Physical properties of aromatic hydrocarbons. I.
Torsional creep and creep recovery behavior of amorphous 1, 3, 5-tri-alpha-naphthyl benzene close to or below glass transition temperature
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Viscoelasticity and plasticity considerations in the fracture of glasslike high polymers.
Fracture theory for amorphous high polymers below glass transition temperature, considering viscoelastic effects on structural defect stress concentration
CRACK PROPAGATION↗
Preparation of highly fluorinated polyurethanes
New polyurethanes, formed from a reaction of a prepolymer diol and a perfluorinated diisocyanate, are nonflammable and possess high corrosion resistance and good low temperature flexibility. Polymer hardness increases rapidly with increasing ratio of diisocaynate to diol, but its glass transition temperature is not adversely affected.
Rochow, S. E.↗
Some aspects of the thermal history of lunar glass.
Electron microprobe examination revealed that glassy lunar fragments had inclusions as well as boundaries between mineral glasses of different compositions. Glassy lunar spherules showed detectable heterogeneity less marked than that of the fragments. The room-temperature refractive indices and densities of the spherules are changed by heat-treating them at 500 to 700 C. The large increases (as much as 2% in density and 0.7% in index of refraction) are difficult to explain on the basis of classical glass-transition phenomena alone unless extremely rapid cooling rates are assumed. Further, the spherules darkened significantly when they were heated in air or a medium vacuum above 625 C.
Cooper, A. R.↗
Method for estimating solubility parameter
Semiempirical correlations have been developed between solubility parameters and refractive indices for series of model hydrocarbon compounds and organic polymers. Measurement of intermolecular forces is useful for assessment of material compatibility, glass-transition temperature, and transport properties.
Lawson, D. D.↗
Preparing thermoplastic aromatic polyimides
Method prepares aromatic polyimides with significantly reduced glass-transition temperatures and without accompanying loss of high-level thermo-oxidative stability which has been typical. This has been made possible by use of diamine monomers with specific stereoisomeric features.
Bell, V. L.↗
Low-resistivity homogeneous elastomers
Mixture of polyurethane polyelectrolyte and soluble, conducting organic compound produces homogeneous elastomer which has resistivity several orders of magnitude less than polyelectrolyte alone. Elastomeric material has novel resistivity dependence on temperature, that is, resistivity changes dramatically over narrow temperature range in vicinity of glass transition temperature.
Somoano, R. B.↗
Characterization of Adhesives for Attaching Reusable Surface Insulation on Space Shuttle Vehicles
An extensive development and testing program on adhesive systems shows that: (1) A closed cell silicone rubber sponge bonded to substrates with thin bond lines of glass filled adhesive exhibits density and modulus values approximately one third that of solid silicone adhesives; (2) utilization of glass or phenolic microballoons as fillers in silicone adhesives reduces density but increases moduli of the vulcanized materials; (3) the silicone elastomer based adhesives appear to be complex systems rather than homogeneous, isotropic materials. Tensile, shear, and compression properties plotted versus temperature verify this conjecture; and (4) constant strain-stress relaxation tests on glass-filled adhesive show that stress relaxation is most pronounced near the glass transition temperature.
Owen, H. P.↗
Low-temperature relaxations in amorphous polyolefins
The dynamic mechanical relaxation behavior of two series of amorphous polyolefins, was investigated from 4.2 K to the glass transition. Most of the polymers show a damping maximum or plateau in the 40 to 50 K region. Various mechanisms which have been suggested for cryogenic relaxations in amorphous polymers are considered as they might relate to the polyolefins. Two secondary relaxation processes above 80 K are distinguished. A relaxation at about 160 K (beta) in the second and third member of each series is associated with restricted blackbone motion. This process requires a certain degree of chain flexibility since it is not observed in the first member of each series. A lower temperature process (gamma) is observed in each member of the second series and is attributed to motion of the ethyl side group.
Hiltner, A.↗
Study to define behavior of liquid lubricants in an elastohydrodynamic contact
The spectra of an ester and a saturated hydrocarbon polymer were obtained at pressures ranging from ambient to 2 GN/sq m (20 kilobar) and at temperatures between ambient and 180 C in absorption and between 150 C and 210 C in emission. To simulate contact conditions the fluids were contained in the tiny sample volume of a diamond cell, i.e., the hole in a metal spacer separating two diamonds pressed against each other in a nut crackerlike arrangement. Pressures could be deduced from bandshifts and states of aggregation from bandwidths in the fluorescence spectrum of a ruby crystal immersed in the fluids. An infrared Fourier transform spectrometer was used with attachments specially designed to analyze the radiation passed through the sample and both diamonds (absorption technique) or the radiation emanating from the heated sample and passing through only one diamond (emission technique). The latter technique is applicable to operating EHD contacts. Spectral changes pointing to possible glass transitions and composition changes were observed. Emission and absorption spectra were generally equivalent. Some emission bandshapes appear to be temperature sensitive enough to be useful as internal temperature probes.
Lauer, J. L.↗
Isomer effects on polyimide properties
The effect of structure variation on the solubility and glass-transition temperature of polyimide polymers is investigated. The addition of alkyl substituents to an aromatic ring in the polymer molecule, the reduction in the number of imide rings per average polymer chain-length, and a variation in the symmetry of the polymer molecule are studied. The synthesis of key intermediates for the preparation of the monomers required in this investigation is reported along with progress made in the synthesis of polyimide-precursor amines that contain functional groups to allow for post-cure cross-linking.
