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A method of preparing insoluble thermoplastic aromatic polyimides is described, having uniquely low softening temperatures by reacting, in a suitable solvent, an aromatic dianhydride, and a meta-substituted aromatic diamine.
A thermoplastic rubber is made from a mixture of between about 10 percent and about 50 percent of asphalt, between about 5 percent and about 30 percent fluxing oil, and between about 35 percent and about 70 percent of a copolymer of polyethylene and vinyl acetate.
Relative toxicity data on the pyrolysis products of a variety of thermoplastic and thermoset polymers are presented. The data are presented in terms of time to incapacitation and time to death with a fixed sample weight of 1.0 g, and in terms of the apparent lethal concentration required to produce 50 percent mortality within a fixed exposure period of 30 min.
The thermochemical and flammability characteristics of some typical thermoplastic materials currently in use and others being considered for use in aircraft interiors are described. The properties studied included (1) thermal mechanical properties such as glass transition and melt temperature, (2) changes in polymer enthalpy by differential scanning calorimetry, (3) thermogravimetric analysis in an anaerobic and oxidative environment, (4) oxygen index, (5) smoke evolution, (6) relative toxicity of the volatile products of pyrolysis, and (7) selected physical properties. The generic polymers which were evaluated included: acrylonitrile-butadiene-styrene, bisphenol A polycarbonate, bisphenol fluorenone carbonatedimethylsiloxane block polymer, phenolphthalein-bisphenol A polycarbonate, phenolphthalein polycarbonate, polyether sulfone, polyphenylene oxide, polyphenylene sulfide, polyaryl sulfone, chlorinated polyvinyl chloride homopolymer, polyvinyl fluoride, and polyvinylidene fluoride. Processing parameters including molding characteristics of some of the advanced polymers are described. Test results and relative rankings of some of the flammability, smoke and toxicity properties are presented.
The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated included polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated included epoxy, bismaleimide, a modified phenolic and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.
The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated include polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated include epoxy, bismaleimide, a modified phenolic, and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass-reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented, and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.
The thermochemical and flammability properties of thermoplastic and thermoset polymers are discussed. The results of a thermogravimetric analysis of the polymers conducted on a DuPont 950 thermogravimetric analyzer using both nitrogen and air atmospheres are presented. Experimental data on smoke evolution are given, and the methodology for assessing the relative toxicity of the pyrolysis effluents is described. The values obtained from the flammability tests are compared with the stoichiometric char yield, and it is shown that the ignition tendency of the polymers is a linear function of the resin char yield
The compounds of the class of aromatic polyamides useful as matrix resins in the manufacture of composites or laminate fabrication were developed. The process for preparing this thermoplastic-thermoset polyamide system involves incorporating a latent crosslinking moiety along the backbone of the polyamide to improve the temperature range of fabrication thereof wherein the resin softens at a relatively low temperature (approx. 154 C) and subsequently sets-up or undergoes crosslinking when subjected to higher temperature (approx. 280 C).
In order to improve solvent resistance of aromatic thermoplastic polymers, ethynyl-terminated aromatic sulfone polymers (ETS), sulfone/ester polymers (SEPE) containing pendent ethynyl groups, and phenoxy resin containing pendent ethynyl groups are synthesized. Cured polysulfones and phenoxy resins containing ethynyl groups on the ends or pendent on the molecules exhibited systematic behavior in solvent resistance, film flexibility, and toughness as a function of crosslink density. The film and composite properties of a cured solvent-resistant ETS were better than those of a commercially available solvent sensitive polysulfone. The study was part of a NASA program to better understand the trade-offs between solvent resistance, processability and mechanical properties which may be useful in designing composite structures for aerospace vehicles.
Several thermoplastic polyimide resins that show potential as matrix resins developed. Number of processes for composite fabrication evaluated, including powder processing, which involves deposition of resin powder on graphite fiber from nonresin-solvent slurry. Although powder slurry approach is viable, use of solvent system more amenable with current prepreg manufacturing methods.
