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At least 217 records · Page 12

A new readily processable polyimide

As part of an effort to develop tough solvent resistance thermoplastics for potential use as structural resins on aerospace vehicles, a new processable polyimide was evaluated. The synthesis involved the reaction of a new diamine, 1,3-bis 2-(3-aminophenoxy)ethyl ether, with 3,3',4,4'-benzophenonetetracarboxylic dianhydride to form the polyamic acid and subsequent conversion of it to the polyimide. Various physical properties such as thermal stability, solvent resistance, glass transition temperature, crystalline melt temperature, melt viscosity and mechanical properties such as fracture toughness, adhesive, film and composite properties are reported. Of particular interest is the extremely high titanium to titanium tensile shear strength obtained for this polyimide.

Harris, F. W.↗

Simulated space environment effects on the optical properties of poly(arylene ethers)

Results are reported from a study of the stability of poly(arylene ethers) formed in a reaction of 1,3 -bis(4-chlorobenzoyl)benzene and various bisphenols after experiencing long-term exposure to space conditions. Transparent poly(arylene ethers) films were subjected to separate electron and UV bombardments, as were polysulfone and Kapton films for comparisons. The order of exposure to the two types of radiation was reversed for two sample populations. The optical properties and glass transition temperatures of the samples were determined after irradiation. The poly(arylene ethers) films exhibited good resistance to the electron radiation but suffered severe degradation in the UV environment. The loss of optical transmissivity was proportional to the UV radiation dose.

Sykes, George F.↗

An ab initio study on (C5H5V)2C8H8

The bonding in the organometalic compound nu-(eta exp 5-(cyclooctatetraene) bis (eta exp 2 cyclopentadienyl) vanadium) involves a complex mixture of metal-metal and metal-ligand contributions. Although there is a direct V-V 3d interaction it is not as strong as a double bond with some triple bond character as has been suggested based upon experiment. The balance between metal-metal and metal-ligand bonding results in the appearance of a low-lying triplet state which retains the V-V 3d bonding. A small singlet-triplet separation is consistent with the change in magnetic properties with temperature.

Luthi, Hans P.↗

Readily Processable Polyimide

Polymer exhibits resistance to hydraulic fluid, excellent processability, and extremely high adhesive strength. Synthesis involves reaction of new diamine, 1,3-bis 2-ethyl ether, with 3,3',4,4'-benzophenonetetracarboxylic dianhydride to form polyamic acid and subsequent conversion to polyimide.

Hergenrother, Paul M.↗

In situ deposits of copper and copper oxide containing condensation polyimide films

Novel copper-polyimide composites have been synthesized via simultaneous thermal decomposition of solid solutions of bis (trifluoroacetylacetonato) copper (II) and thermal cyclodehydration of polyimide acid. In contrast to conventional filled polymer composites which are prepared by dispersion of particles or fibers in a polymer matrix this study has yielded in general uniform Cu or CuO dispersions of very small particle size that reside near the film surface that was exposed to the atmosphere during curing. The nature of the copper deposit, the thickness of the copper deposit, and the polyimide overlayer which bonds the copper to the polymer substrate depend on the curing atmosphere used. A variety of analytical surface methods along with thermogravimetric analysis and variable temperature (surface and volume) electrical resistivity measurements have been used to characterize these thin, flexible copper doped polyimide films.

Porta, G. M.↗

Isomeric oxydiphthalic anhydride polyimides

Much of the polyimide research at Langley Research Center has focused on isomeric modification of the diamine component; polyimides having considerably improved processability and adhesion have resulted. The present structure-property study was designed to investigate how isomeric attachment of the three oxydiphthalic anhydride (ODPA) polyimides affects their properties. Each dianhydride, 3,4,3',4'-oxydiphthalic anhydride (4,4'-OPDA,I), 2,3,2',3'-oxydiphthalic anhydride (3,3'-ODPA,II), and 2,3,3',4'-oxydiphthalic anhydride (3,4'-OPDA,III), was reacted with p-phenylenediamine, 4,4'-oxydianiline, 3,3'-diaminodiphenylsulfone, 3,3'-diaminobenzophenone, and 4,4'-bis(3-aminophenoxy)benzophenone in DMAc. The inherent viscosities of the resulting poly(amic acids) were determined. Thermally imidized films were studied for their creasability and solubility, as well as by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and wide angle X-ray scattering (WAXS). A comparison of these properties will be made.

