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Butyl acrylate syrups useful potting compounds for encapsulating photovoltaic cells in modular arrays. Material pourable liquid pumped into module, then cured to rubbery consistency. Cured material is thermoset elastomer highly transparent, low cost, flexible and with good low-temperature properties.
A flow model which describes the process of resin consolidation during prepreg lamination was developed. The salient features of model predictions were explored. It is assumed that resin flows in all directions originate from squeezing action between two approaching adjacent fiber/fabric layers. In the horizontal direction, a squeezing flow between two nonporous parallel plates is analyzed, while in the vertical direction a poiseuille type pressure flow through porous media is assumed. Proper force and mass balance was established for the whole system which is composed of these two types of flow. A flow parameter, CF, shows to be a measure of processibility for the curing resin. For a given external load-F the responses of resin flow during prepreg lamination, as measured by CF, are categorized into three regions: (1) the low CF region where resin flows are inhibited by the high chemoviscosity during initial curing stages; (2) the median CF region where resin flows are properly controllable; and (3) the high CF region where resin flows are ceased due to fiber/fabric compression effects. Resin losses in both directions are calculated. Potential uses of this model and quality control of incoming prepreg material are discussed.
A study was made of the behavior of radicals generated by Co-60 gamma radiation in the epoxy system tetraglycidyl-4,4'-diaminodiphenyl methane (TGDDM) cured with 4,4'-diaminodiphenyl sulfone (DDS). The molar ratio of TGDDM to DDS was varied in the epoxy samples, and they were prepared under the same curing conditions to obtain various extents of crosslinking. ESR spectrometry data suggest that the rate of decay of radicals is related to inhomogeneities in the resin, with radicals in the highly crosslinked regions having long decay times. The inhomogeneities are thought to be due to statistical variation associated with the complex crosslinking reactions or to difficulties in mixing the reactants.
Materials were selected and fabrication procedures developed for orthotropic birefringent materials. An epoxy resin (Maraset 658/558 system) was selected as the matrix material. Fibers obtained from style 3733 glass cloth and type 1062 glass roving were used as reinforcement. Two different fabrication procedures were used. In the first one, layers of unidirectional fibers removed from the glass cloth were stacked, impregnated with resin, bagged and cured in the autoclave at an elevated temperature. In the second procedure, the glass roving was drywound over metal frames, impregnated with resin and cured at room temperature under pressure and vacuum in an autoclave. Unidirectional, angle-ply and quasi-isotropic laminates of two thicknesses and with embedded flaws were fabricated. The matrix and the unidirectional glass/epoxy material were fully characterized. The density, fiber volume ratio, mechanical, and optical properties were determined. The fiber volume ratio was over 0.50. Birefringent properties were in good agreement with predictions based on a stress proportioning concept and also, with one exception, with properties predicted by a finite element analysis. Previously announced in STAR as N81-26183
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.
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.
Orientation of fibers in graphite-fiber-reinforced plastics easily determined with new method. Materials scientists thus ensure that fibers, usually not visible after graphite/plastic composite has been cured, properly oriented in test specimens and test results accurately represent the characteristics of composite. Method based on fact that continuous graphite fibers embeded in cured polymer matrix actually parallel conductors. Thus, resistance measured across laminate is at minimum when probes of ohmmeter connected to opposite ends of fibers.
Ethynyl-containing phenoxy resins have excellent shelf life in solution or in bulk. Cured ethynyl-containing phenoxy resins offer lower moisture absorption, higher use temperatures, and better thermal stability over stateof-the-art cross-linked phenoxy resins. Depending upon cross-link density, cured ethynyl-modified phenoxy resins are solvent resistant but still thermoformable and relatively tough. Modified resins show potential for use as adhesives, composite matrices, solvent-resistant coatings, membranes, insulators, and films.
The following approaches improved the solvent resistance and raised the Tg of thermoplastics: end-capping aligomers with ethynyl groups; incorporating ethynyl groups pendent along the polymer chain; and correcting polymers containing pendent ethynyl groups with a low molecular weight diethynyl compound. The following conclusions were reached: (1) film and composite properties off an ethynyl-terminated sulfone were better than those of UDEL (trademark); (2) fracture energy of an ethynyl-terminated sulfone was lower than that of UDEL (trademark); (3) residual palladium in the cured ethynyl-terminated sulfone lower the thermooxidative stability of the cured resin; (4) the properties of a phenoxy resin were altered considerably by placing pendent ethynyl groups along the polymer chain; and (5) property trade-offs must be considered when thermoplastics are modified via reactant groups.
The role of matrix ductility on the toughenability and toughening mechanism of elastomer-modified DGEBRA epoxies was investigated. Matrix ductility was varied by using epoxide resins of varying epoxide monomer molecular weights. These epoxide resins were cured using 4,4' diaminodiphenyl sulfone (DDS) and, in some cases, modified with 10% HYCAR(r)CTBN 1300X8. Fracture roughness values for the neat epoxies were found to be almost independent on the monomer molecular weight of the epoxide resin used. However, it was found that the fracture toughness of the elastomer-modified epoxies was very dependent upon the epoxide monomer molecular weight. Tensile dilatometry indicated that the toughening mechanism, when present, is similar to the mechanisms found for the piperidine cured epoxies in Part 1. SEM and OM corroborate this finding. Dynamic mechanical studies were conducted to shed light on the toughenability of the epoxies. The time-dependent small strain behavior of these epoxies were separated into their bulk and shear components. The bulk component is related to brittle fracture, whereas the shear component is related to yielding. It can be shown that the rates of shear and bulk strain energy buildup for a given stress are uniquely determined by the values of Poisson's ratio, nu. It was found that nu increases as the monomer molecular weight of the epoxide resin used increases. This increase in nu can be associated with the low temperature beta relaxation. The effect of increasing cross-link density is to shift the beta relaxation to higher temperatures and to decrease the magnitude of the beta relaxation. Thus, increasing cross-link density decreases nu and increases the tendency towards brittle fracture.
