides with reactive endcaps were developed at the Lewis Research Center (renamed NASA Glenn) to ensure the easy processing of imide oligomers in methanol during composite fabrication.

Chuang, Kathy↗

DOE OSTI2023

Unexpected Thermomechanical Behavior of Off-Stoichiometry Epoxy/Amine Materials

Recent studies on off-stoichiometric thermosets reveal unique viscoelastic behavior derived from increased free volume and physical interactions between chain ends. To understand structural characteristics arising from cure and its effect on properties, we developed a Monte Carlo model based on step-growth polymerization. Our model accurately predicted structure–property trends for a two-component system of EPON 828 (EPON) and ethylenediamine. A second epoxy monomer, D.E.R. 732 (DER), was investigated to modulate T g . Binary mixtures of EPON and DER in off-stoichiometric, amine-rich formulations resulted in nonlinear evolution of thermomechanical properties with respect to initial formulation stoichiometry. Modifying our model with kinetic parameters allowing for differential epoxide/amine reaction kinetics only partially accounted for trends in T g , suggesting that spatiotemporal contributions-not captured by our model-were significant determinants of material properties compared to polymer architecture for three-component systems. Here these findings underpin the importance of spatial awareness in modeling to inform the development of dynamic thermosets.

36 MATERIALS SCIENCE↗

NASA NTRS1976

Fundamental analysis of the failure of polymer-based fiber reinforced composites

A mathematical model is described which will permit predictions of the strength of fiber reinforced composites containing known flaws to be made from the basic properties of their constituents. The approach was to embed a local heterogeneous region (LHR) surrounding the crack tip into an anisotropic elastic continuum. The model should (1) permit an explicit analysis of the micromechanical processes involved in the fracture process, and (2) remain simple enough to be useful in practical computations. Computations for arbitrary flaw size and orientation under arbitrary applied load combinations were performed from unidirectional composites with linear elastic-brittle constituent behavior. The mechanical properties were nominally those of graphite epoxy. With the rupture properties arbitrarily varied to test the capability of the model to reflect real fracture modes in fiber composites, it was shown that fiber breakage, matrix crazing, crack bridging, matrix-fiber debonding, and axial splitting can all occur during a period of (gradually) increasing load prior to catastrophic fracture. The computations reveal qualitatively the sequential nature of the stable crack process that precedes fracture.

Kanninen, M. F.↗

DOE OSTI2026

Ambient-Pressure Chemical Recycling of Thermoset Carbon Fiber-Reinforced Polymers via Low-Temperature Solvolysis: Techno-Economic and Life-Cycle Assessment

Carbon fiber-reinforced polymer (CFRP) waste is rapidly accumulating, with global volumes projected to exceed 500,000 tons annually by 2050. Virgin carbon fiber production is extremely energy- and cost-intensive, and growing demand has intensified supply-chain vulnerabilities associated with precursor availability and reliance on critical materials. Scalable recycling technologies therefore offer not only environmental benefits but also opportunities to reduce material costs and strengthen domestic composite supply chains. This study introduces an efficient, mild chemical recycling method for epoxy-amine CFRPs, utilizing acetic acid (80 wt%) and zinc acetate (1 wt%) at atmospheric pressure and low temperature (~110 °C). The solvolysis process preserves residual resin (~40%) on recycled carbon fibers (rCF), enhancing interfacial bonding in remanufactured composite materials. Recycled fibers retain ~90% of their mechanical properties, and recovered oligomers show potential for reuse in epoxy formulations, supporting material circularity. Techno-economic analysis (TEA) and life-cycle assessment (LCA) confirm the scalability and sustainability of this process.

Recycling CFRP↗

DOE OSTI2022

Surface Functionalized Barium Titanate Nanoparticles: A Combined Experimental and Computational Study

Barium titanate (BTO) nanoparticles show great potential for use in electrostatic capacitors with high energy density. This includes both polymer composite and sintered capacitors. However, questions about the nanoparticles' size distribution, amount of agglomeration, and surface ligand effect on performance properties remain. Reducing particle agglomeration is a crucial step to understanding the properties of nanoscale particles, as agglomeration has significant effects on the composite dielectric constant. BTO surface functionalization using phosphonic acids is known reduce BTO nanoparticle agglomeration. We explore solution synthesized 10 nm BTO particles with tert-butylphosphonic acid ligands. Recent methods to quantifying agglomeration using an epoxy matrix before imaging shows that tert-butylphosphonic acid ligands reduce BTO agglomeration by 33%. Thermometric, spectroscopic, and computational methods provide confirmation of ligand binding and provide evidence of multiple ligand binding modes on the BTO particle surface.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Laboratory Radar Measurements in Support of the NASA Orbital Debris Program Office’s Size Estimation Model

