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Curing technique for producing variable viscosity seal has hard sealing surface supported by softer rubber. Valve seal is clamped between two jaws for curing with hotter jaw at temperature of approximately 350 F and lower at room temperature. Result is durable tight valve-seat.
Lamination setup is used to produce void-free bonds by first employing vacuum to outgas materials and adhesive at temperature below curing temperature and then subjecting assembly to pressure and temperature necessary to cure.
Electromagnetic curing is used to bond strain gage to aluminum tensile bar. Electromagnetic energy heats only plastic/metal interface by means of skin effect, preventing degradation of heat-treated aluminum. Process can be easily applied to other metals joined by high-temperature-curing plastic adhesives.
A process is described for the preparation of composite laminate.structures of glass cloth preimpregnated with polybismaleimide resin and adhered to a polybismaleimide glass or aromatic polyamide paper honeycomb cell structure that is filled or partially filled with a syntactic foam consisting of a mixture of bismaleimide resin and carbon microballoons. The carbon microballoons are prepared by pyrolyzing phenolic microballoons and subsequently bonded using a 2% bismaleimide solution. The laminate structures are cured for two hours at 477 deg K and are adhered to the honeycomb bismaleimide adhesive using a pressure of 700 KN/sq m pressure at 450 deg K. The laminate composite is then post-cured for two hours at 527 deg K to produce a composite laminate having a density in the range from about 95 kilograms per cubic meter to 130 kilograms per cubic meter.
The synthesis of a class of bis(imide-amine) curing agents for epoxy matrix resins is discussed. Glass transition temperatures and char yield data of an epoxy cured with various bis(imide-amines) are presented. The room temperature and 350 F mechanical properties, and char yields of unidirectional graphite fiber laminates prepared with conventional epoxy and imide-modified epoxy resins are presented.
This report describes the results of a one-year program designed to synthesize new, nonvolatile crosslinking monomers and to prove their feasibility in the development of lower temperature curing PMR-polyimide resins with high temperature capability. The objective of this program is to develop PMR-polyimide resins capable of being processed at a maximum temperature of 232C to 288C (450F to 500F) without sacrifice of the high temperature 316C (600F) capability of the state-of-the-art PMR-15 polyimide resin. Four monomethyl esters were synthesized and characterized for use in the crosslinking studies. It was found that all four crosslinkers were capable of entering into a crosslinking reaction to produce polymer specimens which were strong, dense and free of voids. The infrared and DSC studies of each crosslinker with monomers 4,4'-methylenedianiline (MDA) and the dimethyl ester of 3,3',4,4'-benzophenonetetracarboxylic acid (BTDE) comprising the resin systems, crosslinker/MDA/BTDE suggested that curing could be accomplished at 288C (550F). However, fabrication of dense, void free polymer specimens required a temperature of 316C (600F) and a pressure of 0.69 MPa (100 psi). The crosslinkers, monomethyl ester of 2,5-bicyclo[2.2.1]heptadiene-2,3-dicarboxylic acid (NDE) and monomethyl ester of maleic acid (MAE) were selected for evaluation in Celion 6000/PMR polyimide composites. These composites were characterized at RT, 288C (550F) and 316C (600F) initially and after isothermal aging at 288C (550F) and 316C (600F) for several hundred hours. The results of the isothermal aging studies suggested that both PMR systems NDE-MDA-BTDE and MAE-MDA-BTDE are promising candidates as matrices for addition type polyimide composites. These studies demonstrated that alternate crosslinkers to NE/MDA/BTDE are feasible, but mechanisms to lower the crosslinking temperature must be developed to provide lower temperature processing PMR-type polyimides.
