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At least 145 records · Page 8

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↗

The polymerization of amino acid adenylates on sodium-montmorillonite with preadsorbed polypeptides

The spontaneous polymerization of amino acid adenylates on Na-montmorillonite in dilute, neutral suspension, after polypeptides were adsorbed on the clay, is studied. It is found that the degrees of polymerization of the oligopeptides and polypeptides obtained is dependent on the amounts of polypeptides that were preadsorbed. It is concluded that a catalytic activity may derive from c-spacings that offer adsorption sites for the reagent amino acid adenylate within the peripheral recesses of irregularly stacked clay platelets by bringing the anhydride bonds and neutral amino groups into favorable reaction distances.

Paecht-Horowitz, Mella↗

Interphase tailoring in graphite-epoxy composites

The fiber-matrix interphase in graphite fiber-epoxy matrix composites is presently modified through the electrodeposition of a coating of the polymer poly(styrene-comaleic anhydride), or 'SMA' on the graphite fibers; optimum conditions have been established for the achievement of the requisite thin, uniform coatings, as verified by SEM. A single-fiber composite test has shown the SMA coating to result in an interfacial shear strength to improve by 50 percent over commercially treated fibers without sacrifice in impact strength. It is suggested that the epoxy resin's superior penetration into the SMA interphase results in a tougher fiber/matrix interface which possesses intrinsic energy-absorbing mechanisms.

Subramanian, R. V.↗

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↗

Polyamideimides containing carbonyl and ether connecting groups

Polyamidenimides were prepared from the reaction of trimellitic anhydride chloride with seven diamines containing carbonyl and ether groups between the aromatic rings. Several of these polyamideimides were semicrystalline as evidenced by wide-angle X-ray diffraction and differential scanning calorimetry. Glass transition temperatures ranged between 187 and 245 C, and crystalline transition temperatures ranged between 317 and 416 C. A series of copolyamideimides from a mixture of 1,3-bis(4-aminophenoxy 4-prime-benzoyl) benzene and 1,4-bis(4-aminophenoxy 4-prime-benzoyl)benzene were similarly prepared. These copolyamideimides were semicrystalline and formed tough, solvent resistant films with good tensile properties.

Havens, S. J.↗

Fast-Acting Rubber-To-Coated-Aluminum Adhesive

Cyanoacrylate adhesive used to join rubber to coated aluminum easier to apply and more effective. One-part material applied in single coat to aluminum treated previously with epoxy primer and top coat. Parts mated as soon as adhesive applied; no drying necessary. Sets in 5 minutes. Optionally, accelerator brushed onto aluminum to reduce setting time to 30 seconds. Clamping parts together unnecessary. Adhesive comes in four formulations, all based on ethyl cyanoacrylate with various amounts of ethylene copolymer rubber, poly(methyl methacrylate), silicon dioxide, hydroquinone, and phthalic anhydride.

Comer, Dawn A.↗

New Polyimide Has Many Uses

Low-toxicity and low-mutogenicity monomer key to new high-performance polyimide. LaRC-IA is thermoplastic polyimide made from 3-4'-oxydianiline and 4,4'-oxydiphthalic anhydride. Good processing characteristics, low toxicity, and no mutagenicity. Adhesives, composite matrix resins, heat resin moldings, and coating films made of new polymer found to exhibit properties identical or superior to commercially available polyimides. Potential applications wide ranging. With and without end capping, employed to prepare unfilled moldings, coatings and free films, adhesive tape, adhesively bonded substrates, prepregs, and composites.

St. Clair, Terry L.↗

Imide/Arylene Ether Copolymers

New imide/arylene ether copolymers prepared by reacting anhydride-terminated poly(amic acids) with amine-terminated poly(arylene ethers) in polar aprotic solvents. Each resulting copolymer may have one glass-transition temperature or two, depending on chemical structure and/or compatibility of block units. Most of copolymers form tough, solvent-resistant films with high tensile properties. Films cast from solution tough and flexible, and exhibit useful thermal and mechanical properties. Potentially useful as moldings, adhesives, or composite matrices. Because of flexible arylene ether blocks, these copolymers easier to process than polyimides.