The NASA Orbital Debris Program Office (ODPO) relies on ground-based radar measurements from both the Haystack Ultrawideband Satellite Imaging Radar (HUSIR) and the Goldstone Solar System Radar (Goldstone) to characterize mm to cm debris population in low Earth orbit (LEO). Radar measurements help characterize the size of orbital debris objects, particularly fragmentation debris. However, debris size is not directly measured by radar but inferred from the measured radar cross section (RCS) which depends on several parameters in addition to physical size including electrical conductivity and polarization. To interpret the observed RCS of orbital debris objects detected by radar measurements as physical sizes, NASA uses an empirical size estimation model (SEM) based on laboratory RCS measurements of breakup fragments generated during hypervelocity impact tests as well as some pieces of non-impact-generated “artificial” debris-like objects expected to be representative of the debris population. Since the development of the ODPO SEM, many new materials have been introduced to spacecraft construction. Consequently, ODPO plans to update the radar SEM based on planned laboratory RCS measurements of debris fragments from DebriSat, a ground-based hypervelocity impact experiment conducted in 2014 that consisted of a high-fidelity spacecraft model characteristic of a modern LEO spacecraft. Prior to measuring DebriSat fragments, a set of calibration targets with well-defined geometries and material compositions were measured at The Ohio State University’s ElectroScience Laboratory (OSU-ESL) compact radar range. These calibration measurements help to validate, and understand any limitations of, laboratory measurements of RCS. Calibration targets include idealizations of typical shape categories seen in DebriSat fragments such as nuggets, flat plates, and cylinders. As with DebriSat, calibration target materials were chosen to represent typical modern-day spacecraft components and include stainless steel, aluminum, printed circuit board (PCB) substrate, and carbon fiber-reinforced polymer (CFRP). These materials also represent a wide range of electrical conductivities, which strongly influences measured RCS and inferred target size. The RCS calibration measurements were collected over a frequency sweep from 2 to 18 GHz and stepping through different azimuth angles from 0 to 360 degrees at an elevation of 0 degrees. A second set of calibration measurements is in work consisting of more complex shapes such as bent rods and plates as well as different mounting options including epoxy and a 3D printed holder. These further measurements along with our initial calibration set will inform selection of representative DebriSat fragments for laboratory RCS measurements that will contribute to the planned update to the ODPO radar SEM. An appropriate subset of both the radar calibration and DebriSat samples will also be measured in the ODPO Optical Measurements Center to cross-calibrate size estimates over these different wavelength regimes.

Radar↗

NASA NTRS1982

Characterization and degradation studies on synthetic polymers for aerospace application

The anti-misting additive for jet fuels known as FM-9 (proprietary polymer) was characterized by elemental analysis, solubility studies and molecular weight determination. Physical properties of surface tension, viscosity, specific gravity and other physical parameters were determined. These results are compared with properties of polyisobutylene and fuels modified with the same; the misting characteristics of polyisobutylene and FM-9 in Jet A fuel are included. Characterization and degradation of phthalocyanine and its derivatives were accomplished by use of a mass spectrometer and a pyroprobe solid pyrolyzer. Metal phthalocyanine tetracarboxylic acids and phthalocyanine-tetraamine cured epoxies were studied. Epoxy/graphite composite panels were exposed to a NASA-Ames radiant panel fire simulator in the flaming and non-flaming modes; toxic gases of HCN and HZS were measured along with oxygen, Co2, Co, and organic gases.

Hsu, M. T. S.↗

DOE OSTI2022

Calibrating the SPECTACULAR constitutive model using legacy Sandia data for two filled epoxy systems: 828/CTBN/DEA/GMB and 828/DEA/GMB