Adhesive systems which could be used to bond composite-to-composite, composite-to-titanium, and honeycomb sandwich structures with operational capability at 589K for a minimum of 125 hours were evaluated. Evaluations were based on mechanical property tests such as lap shear and flatwise tensile and on processability. Quasi-isotropic Celion 6000/PMR-15 composite adherend was used to construct lap shear and flatwise tensile specimens. Hexcel's HRH-327-3/16-6.0 glass polyimide honeycomb core was also utilized in the flatwise tensile specimens. Numerous processing variations were also studied that led to selected cure cycles for each adhesive. Shear specimens having either 12 mm or 75 mm overlaps were used to determine the effect of bond size on processability and lap shear properties. The data indicate that processing of FM-34, FM-34B-18, LARC-13 and NRO56X can be achieved using a cure compatible with the composite adherend. No significant differences in mechanical properties were observed among the three adhesive systems and all three are suitable candidates for 589K/125 hour service.
The successful fabrication of high temperature resistant composites depends mainly on the processability of the resin binder matrix. For two new bismaleimide type resins the processing of graphite fabric prepregs to composites is described. One resin coded M 751 has to be processed from N-Methylpyrrolidone, the other resin evaluated is a so-called hot melt solvent-less system. Commercial T300/3000 Graphite fabrics were used as reinforcement. The M 751 - Resin is a press grade material and laminates are therefore moulded in high pressure conditions (400 N/sq cm). The solvent-less resin system H 795 is an autoclave grade material and can be cured at 40 N/sq cm. The cure cycles for both the press grade and the autoclave grade material (Fiberite W 143 fabric prepregs) are provided and the mechanical properties of laminates at low (23 C) and high (232 C) temperatures were measured. For comparison, the neat resin flexural properties are also presented. The water absorption for the neat resins and the graphite fabric laminates after a 1000 hour period was evaluated.
Twenty seven addition cured phenolic resin compositions were prepared and tested for their ability to give char residues comparable to state-of-the-art phenolic resins. Cyanate, epoxy, allyl, acrylate, methacrylate and ethynyl derivatized phenolic oligomers were investigated. The novolac-cyanate and propargyl-novolac resins provided anaerobic char yields at 800 C of 58 percent. A 59 percent char yield was obtained from modified epoxy novolacs. A phosphonitrilic derivative was found to be effective as an additive for increasing char yields. The novolac-cyanate, epoxy-novolac and methacrylate-epoxy-novolac systems were investigated as composite matrices with Thornel 300 graphite fiber. All three resins showed good potential as composite matrices. The free radical cured methacrylate-epoxy-novolac graphite composite provided short beam shear strengths at room temperature of 93.3 MPa (13.5 ksi). The novolac-cyanate graphite composite produced a short beam shear strength of 74 MPa (10.7 ksi) and flexural strength of 1302 MPa (189 ksi) at 177 C. Air heat aging of the novolac-cyanate and epoxy novolac based composites for 12 weeks at 204 C showed good property retention.
Experimental work on the manufacture and strength of graphite-epoxy composites is considered. The correct data and thus a true assessment of the strength properties based on a proper and scientifically modeled test specimen with engineered design, construction, and manufacture has led to claims of a very broad spread in optimized values. Such behavior is in the main due to inadequate control during manufacture of test specimen, improper curing, and uneven scatter in the fiber orientation. The graphite fibers are strong but brittle. Even with various epoxy matrices and volume fraction, the fracture toughness is still relatively low. Graphite-epoxy prepreg tape was investigated as a sandwich construction with intermittent interlaminar bonding between the laminates in order to produce high strength, high fracture toughness composites. The quality and control of manufacture of the multilaminate test specimen blanks was emphasized. The dimensions, orientation and cure must be meticulous in order to produce the desired mix.
The contributions of individual resin components to total resin weight loss in 600 F air aged Celion 6000/PMR-15 polyimide composites were determined from the overall resin weight loss in the composite by chemically separating the PMR-15 matrix resin into its monomeric components. The individual resin components were also analyzed by spectroscopic techniques in order to elucidate curing and degradation mechanisms of the PMR-15 matrix resin. The isothermal weight loss of the individual resin components during prolonged 600 F thermo-oxidative aging of the composite was correlated to the changes observed in the Fourier Transform infrared spectra and Fourier Transform nuclear magnetic resonance spectra of the individual resin components. The correlation was used to identify the molecular site of the thermo-oxidative changes in PMR-15 polyimide matrix resin during 600 F curing the prolonged 600 F thermo-oxidative aging.