Gerber, Margaret K.↗

A study of thermal transitions in a new semicrystalline thermoplastic polyimide

A polyimide derive from 4,4'-isophthaloyl diphthalic anhydride (IDPA) and 1,3-bis (4-aminophenoxy 4'-benzoyl) benzene (1,3-BABB) having semicrystalline behavior was prepared and characterized by differential scanning calorimetry (DSC) and wide angle X-ray scattering (WAXS). Thus a poly(amic acid) film cured in air for one hour each at 100 and 200 C displayed an endotherm at 286 C, followed by a crystallization exotherm at 317 C, and a second melting transition at 350 C. The 286 C melting point appeared to result from earlier solvent-induced crystallization. Films cast from DMAc, air dried, and soaked in methylene chloride could not be induced into semicrystallinity. The fully cured polyimide has a Tg of 216 C. Films heated to temperatures as high as 100 C for one hour in air were transparent and light yellow in color. Those films heated to or above 125 C were translucent. Polarized light microscopy revealed the presence of spherulites 608 micrometers in diameter in a sample cured to 275 C in air. Two film samples, one cured to 275 and the other to 325 C, were evaluated for tensile and ultimate strength, modulus, and percent elongation at 25 and 200 C. These values remained essentially constant at each test temperature.

Pratt, J. Richard↗

Improved high-temperature resistant matrix resins

A study was performed with the objective of developing matrix resins that exhibit improved thermo-oxidative stability over state-of-the-art high temperature resins for use at temperatures up to 644 K (700 F) and air pressures up to 0.7 MPa (100 psia). The work was based upon a TRW discovered family of polyimides currently licensed to and marketed by Ethyl Corporation as EYMYD(R) resins. The approach investigated to provide improved thermo-oxidative properties was to use halogenated derivatives of the diamine, 2, 2-bis (4-(4-aminophenoxy)phenyl) hexafluoropropane (4-BDAF). Polyimide neat resins and Celion(R) 12,000 composites prepared from fluorine substituted 4-BDAF demonstrated unexpectedly lower glass transition temperatures (Tg) and thermo-oxidative stabilities than the baseline 4-BDAF/PMDA polymer.

Green, H. E.↗

Determination of the thermal stability of perfluoroalkylethers by tensimetry: Instrumentation and Procedure

A computerized tensimeter and experimental procedure for determination of the thermal decomposition temperature (T sub d) of perfluoro alkylethers were developed and tested. Both the apparatus and the procedure are described in detail. Results of testing with bis(2-ethylhexyl) phthalate and trimethylolpropane triheptanoate demonstrate that the reciprocal of the decomposition temperature is a linear function of the logarithm of the gas volume/heated liquid volume ratio. The T sub d obtained for each compound at a gas volume/heated liquid volume ration of one was similar to the value previously reported using an isoteniscope technique. Results of testing with a polymer of hexafluoropropylene oxide demonstrate that this instrument and procedure can be used to determine the T sub d of perfluoroalkylethers.

Helmick, Larry S.↗

Polyimide/metal composite films via in situ decomposition of inorganic additives - Soluble polyimide versus polyimide precursor

Polyimide-metal oxide (Co3O4 or CuO) composite films have been prepared via in situ thermal decomposition of cobalt (II) chloride or bis(trifluoroacetylacetonato)copper(II). A soluble polyimide (XU-218) and its corresponding prepolymer (polyamide acid) were individually employed as the reaction matrix. The resulting composites exhibited a greater metal oxide concentration at the air interface with polyamide acid as the reaction matrix. The water of imidization that is released during the concurrent polyamide acid cure and additive decomposition is believed to promote metal migration and oxide formation. In contrast, XU-218 doped with either HAuCl4.3H2O or AgNO3 yields surface gold or silver when thermolyzed (300 C).

Rancourt, J. D.↗

Conserving approximations for strongly correlated electron systems - Bethe-Salpeter equation and dynamics for the two-dimensional Hubbard model

A semianalytical approach is described for strongly correlated electronic systems which satisfies microscopic conservation laws, treats strong frequency and momentum dependences, and provides information on both static and dynamic properties. This approach may be used to treat large systems and temperatures lower than those currently accessible to finite-temperature quantum Monte Carlo techniques. Examples of such systems include heavy-electron compounds, organic Bechegaard salts, bis-(ethylenedithiolo)-TTF superconductors, and the oxide superconductors. The technique is based on the derivation and self-consistent solution of infinite-order conserving approximations. The technique is used to derive a low-temperature phase diagram and dynamic correlation functions for the two-dimensional Hubbard lattice model.

Bickers, N. E.↗

Polyimides containing carbonyl and ether connecting groups - II

In a study of polyimides containing carbonyl and ether connecting groups between aromatic rings, several new polyimides were prepared and characterized. A few of these polymers were semicrystalline. Glass transition temperatures ranged from 164 to 258 C, and crystalline melt temperatures were observed between 350 and 424 C. The semicrystalline polyimide from the reaction of 3.3',4,4'-benzophenonetetracarboxylic dianhydride and 1,3-bis(4-aminophenoxy-4'-benzoyl)benzene provided transparent orange films with excellent tensile properties, exceptional resistance to solvents and strong base, and high thermooxidative stability. In addition, this polyimide provided excellent adhesive strength for joining titanium (6Al-4V) to titanium.