The SPECTACULAR model is a development extension of the Simplified Potential Energy Clock (SPEC) model. Both models are nonlinear viscoelastic constitutive models used to predict a wide range of time-dependent behaviors in epoxies and other glass-forming materials. This report documents the procedures used to generate SPECTACULAR calibrations for two particulate-filled epoxy systems, 828/CTBN/DEA/GMB and 828/DEA/GMB. No previous SPECTACULAR or SPEC calibration exists for 828/CTBN/DEA/GMB, while a legacy SPEC calibration exists for 828/DEA/GMB. To generate the SPECTACULAR calibrations, a step-by-step procedure was executed to determine parameters in groups with minimal coupling between parameter groups. This procedure has often been deployed to calibrate SPEC, therefore the resulting SPECTACULAR calibration is backwards compatible with SPEC (i.e. none of the extensions specific to SPECTACULAR are used). The calibration procedure used legacy Sandia experimental data stored on the Polymer Properties Database website. The experiments used for calibration included shear master curves, isofrequency temperature sweeps under oscillatory shear, the bulk modulus at room temperature, the thermal strain during a temperature sweep, and compression through yield at multiple temperatures below the glass transition temperature. Overall, the calibrated models fit the experimental data remarkably well. However, the glassy shear modulus varies depending on the experiment used to calibrate it. For instance, the shear master curve, isofrequency temperature sweep under oscillatory shear, and the Young's modulus in glassy compression yield values for the glassy shear modulus at the reference temperature that vary by as much as 15 %. Also, for 828/CTBN/DEA/GMB, the temperature dependence of the glassy shear modulus when fit to the Young's modulus at different temperatures is approximately four times larger than when it is determined from the isofrequency temperature sweep under oscillatory shear. For 828/DEA/GMB, the temperature dependence of the shear modulus determined from the isofrequency temperature sweep under oscillatory shear accurately predicts the Young's modulus at different temperatures. When choosing values for the shear modulus, fitting the glassy compression data was prioritized. The new and legacy calibrations for 828/DEA/GMB are similar and appear to have been calibrated from the same data. However, the new calibration improves the fit to the thermal strain data. In addition to the standard calibrations, development calibrations were produced that take advantage of development features of SPECTACULAR , including an updated equilibrium Helmholtz free energy that eliminates undesirable behavior found in previous work. In addition to the previously mentioned experimental data, the development calibrations require data for the heat capacity during a stress-free temperature sweep to calibrate thermal terms.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Identification of Known and Novel Monomers for Poly(hydroxyurethanes) from Biobased Materials

Sourcing polymers from biobased materials is desirable for a transition to a more sustainable world. However, finding new monomers sourced from biobased molecules requires extensive experimental effort, due to the fact that most biomolecules lack the functional groups or properties needed to serve as a monomer in a particular polymeric system without chemical modification. In this work, we demonstrate a computational screening method to obtain monomers of a non-isocyanate polyurethane (NIPU), polyhydroxyurethane (PHU), from biomolecules. Our method generates candidate monomers from a list of 15 selected biobased starting molecules by performing chemical transformations that are standard to chemical catalysis and organic synthesis on these starting molecules and then screening the results for molecules with moieties that can be used as monomers for a PHU. Product molecules from two generations of reaction, a total number of 20,057, were analyzed automatically to identify molecules that have two or more epoxy or cyclic carbonate functional groups as candidates for further derivatization. These 21 candidate molecules were then subjected to another two generations of reaction, producing a set of 17,913 additional molecules. Further scrutiny of this set for desired functional groups characterizing PHUs and querying against the PubChem database was carried out, and 15 known molecules that are commercially available were identified, with the desirable features that they are predicted to be derived from biobased starting molecules in four or fewer steps. Moreover, molecule space generated from this process was primarily comprised of molecules that were not known to PubChem, indicating the framework also has the ability to generate novel candidate monomers that originate from biobased starting points.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Improve durability and surface quality of additively manufactured molds using carbon fiber prepreg

Hybrid tooling is an emerging concept introduced in the aerospace industries to reduce weight and cost of traditional tools. A hybrid tool features a skin, which provides desired surface quality, durability, and a low-density substrate to reduce the weight of the mold. The big area additive manufacturing (BAAM) technology permits rapid production of thermoplastic polymer intensive large-scale structures. The present study features a carbon fiber reinforced polyphenylene sulfide (CF-PPS) substrate fabricated using Oak Ridge National Laboratory's BAAM system. Carbon fiber-bismaleimide (CF-BMI) prepreg skin was then bonded to the BAAM tool through high-pressure autoclave molding. Process optimization was conducted to improve the bonding between CF-PPS and CF-BMI (transverse tensile strength increased from 0.54 to 4.8 MPa). Durability of the mold was demonstrated from fabricating seven (7) carbon fiber-Huntsman epoxy hand lay-up parts utilizing the mold.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Correlation of dynamic dielectric measurements with viscosity in polymeric resin systems

Dynamic dielectric analysis has been used to study curing polymer systems and thermoplastics. Measurements have been made over a frequency range of six decades. This wide range of frequencies increases the amount of information which can be obtained. The data are analyzed in terms of the frequency dependence of the specific conductivity sigma and the relaxation time tau, parameters which are characteristic of the cure state of the material and independent of size of the sample. Dynamic dielectric measurements have been correlated with viscosity for the polysulfone thermoplastic UDEL-P1700 and with viscosity and ultrasonic measurements on the DGEBA-type epoxy Epon 828 cured with Agent U. The experimental results suggest that when ionic processes dominate the dielectric response, the intensive property sigma is a good monitor of the resin's viscosity. The results show that the dielectric relaxation time tau can be used to monitor the state of the system and the extent and rate of the reaction.

Kranbuehl, D.↗