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At least 829 records · Page 46

Factors Affecting the Processing of Epoxy Film Adhesives

The increasing awareness that adhesive performance is controlled not only by the condition of the adherend surface but also the condition or state of the adhesive and the process parameters used during fabrication is expected to result in improved reliability, as well as bond performance. The critical process variables which have been found to control adhesive bond formation and ultimate bond strength in 250F and 350F curing epoxy adhesives are described in terms of fabrication parameters and adhesive characteristics. These include the heat-up rate and cure temperature during processing and the adhesive moisture content and age condition (degree of advancement). The diagnostic methods used to delineate the effects of these process variables on adhesive performance are illustrated. These are dielectric, thermomechanical (TMA) and dynamic mechanical (DMA) analyses. Correlation of test results with measured mechanical tensile lap shear strengths of bonded joints is presented and the results briefly discussed in terms of the additives and hardeners used in the adhesive systems.

Pike, R. A.↗

An improved processible acetylene-terminated polyimide for composites

The newest member of a family of thermosetting acetylene-substituted polyimide oligomers is HR600P. This oligomer is the isoimide version of the oligomer known as HR600P and Thermid 600. Although both types of material yield the same heat resistant end products after cure, HR600P has much superior processing characteristics. This attributed to its lower melting temperature (160 + or - 10 C, 320 + or - 20 F) in contrast to 202 C (396 F) for Thermid MC-600, its longer gel time at its processing temperature (16 to 30 minutes bvs 3 minutes), and its excellent solubility in low boiling solvents such as tetrahydrofuran, glymes, or 4:1 methyl ethyl ketone/toluene mixtures. These advantages provide more acceptable coating and impregnation procedures, allow for more complete removal at lower temperatures, provide a longer pot life or working time, and allow composite structure fabrication in conventional autoclaves used for epoxy composite curing. The excellent processing characteristics of HR600P allow its use in large area laminated structures, structural composites, and molding compositions.

Landis, A. L.↗

Chemical control of rate and onset temperature of nadimide polymerization

The chemistry of norbornenyl capped imide compounds (nadimides) is briefly reviewed with emphasis on the contribution of Diels-Alder reversion in controlling the rate and onset of the thermal polymerization reaction. Control of onset temperature of the cure exotherm by adjusting the concentration of maleimide is demonstrated using selected model compounds. The effects of nitrophenyl compounds as free radical retarders on nadimide reactivity are discussed. A simple copolymerization model is proposed for the overall nadimide cure reaction. An approximate numerical analysis is carried out to demonstrate the ability of the model to simulate the trends observed for both maleimide and nitrophenyl additions.

Lauver, R. W.↗

Characterization methodology for PMR-15

Characterization of model compounds, monomers, resin solutions and cure cycles of PMR-15 polyimide are performed. Successful separation of various reaction products is also accomplished by liquid chromatography. The PMR-15 cure analysis is performed by fourier transform spectroscopy and gas chromatograph - mass spectrometry. Characterization receiving inspection tests for Quality Control are recommended.

Hunter, A. B.↗

Quality assurance procedures for V378A matrix resin

A characterization methodology has been developed on which to base quality assurance procedures for U.S. Polymeric V378A bismaleimide matrix resin. Chemical composition is established by partition reverse phase and size exclusion liquid chromatography. Cure rheology behavior is quantitatively characterized by dynamic viscoelastic analysis using the parallel plate technique. The overall cure process is characterized by differential scanning calorimetry. The sensitivity of the procedures is evaluated by studying the effects of ambient out time on the chemical end behaviorial properties of the resin.

Hamermesh, C. L.↗

The 371 deg C mechanical properties of graphite/polyimide composites

A series of condensation polyimides based on pyromellitic dianhydride is synthesized and evaluated for potential application at 371 C. Several three-and four-ring benzenoid diamine systems containing oxygen bridging groups are investigated. Thermomechanical analysis of neat resin specimens indicate that the polyimide prepared from the dimethyl ester of pyrometallitic acid (PMDE) and 2,2-bis4-(4'-aminophenoxy) phenyl]-1,1,1,3,3,3- hexafluoropropane (BDAF) is the only resin system which has a glass transition temperature (Tg) above 371 C. The Tg of the PMDE/BDAF polyimide is found to be 390 C after a postcure air at 371 C for 24 hr. Unidirectional composites are fabricated from the PMDE/BDAF system and unsized Celion 6000 graphite fibers. Final cure temperatures in the range of 371 to 427 C with an applied pressure of 10.34 to 13.78 MPa are investigated. The void content of the composites ranges from 4.6 to 8.6 percent. Composites cured at 399 C under a pressure of 10.34 MPa and postcured in air at 371 C for 24 hr exhibit the highest 371 C interlaminar shear strength (ILSS, 40.7 MPa) and flexural strength (758 MPa). The thermo-oxidative stability of the composites is determined by subjecting specimens to isothermal exposure at 371 C in air at atmospheric pressure, as well as a pressure of 0.52 MPa. Specimens exposed at atmospheric pressure exhibit a weight loss of 12 percent after 200 hr of exposure and 88 percent retention of its original 371 C ILSS. In contrast, the specimens exposed at 0.52 MPa pressure exhibit a comparable weight loss after only 72 hr, and a 71 percent retention of its original 371 C ILSS.