Hergenrother, P. M.↗

Novel polyimide compositions based on 4,4': Isophthaloyldiphthalic anaydride (IDPA)

A series of twelve high temperature, high performance polyimide compositions based on 4,4'-isophthaloyl diphthalic anhydride (IDPA) was prepared and characterized. Tough, film-forming, organic solvent-insoluble polyimides were obtained. Three materials were semicrystalline. Several gave excellent long-term thermooxidative stability by isothermal thermogravimetric analysis (ITGA) at 300 C and 350 C in air when compared to Kapton H film (duPont). One extensively studied material displayed different levels of semicrystallinity over a wide range of final cure time/temperatures. The polyimide from IDPA and 1,3-bis (4-aminophenoxy 4'-benzoyl) benzene exhibited multiple crystallization and melting behavior, implying the existence of two kinetic and two thermodynamic crystallization and melting transitions by differential scanning calorimetry (DSC).

Pratt, J. Richard↗

Bisannelation with a benzo(1,2-c:4,5-c-prime) difuran equivalent - A new route to linear acene derivatives

It was observed that the base peak in the mass spectra of all the Diels-Alder bis adducts of anthracene diendoxide as well as of its tetrahydro derivative appear at m/e 158, corresponding to the radical cation of benzo(1,2-c:4,5-c-prime) difuran (BDF). This paper describes a synthetic equivalent of BDF and demonstrates its utility for obtaining linear acene derivatives.

Luo, Jihmei↗

Chemistry and properties of new poly(arylene ether imidazoles)

As part of a program to develop high-temperature high-performance structural resins for aerospace applications, the chemistry and properties of new poly(arylene ether imidazoles) were investigated. The polymers were prepared by the nucleophilic displacement reaction of aromatic bis(imidazolephenols) with activated aromatic difluoro compounds. The amorphous thermoplastic polymers exhibited glass transition temperatures from 230 to 301 C, inherent viscosities from 0.46 to 1.46 dL/g, and number-average molecular weights as high as 59,300 g/mole. The polymers exhibit good toughness, adhesive, composite, and film properties. The chemical, physical, and mechanical properties of these materials are discussed.

Connell, J. W.↗

Evaluation of two bisimide additives in LARC-TPI adhesive

The processability of aromatic polyimides can be improved by the addition of bis (amide) acids or bisimides to LARC-TPI. These low molecular weight additives apparently lower the melt viscosity of aromatic polyimides without affecting the glass transition temperature. Well-consolidated, fiber reinforced composites were fabricated using this technology. LARC-TPI can be processed as a thermoplastic polyimide to form high strength bonds, however, this is generally accomplished by processing at relatively high bonding pressures. An adhesive investigation is presented on the effects of two bisimide additives to LARC-TPI in an attempt to improve the bonding process by lowering the viscosity of the material to achieve improved bond strength properties. Apparently, the high flow which is exhibited by the additives when they melt, tended to be masked by the more viscous LARC-TPI.

Progar, Donald J.↗

Additives to reduce susceptibility of thermosets and thermoplastics to erosion from atomic oxygen

Polymeric materials have many attractive features such as light weight, high strength, and broad applicability in the form of films, fibers, and molded objects. In low earth orbit (LEO), these materials, when exposed on the exterior of the spacecraft, have the serious disadvantage of being susceptible to erosion by atomic oxygen (AO). AO is the most common chemical species at LEO altitudes. AO can be an extremely efficient oxidizing agent as was apparent from the extensive erosion of organic films exposed in STS missions. The mechanism for erosion involves the reaction of oxygen atoms at the surface of the substrate to form small molecular species. The susceptibility of polymeric materials varies with their chemical composition. Films with silicon atoms incorporated in the molecular structures have large coefficients of thermal expansion. This limits their utility. In an alternative approach additives were sought that mix physically and form a protective oxide layer when the film is exposed to AO. A large number of organic compounds containing silicon, germanium, or tin atoms were screened. Most were found to have very limited solubility in the polyetherimide (Ultem) films that were being protected from AO. However, one, bis(triphenyl tin) oxide, (BTO), is miscible in Ultem up to about 25 percent. Films of Ultem polyimide containing up to 25 wt percent BTO were prepared by evaporation of solvent from a solution of Ultem and BTO. The effects of AO on these films were simulated in the oxygen atmosphere of a radio frequency glow-discharge chamber. In the second part of this study, atoms were incorporated in epoxy resins. Experiments are in progress to measure the resistance of films of the cured epoxy to AO in the discharge chamber.

Orwoll, Robert A.↗

Determination of the thermal stability of fluids by tensimetry - Instrumentation and procedure

A computerized tensimeter and experimental procedure for determination of the thermal decomposition temperature (T sub d) of perfluoro alkylethers were developed and tested. Both the apparatus and the procedure are described in detail. Results of testing with bis(2-ethylhexyl) phthalate and trimethylolpropane triheptanoate demonstrate that the reciprocal of the decomposition temperature is a linear function of the logarithm of the gas volume/heated liquid volume ratio. The T sub d obtained for each compound at a gas volume/heated liquid volume ration of one was similar to the value previously reported using an isoteniscope technique. Results of testing with a polymer of hexafluoropropylene oxide demonstrate that this instrument and procedure can be used to determine the T sub d of perfluoro alkylethers.

Helmick, Larry S.↗