Jensen, Brian J.↗

Processable polyimide adhesive and matrix composite resin

A high temperature polyimide composition prepared by reacting 4,4'-isophthaloyldiphthalic anhydride with metaphenylenediamine is employed to prepare matrix resins, adhesives, films, coatings, moldings, and laminates, especially those showing enhanced flow with retention of mechanical and adhesive properties. It can be used in the aerospace industry, for example, in joining metals to metals or metals to composite structures. One area of application is in the manufacture of lighter and stronger aircraft and spacecraft structures.

Pratt, J. Richard↗

New addition curing polyimides

In an attempt to improve the thermal-oxidative stability (TOS) of PMR-type polymers, the use of 1,4-phenylenebis (phenylmaleic anhydride) PPMA, was evaluated. Two series of nadic end-capped addition curing polyimides were prepared by imidizing PPMA with either 4,4'-methylene dianiline or p-phenylenediamine. The first resulted in improved solubility and increased resin flow while the latter yielded a compression molded neat resin sample with a T(sub g) of 408 C, close to 70 C higher than PME-15. The performance of these materials in long term weight loss studies was below that of PMR-15, independent of post-cure conditions. These results can be rationalized in terms of the thermal lability of the pendant phenyl groups and the incomplete imidization of the sterically congested PPMA. The preparation of model compounds as well as future research directions are discussed.

Frimer, Aryeh A.↗

Structure-property study of keto-ether polyimides

As part of an on-going effort to develop an understanding of how changes in the chemical structure affect polymer properties, an empirical study was performed on polyimides containing only ether and/or carbonyl connecting groups in the polymer backbone. During the past two decades the structure-property relationships in linear aromatic polyimides have been extensively investigated. More recently, work has been performed to study the effect of isomeric attachment of keto-ether polyimides on properties such as glass transition temperature and solubility. However, little work has been reported on the relation of polyimide structure to mechanical properties. The purpose of this study was to determine the effect of structural changes in the backbone of keto-ether polyimides on their mechanical properties, specifically, unoriented thin film tensile properties. This study was conducted in two stages. The purpose of the initial stage was to examine the physical and mechanical properties of a representative group (four) of polyimide systems to determine the optimum solvent and cure cycle requirements. These optimum conditions were then utilized in the second stage to prepare films of keto-ether polyimides which were evaluated for mechanical and physical properties. All of the polyimides were prepared using isomers of oxydianiline (ODA) and diaminobenzophenone (DABP) in combination with 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) and 4,4'-oxydiphthalic anhydride (ODPA).

Dezern, James F.↗

Processing for maximizing the level of crystallinity in linear aromatic polyimides

The process of the present invention includes first treating a polyamide acid (such as LARC-TPI polyamide acid) in an amide-containing solvent (such as N-methyl pyrrolidone) with an aprotic organic base (such as triethylamine), followed by dehydrating with an organic dehydrating agent (such as acetic anhydride). The level of crystallinity in the linear aromatic polyimide so produced is maximized without any degradation in the molecular weight thereof.

St.clair, Terry L.↗

Imide/arylene ether copolymers

Imide/arylene ether block copolymers are prepared by reacting anhydride terminated poly(amic acids) with amine terminated poly(arylene ethers) in polar aprotic solvents and by chemically or thermally cyclodehydrating the resulting intermediate poly(amic acids). The resulting block copolymers have one glass transition temperature or two, depending upon the particular structure and/or the compatibility of the block units. Most of these block copolymers form tough, solvent resistant films with high tensile properties.