Delvigs, P.↗

Chemoviscosity modeling for thermosetting resins

A chemoviscosity model, which describes viscosity rise profiles accurately under various cure cycles, and correlates viscosity data to the changes of physical properties associated with structural transformations of the thermosetting resin system during cure, was established. Work completed on chemoviscosity modeling for thermosetting resins is reported.

Tiwari, S. N.↗

Optically transparent/colorless polyimides

Several series of linear aromatic polyimide films have been synthesized and characterized with the objective of obtaining maximum optical transparency. Two approaches have been used as part of this structure-property relationship study. The first approach is to vary the molecular structure so as to separate chromophoric centers and reduce electronic interactions between polymer chains to lower the intensity of color in the resulting polymer films. A second and concurrent approach is to perform polymerizations with highly purified monomers. Glass transition temperatures of thermally cured polyimide films are obtained by thermomechanical analysis and thermal decomposition temperatures are determined by thermogravimetric analysis. Transmittance UV-visible spectra of the polyimide films are compared to that of a commercial polyimide film. Fully imidized films are tested for solubility in common organic solvents. The more transparent films prepared in this study are evaluated for use on second-surface mirror thermal control coating systems. Lightly colored to colorless films are characterized by UV-visible spectroscopy before and after exposure to 300 equivalent solar hours UV irradiation and varying doses of 1 MeV electron irradiation. The effects of monomer purity, casting solvent and cure atmosphere on polyimide film transparency are also investigated.

Stclair, A. K.↗

Toughening reinforced epoxy composites with brominated polymeric additives

Cured polyfunctional epoxy resins including tris (hydroxyphenyl) methane triglycidyl ether are toughened by addition of polybrominated polymeric additives having an EE below 1500 to the pre-cure composition. Carboxy terminated butadiene acrylonitrile rubber is optionally present in the precure mixture as such or as a pre-formed copolymer with other reactants. Reinforced composites, particularly carbon reinforced composites, of these resins are disclosed and shown to have improved toughness.

Nir, Z.↗

Evaluation of high temperature structural adhesives for extended service, phase 4

The evaluation of three phenylquinoxaline polymers as high temperature structural adhesives is presented. These included an experimental crisskubjabke oiktner (X-PQ) and two experimental materials (PPQ-2501) and (PPQ-HC). Lap shear, crack extension, and climing drum peel specimens were fabricated from all three polymers, and tested after thermal, combined thermal/humidity, and stressed Skydrol exposure. All three polymers generally performed well as adhesives at initial test temperatures from 219K (-67 F) to 505K (450 F) and after humidity exposure. The 644K (700 F) cured test specimens exhibited superior Skydrol resistance and thermal stability at 505K (450 F) when compared to the 602K (625 F) cured test specimens.

Hendricks, C. L.↗

Fracture morphology of 2-D carbon-carbon composition

Out-of-plane tensile tests of a woven fabric carbon-carbon composite were performed in a scanning electron microscope equipped with a tensile stage and a videotape recording system. The composite was prepared from T-300 8-harness satin graphite fabric and a phenolic resin. The (0/90/0/90/0 sub 1/2) sub 2 laminate, with a Theta describing the orientation of the warp fibers of the fabric, was cured at 160 C and pyrolized at 871 C. This was followed by four cycles of resin impregnation, curing, and pyrolysis. A micrograph of the cross section of the composite is presented. Inspection of the specimen fracture surface revealed that the filaments had no residual matrix bonded to them. Further inspection revealed that the fracture was interlaminar in nature. Failure occurred where filaments of adjacent plies had the same orientation. Thus it is postulated that improvement in transverse tensile strength of 2-D carbon-carbon depends on the improvement of the filament-matrix bond strength.