Stump, B. L.↗
Effects of multifunctional crosslinking agents on the thermomechanical properties of polyimide films
Three polyfunctional amines were synthesized. Polyimide films containing varying amounts of the amine crosslinking agents were prepared. Their thermomechanical properties were compared with those of control film samples prepared from difunctional amines. The effect of crosslink density on isothermal weight loss, polymer softening, and glass transition temperature is discussed.
Delvigs, P.↗
Effects of multifunctional crosslinking agents on the thermomechanical properties of polyimide films
The potential of high temperature resistant polymers such as polyimides (PI) and polyphenylquinoxalines (PPQ) as matrix resins in fiber-reinforced composites has not been fully realized to date. One of the problems associated with these resins is that they exhibit creep, or thermoplastic yielding under load at temperatures approaching 316 C (600 F). The purpose of this investigation was to further reduce thermoplastic behavior of polyimide resins by substituting a controlled amount of the diamine monomer with crosslinking agents having a higher amine functionality. The knowledge gained from a study of the thermomechanical properties of the crosslinked resins would then be used in the fabrication of fiber-reinforced polyimide composites. This report describes the synthesis and characterization of three new polyfunctional amines. Polyimide films containing varying amounts of the cross-linking agents were prepared, and their properties compared with those of control samples prepared with difunctional amines. The effect of crosslink density on isothermal weight loss, polymer softening, and glass transition temperatures is discussed.
Delvigs, P.↗
Rate and time dependent behavior of structural adhesives
Studies on two adhesives (Metlbond 1113 and 1113-2) identified as having applications in the bonding of composite materials are presented. Constitutive equations capable of describing changes in material behavior with strain rate are derived from various theoretical approaches. It is shown that certain unique relationships exist between these approaches. It is also shown that the constitutive equation derived from mechanical models can be used for creep and relaxation loading. A creep to failure phenomenon is shown to exist and is correlated with a delayed yield equation proposed by Crochet. Loading-unloading results are presented and are shown to correlate well with the proposed form of the loading-unloading equations for the modified Bingham model. Experimental results obtained for relaxation tests above and below the glass transition temperature are presented. It is shown that the adhesives obey the time-temperature superposition principle.
Renieri, M. P.↗
Development of polyphenylquinoxaline graphite composites
Six polyphenylquinoxalines (PPQ) containing pendant cyano (CN) groups were synthesized. The polymers were characterized in terms of inherent viscosity, glass transition temperature, softening temperature and weight loss due to aging in air at 316 C (600 F). The potential for crosslinking PPQs by trimerization of pendant CN groups was investigated. A polymer derived from 1 mole 3,3,4,4 -tetraaminobenzophenone, .2 mole p-bis(p -cyanophenoxyphenylglyoxalyl)benzene and .8 mole p-bis(phenylglyoxalyl)benzene was selected for more extensive characterization in HM-S graphite fiber-reinforced composites. Mechanical properties were determined using composites made from HM-S fiber and polymer and composites made from HM-S fiber, polymer and a potential CN group trimerization catalyst. Composite mechanical properties, inter-laminar shear strength and flexure properties, were determined over the temperature range of +21 C to 316 C.
Shdo, J. D.↗
Effects of tetraamine crosslinking agents on the thermomechanical properties of PMR polyimide composites
The effects were investigated of partial substitution of tetraamine crosslinking agents for diamine reactants on the thermomechanical properties of PMR polyimide resins and graphite fiber-reinforced composites. The effect of tetraamine content on isothermal weight loss, glass transition, and softening temperatures of neat resin samples is discussed. Composites were fabricated using PMR methodology. Monomeric solution of various stoichiometric ratios was used to impregnate Hercules HTS graphite fiber. The mechanical property retention characteristics of the composites at 316 C (600 F) are described.
Delvigs, P.↗
Environmental effects on polymeric matrix composites
Current epoxy resins utilized in high performance structural composites absorb moisture from high humidity environments. Such moisture absorption causes plasticization of the resin to occur with concurrent swelling and lowering of the glass transition temperature. Similar effects are observed in composites. Data are presented showing the effects of absorbed moisture on Hercules AS/3501-5 graphite/epoxy composites. Prediction of moisture content and distribution in composites, along with reduction in mechanical properties, are discussed.
Whitney, J. M.↗
Study of improved resins for advanced supersonic technology composites. Part 1: Heteroaromatic polymers containing ether groups. Part 2: Curing chemistry of aromatic polymers and composite studies
Fourteen ether-containing, aromatic dianhydrides have been synthesized from N-phenyl-3 or 4-nitrophthalimide and various bisphenols. The process involves nucleophilic displacement of activated nitro groups with bisphenolate ions. Ether-containing dianhydrides were indefinitely stable in the presence of atmospheric moisture. One-step, high temperature solution polymerization of the ether-containing dianhydrides with m-phenylene diamine, 4,4'-oxydianiline and 1, 3-bis(4-aminophenoxy)benzene afforded 42 polyetherimides. The polyetherimides were all soluble in m-cresol except two which were found to be crystalline. The glass transition temperatures of the polyetherimides ranged from 178 to 277 C. Soluble polybenzimidazopyrrolones containing ether groups were also prepared from the same ether-containing dianhydrides and aromatic tetraamines by one-step solution polymerization. Using low molecular weight polyetherimides, various thermoset resin systems were developed and tested as matrices for fiber-reinforced composites. The curing chemistry involving reaction of the phthalonitrile group and the o-diaminophenyl group was found to be generally applicable to crosslinking various aromatic polymers other than polyimides.
Takekoshi, T.↗