A process for preparing dianhydrides that are miscible with hydroxyl prepolymers at moderate temperatures and can cure hydroxyl prepolymers to elastomers at moderate temperatures is disclosed. The dianhydrides are prepared by solution reaction of a prepolymer diol with excess hydride followed by removal of unreacted dianhydride. The prepolymer dianhydrides are miscible with hydroxyl substituted hydrocarbon prepolymers and cure the prepolymers to polyester-linked elastomers.
Studies were performed to synthesize a novel class of bis (imide-amine) curing agents for epoxy matrix resins. Glass transition temperatures and char yield data of an epoxy cured with various bis (imide-amines) are presented. The room temperature and 350 F mechanical properties, and char yields of unidirectional graphite fiber laminates prepared with conventional epoxy and imide-modified epoxy resins are presented.
A porous tooling system was selected for the processing of Graphite/PMR-15 Polyimide laminates in thickness up to 3.2 mm. (0.125 inch). This tool system must have a reasonable strength, permeability dimensional stability, and thermal conductivity to accomplish curing at 600 F and 200 psi and 200 psi autoclave temperature and pressure. A permeability measuring apparatus was constructed and permeability vs. casting water level determined to produce tools at three different permeability levels. On these tools, laminates of 5, 11, and 22 plies (.027, .060, and 0.121 inch) were produced and evaluated by ultrasonic, mechanical, and thermal tests to determine the effect of the tool permeability on the cured laminates. All tools produced acceptable laminates at 5 and 11 plies but only the highest permeability produced acceptable clear ultrasonic C-Scans. Recommendations are made for future investigations of design geometry, and strengthening techniques for porous ceramic tooling.
The most promising of a number of new addition type polyimides and polyaromatic melamine (NCNS) resins for use in high performance composite materials. Three different cure temperature ranges were of interest: 530-560 K (500-550 F), 475-530 K (400-500 F), and 450 K (350 F). Examined were a wide variety of polyimide precursors terminated with 5 norbornene groups and addition polymerized at 560 K similar to PMR-15 and LARC-160 polyimides. In addition, a number of lower curing cinnamal end capped polyimides and a bismaleimide were investigated but were not found promising. A group of NCNS resins were investigated and some were found to be superior to current epoxy resins in moisture resistance, oxidative aging and flame and smoke properties.
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.
A description is given of the manufacturing processes developed for large-quantity production of space structure graphite/epoxy composite tubes. The tubes are to be delivered to orbit by the Space Shuttle and assembled by astronaut-assisted assembly machines. The tooling and manufacturing system uses a novel method of dry fiber placement which carefully controls fiber position and orientation and a non-autoclave cure for the epoxy resin. The means of dimensional tolerance control over differential thermal expansion between metal tooling and graphite tubes, resin shrinkage during cure, hot pressurized resins in close tolerance tooling, and tool wear, are examined in detail. A successful pilot production program is also reported.
An experimental program was carried out to investigate the effects of temperature and moisture on the damage development and fracture response of graphite/epoxy composites. Fracture response data were obtained for 20-ply laminates of different layup patterns for both room temperature and immediately after the application of a temperature transient causing the specimen to attain 150 C. It is found that elevated temperature degrades the notched strength of some laminates while not degrading others. The unnotched strength of all laminates tested at elevated temperatures was degraded. The effect of preloading on damage growth and moisture absorption, the effect of autoclave pressure during the laminate cure on fracture, and the variation of interlaminar shear properties with layup, moisture exposure, laminate material, and cure pressure are also discussed.