Avery, W. B.↗

Investigations of toughening mechanisms of epoxy resins

Composite material technology was applied to the solid rocket booster by the development of a carbon filament-epoxy resin case which yields a net increase of 4000 lbs. in payload in the shuttle. The question of reusability of the new composite tanks has not yet been answered and will depend on the toughness of the matrix resin. The present study was aimed at providing conditions whereby test specimens of the epoxy resin (EPON/85) and curing agents of systematically varied structures could be produced in a controlled manner. Three sets of conditions were found that might allow the isolation of the structural effects on toughness from the cure effects. The kinetic methods leading to the determination of these conditions are described.

Koenig, T.↗

Polyimide analysis using diffuse reflectance-FTIR

The thermal imidization of a number of polyimide precursors in the form of powders, films, and prepregs was examined by an in situ diffuse reflectance-FTIR technique where infrared spectra were determined while the material was being heated. An analysis of these spectra revealed that, with the exception of one water soluble adhesive, each precursor developed an anhydride band around 1850 cm/cu during imidization. This band diminished in intensity during final stages of cure. Efforts were made to quantify the amount of anhydride in several samples. Evidence obtained could be interpreted to mean that poly(amic acid) resins undergo an initial reduction in molecular weight during imidization before recombining to achieve their ultimate molecular weights as polyimides. Several reports in the literature are cited to support this interpretation. This report serves both to document anhydride formation during imidization and to increase our fundamental understanding of how polyimides cure.

Young, P. R.↗

Synthesis of diamino terminated poly(arylene ether sulfone) oligomers as reactive intermediates in copolymer systems

Reactive diamino terminated oligomers of pre-determined molecular weights can be prepared by either of two synthetic routes depending upon the compound used to introduce the amine functionality. After characterization by spectroscopic and thermal methods, these oligomers can be used in several post-reactions to yield novel block and segmented copolymer systems. A potential application for these poly(arylene ether sulfone) oligomers exists in the curing or co-curing of epoxy resins for improving toughness. They can also be used to prepare toughened bismaleimide systems as well as producing copolymers with improved solvent resistance, especially with respect to chlorinated solvents.

Jurek, M. J.↗

Variational divergence in wave scattering theory with Kirchhoffean trial functions

In a recent study of variational improvement of the Kirchhoff approximation for electromagnetic scattering by rough surfaces, a key ingredient in the variational principle was found to diverge for important configurations (e.g., backscatter) if the polarization had any vertical component. The cause and a cure of this divergence are discussed here. The divergence is demonstrated to occur for arbitrary perfectly conducting scatterers and its universal characterstics are determined, by means of a general divergence criterion that is derived. A variational cure for the divergence is prescribed, and it is tested successfully on a standard scattering model.

Bird, J. F.↗

The pultrusion process for structures on advanced aerospace transportation systems

The pultrusion process, which has the potential for use in the manufacture of structures for aerospace hardware, is described. In this process, reinforcing fibers are pulled continuously through a resin system for wetting and subsequently through a heated die for polymerization. By using this process, fabrication of very long lengths of high strength, lightweight structures with consistently high quality for aerospace applications is possible. The more conventional processes involve hand lay-up, vacuum bagging, autoclaving or oven curing techniques such that lengths of structural elements produced are limited by the lengths of autoclaves or curing ovens. Several types of developmental structural elements are described in which fiberglass, aramid, graphite, and hybrid fiber systems have been used as reinforcements in an epoxy matrix and their flexural properties compared. Reinforcement fibers having tailor-made orientations which achieve tailor-made strength in the pultrusions are described. The potential aerospace applications for the pultruded products are described with advantages cited over conventional hand lay-up methods.

Wilson, Maywood L.↗

Stronger Fire-Resistant Epoxies

New curing agent improves mechanical properties and works at lower temperature. Use of aminophenoxycyclotriphosphazene curing agents yields stronger, more heat- and fire-resistant epoxy resins. Used with solvent if necessary for coating fabrics or casting films.

Fohlen, George M.↗

Validation of the filament winding process model

Tests were performed toward validating the WIND model developed previously for simulating the filament winding of composite cylinders. In these tests two 24 in. long, 8 in. diam and 0.285 in. thick cylinders, made of IM-6G fibers and HBRF-55 resin, were wound at + or - 45 deg angle on steel mandrels. The temperatures on the inner and outer surfaces and inside the composite cylinders were recorded during oven cure. The temperatures inside the cylinders were also calculated by the WIND model. The measured and calculated temperatures were then compared. In addition, the degree of cure and resin viscosity distributions inside the cylinders were calculated for the conditions which existed in the tests.

Calius, Emilo P.↗