The polyimide from BTDA 1,6-hexanediamine and m-phenylenediamine was selected from a prior study for the present study. Methods to prepare prepreg which would provide low void composites at low molding pressures from the thermoplastic polyimide were studied. Cresol solutions of the polyimide were applied to a balanced weave carbon fabric and the cresol removed prior to composite molding. Low void composites were prepared from smoothed prepregs at high pressures (34.5 MPa) and temperatures as low as 260 C. Lower molding pressures lead to higher void composites. Need for a lower melt viscosity in the neat resin is suggested as a requirement to achieve low void composites at low pressures. Some mechanical properties are included.
Dynamic dielectric analysis has been used to study curing polymer systems and thermoplastics. Measurements have been made over a frequency range of six decades. The data are analyzed in terms of capacitance, conductance, dissipation, complex permittivity, and conductivity (sigma). Complex permittivity and sigma are properties which are characteristic of the cure state of the material and independent of the size of the sample. LARC-160, PMR-15, NARMCO 5208, Epon and UDEL-P1700 have been studied. 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.
Oriented unidirectional prepreg tapes formed in ceramic molds. New technique developed at Langley Research Center, using ceramic mold for fabrication of models from graphite/thermoplastic materials. Upper surface of wings and fuselage of advanced airplane selected as shape to test fabrication technique. Technique well suited for other complex shapes as well. Thermoplastic composite easily workable with normal shop equipment and painted and repaired by standard methods.
The effects the processing parameters pressure, temperature, and time have on the quality of continuous graphite fiber reinforced thermoplastic matrix composites were quantitatively accessed by defining the extent to which intimate contact and bond formation has occurred at successive ply interfaces. Two models are presented predicting the extents to which the ply interfaces have achieved intimate contact and cohesive strength. The models are based on experimental observation of compression molded laminates and neat resin conditions, respectively. Identified as the mechanism explaining the phenomenon by which the plies bond to themselves is the theory of autohesion (or self diffusion). Theoretical predictions from the Reptation Theory between autohesive strength and contact time are used to explain the effects of the processing parameters on the observed experimental strengths. The application of a time-temperature relationship for autohesive strength predictions is evaluated. A viscoelastic compression molding model of a tow was developed to explain the phenomenon by which the prepreg ply interfaces develop intimate contact.
Bonded single overlap shear specimens were fabricated from Graphite/PEEK (Polyetheretherketone) composite adherends and titanium adherends. Six advanced thermoplastic adhesives were used for the bonding. The specimens were bonded by an electromagnetic induction technique producing high heating rates and high-strength bonds in a few minutes. This contrasts with conventionally heated presses or autoclaves that take hours to process comparable quality bonds. The Graphite/PEEK composites were highly resistant to delamination during the testing. This allowed the specimen to fail exclusively through the bondline, even at very high shear loads. Nondestructive evaluation of bonded specimens was performed ultrasonically by energizing the entire thickness of the material through the bondline and measuring acoustic impedance parameters. Destructive testing confirmed the unique ultrasonic profiles of strong and weak bonds, establishing a standard for predicting relative bond strength in subsequent specimens.
A study was undertaken to investigate the loading rate effect on delamination fracture initiation toughness of a thermoplastic composite. For this purpose, double cantilever beam specimens of graphite/PEEK were tested in a displacement controlled mode using an Instron tensile test machine. Specimens were loaded at various crosshead speeds ranging from 0.05 cm/min to 100 cm/min. The interlaminar fracture toughness was found to decrease with increasing loading rate, and this decrease was more than one hundred percent over the five decades of loading rate employed.
The bonded shear creep and constant strain rate behaviors of zero, one, and three percent endcapped thermoplastic polyimidesulfone adhesive were examined at room and elevated temperatures. Endcapping was accomplished by the addition of phthalic anhydrides. The primary objective was to determine the effects of molecular weight on the mechanical properties of the adhesive. Viscoelastic and nonlinear elastic constitutive equations were utilized to model the adhesive. Ludwik's and Crochet's relations were used to describe the experimental failure data. The effects of molecular weight changes on the above mentioned mechanical behavior were assessed. The viscoelastic Chase-Goldsmith and elastic nonlinear relations gave a good fit to the experimental stress strain behavior. Crochet's relations based on Maxwell and Chase-Goldsmith models were fit to delayed failure data. Ludwik's equations revealed negligible rate dependence. Ultimate stress levels and the safe levels for creep stresses were found to decrease as molecular weight was reduced.
The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.