Jensen, Brian J.↗

Oxygen plasma resistant phosphine oxide containing imide/arylene copolymers

A series of oxygen plasma resistant imide/arylene ether copolymers were prepared by reacting anhydride-terminated poly(amide acids) and amine-terminated polyarylene ethers containing phosphine oxide units. Inherent viscosities for these copolymers ranged from 0.42 to 0.80 dL/g. After curing, the resulting copolymers had glass transition temperatures ranging from 224 C to 228 C. Solution cast films of the block copolymers were tough and flexible with tensile strength, tensile moduli, and elongation at break up to 16.1 ksi, 439 ksi, and 23 percent, respectively at 25 C and 9.1 ksi, 308 ksi and 97 percent, respectively at 150 C. The copolymers show a significant improvement in resistance to oxygen plasma when compared to the commercial polyimide Kapton. The imide/arylene ether copolymers containing phosphine oxide units are suitable as coatings, films, adhesives, and composite matrices.

Jensen, Brian J.↗

Polyimides with improved compression moldability

The semicrystalline polyimide prepared by reaction of 3,3',4,4' benzophenonetetracarboxylic (BTDA) and 1,3-bis(4-aminophenoxy 4' benzoyl) benzene (1,3-BABB) is modified so that it can be more readily processed to form adhesive bonds, moldings, and composites. The stoichiometric ratio of the two monomers, BTDA and 1,3-BABB is controlled so that the intermediate polyamide acid is of a calculated molecular weight. A polyimide acid with excess anhydride groups is then reacted with the stoichiometrically required amount of monofunctional aromatic or aliphatic amine required for complete endcapping. The stoichiometrically offset, encapped polyimide is processed at lower temperatures and pressures than the unmodified high molecular weight polyimide with the same repeat unit, and exhibits an improved melt stability.

Hergenrother, Paul M.↗

Benzonorbornadiene end caps for PMR resins

Several ortho-disubstituted benzonorbornadiene derivatives are described. These molecules contain acid, ester, or anhydride functionality permitting their use as end caps in PMR (polymerization of monomer reactants) polyimide systems. The replacement of the currently used norbornenyl end caps with benzonorbornadienyl end caps affords resins of increased aromatic content. It also allows evaluation of some mechanistic aspects of PMR cross-linking. Initial testing of N-phenylimide model compounds and of actual resin formulations using the benzonorbornadienyl end cap reveals that they undergo efficient thermal crosslinking to give oligomers with physical properties and thermal stability comparable to commercial norbornene-end-capped PMR systems.

Panigot, Michael J.↗

Characterization of a soluble polyimide

The solid phase thermal imidization of a soluble 4,4-prime-bis (3,4-dicarboxyphynoxy) diphenyl sulfide dianhydride plus 2,2-bis 4-(4-aminophenoxyl)phenyl hexafluoropropane (BDSDA-BDAF) polyimide precursor staged between 40 and 325 C was characterized by gel permeation chromatography, inherent viscosity, and number average molecular weight measurements. The information obtained indicated that this polyamic acid experienced an initial reduction in molecular weight during cure before achieving its ultimate molecular weight as a polyimide. The event was most likely related to the development of an anhydride band that appeared in the infrared spectrum around 1850/cm as the material cured. Correlation through infrared spectroscopy with a previous study dealing with several common, but insoluble, polyimide precursors, suggested that polyimides, in general, exhibit this trend in molecular weight behavior.

Young, Philip R.↗

A thermoplastic copolyimide

A copolyimide, STPI/LARC, was prepared from the reaction of 3,3'4,4'-benzophenonetetracarboxylic dianhydride (BTDA), equimolar quantities of m-phenylenediamine and 4,4'-oxydianiline, and a small amount of phthalic anhydride to control the molecular weight. The processability and adhesive properties of STPI/LARC were compared to those of a commercially available form of LARC-TPI. LARC-TPI, a thermoplastic polyimide, from the reaction of BTDA and 3,3'-diaminobenzophenone, had previously shown promise as a high temperature structural adhesive. Lap shear specimens were fabricated using adhesive tape prepared from each of the two polymers. Lap shear tests were performed at room temperature, 177 C, and 204 C before and after exposure to a 72-hour water-boil and to aging at 204 C.

Progar, D. J.↗