The results of a program designed to develop tough imide modified epoxy resins cured by bisimide amine (BIA) hardeners are described. State-of-the-art epoxides MY720 and DER383 were used, and four bismide amines were evaluated. These were the BIA's derived from the 6F anhydride (4,4'-(hexafluoroisopropylidene) bis(phthalic anhydride) and the diamines 3,3'-diaminodiphynyl sulfone, 4,4'-oxygianiline, 4,4'-methylene dianiline, and 1,12-dodecane diamine. A key intermediate, designated 6F anhydride, is required for the synthesis of the bisimide amines. Reaction parameters to synthesize a precursor to the 6F anhydride (6FHC) in high yields were investigated. The catalyst trifluoromethane sulfonic acid was studied. Although small scale runs yielded the 6FHC in 50 percent yield, efforts to ranslate these results to a larger scale synthesis gave the 6FHC in only 9 percent yield. Results show that the concept of using bisimide amine as curing agents to improve the toughness properties of epoxies is valid.
The amine cured epoxy wet winding resin used in fabrication of the SRM filament wound case is analyzed. High pressure liquid chromatography (HPSC) is utilized extensively to study lot-to-lot variation in both resin and curing agent. The validity of quantitative hplc methodology currently under development in-process resin/catalyst assay is assessed.
A standard specification for a selected class of graphite fiber/toughened thermoset resin matrix material was developed through joint NASA/Aircraft Industry effort. This specification was compiled to provide uniform requirements and tests for qualifying prepreg systems and for acceptance of prepreg batches. The specification applies specifically to a class of composite prepreg consisting of unidirectional graphite fibers impregnated with a toughened thermoset resin that produce laminates with service temperatures from -65 F to 200 F when cured at temperatures below or equal to 350 F. The specified prepreg has a fiber areal weight of 145 g sq m. The specified tests are limited to those required to set minimum standards for the uncured prepreg and cured laminates, and are not intended to provide design allowable properties.
A novel siloxane containing bismaleimide has been prepared by reacting maleic anhydride, benzophenonetetracarboxylic dianhydride and bis(gamma-aminopropyl)tetramethyldisiloxane. Characterization of this monomer was done by comparing its nuclear magnetic resonance spectrum (NMR) to those of model compounds. Solubility of the prepolymer was tested in amide, chlorinated and ether solvents. Films were cast from solution as well as by melt processing and a cure cycle was determined. Infrared spectrum (IR) of the resulting film was obtained. Thermal polymerization was investigated by differential scanning calorimetry (DSC). Thermal properties of the cured resin were followed by means of thermogravimetric analysis (TGA), torsional braid analysis (TBA) and dynamic mechanical analysis (DMA). Thermomechanical analysis (TMA) was used to study the effect of postcure on the glass transition temperature (Tg) of the resin. Adhesive strength of the resin was obtained at ambient temperature.
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.
The effect on selected polyimide properties when pendant alkyl groups were attached to the polymer backbone was investigated. A series of polymers were prepared using benzophenone tetracarboxylic acid dianhydride (BTDA) and seven different p-alkyl-m,p'-diaminobenzophenone monomers. The alkyl groups varied in length from C(1) (methyl) to C(9) (nonyl). The polyimide prepared from BTDA and m,p'-diaminobenzophenone was included as a control. All polymers were characterized by various chromatographic, spectroscopic, thermal, and mechanical techniques. Increasing the length of the pendant alkyl group resulted in a systematic decrease in glass transition temperature (Tg) for vacuum cured films. A 70 C decrease in Tg to 193 C was observed for the nonyl polymer compared to the Tg for the control. A corresponding systematic increase in Tg indicative of crosslinking, was observed for air cured films. Thermogravimetric analysis revealed a slight sacrifice in thermal stability with increasing alkyl length. No improvement in film toughness was observed.
Hydroxy-terminated polyarylates (HTPA) with number-average molecular weights of approximately 2500, 5000, 7500, and 10,000 were synthesized and converted to corresponding 4-ethynylbenzoyloxy-terminated polyarylates (ETPA) by reaction with 4-ethynylbenzoyl chloride. The terminal ethynyl groups were thermally reacted to provide chain extension and crosslinking. The cured ETPA exhibited higher glass transition temperatures (Tg) and better solvent resistance than a high molecular weight linear polyarylate. Solvent resistance was further improved by curing 2,2-bis(4-ethynylbenzoyloxy-4-prime-phenyl) propane, a coreactant, with ETPA at concentrations of approximately 10 percent (w/w).
Aluminum mandrels easy to remove. Lightweight aluminum mandrel for shaping epoxy/aramid ducts simplifies and speeds production. In new process, glass-reinforced epoxy/aramid cloth wrapped on aluminum mandrel. Stainless-steel flanges and other hardware fitted on duct and held by simple tooling. Entire assembly placed in oven to cure epoxy. After curing, assembly placed in alkaline bath dissolves aluminum mandrel in about 4 hours. Epoxy/aramid shell ready for use as duct. Aluminum mandrel used to make ducts of various inside diameters up to 6 in. Standard aluminum forms used. Conventional tube-bending equipment produces requisite curves in mandrels.