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Polyimide foam products having greatly improved burn-through and flame-spread resistance are prepared by the reaction of aromatic polyisocyanates with aromatic dianhydrides in the presence of metallic salts of octoic acid. The salts, for example stannous octoate, ferric octoate and aluminum octoate, favor the formation of imide linkages at the expense of other possible reactions.
Results of an experimental program to develop several types of graphite/polyimide (GR/PI) bonded and bolted joints for lightly loaded flight components for advanced space transportation systems and high speed aircraft are presented. Tasks accomplished include: a literature survey; design of static discriminator specimens; design allowables testing; fabrication of test panels and specimens; small specimen testing; and standard joint testing. Detail designs of static discriminator specimens for each of the four major attachment types are presented. Test results are given for the following: (1) transverse tension of Celion 3000/PMR-15 laminate; (2) net tension of a laminate for both a loaded and unloaded bolt hole; (3) comparative testing of bonded and co-cured doublers along with pull-off tests of single and double bonded angles; (4) single lap shear tests, transverse tension and coefficient of thermal expansion tests of A7F (LARC-13 amide-imide modified) adhesive; and (5) tension tests of standard single lap, double lap, and symmetric step lap bonded joints. Also, included are results of a finite element analysis of a single lap bonded composite joint.
A linear thermoplastic polyimide, LARC-TPI, has been characterized and developed for a variety of high-temperature applications. In its fully imidized form, this new material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI is being evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100% void-free laminates for flexible circuit applications. The further development of LARC-TPI as a potential molding powder, composite matrix resin, high-temperature film and fiber will also be discussed.
Standard and advanced bonded joint concepts were evaluated to develop a data base for the design and analysis of advanced composite joints for use at elevated temperatures (561K (550F)). Design concepts for specific joint applications and the fundamental parameters controlling the static strength characteristics of such joints were identified. Test results are presented for rail shear and sandwich beam compression tests and tension tests of moisture conditioned specimens and bonded on "T" sections. Coefficients of thermal expansion data are presented for A7F (LARC 13 Amide-imide modified) adhesion. Static discriminator test results for type 1 and type 2 bonded and bolted preliminary attachment concepts are presented and discussed.
A linear thermoplastic polyimide, LARC-TPI, was characterized and developed for a variety of high temperature applications. In its fully imidized form, this material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI was evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100 void-free laminates for flexible circuit applications. The development of LARC-TPI as a potential molding powder, composite matrix resin, high temperature film and fiber is also discussed.
The development of a class of high-temperature-resistant resins known as PMR polyimides has been reported by Serafini et al. (1972). Serafini and Vannucci (1975) found that the lower formulated molecular weight (FMW) compositions exhibited increased resin flow, but with some sacrifice in elevated temperature thermo-oxidative stability. Vannucci (1977) reported that the resin flow characteristics of the PMR composition having an FMW of 1500 could be varied by controlling the degree of resin advancement or imidization. The current investigation is concerned with an alternative approach to obtain improved flow PMR polyimides without sacrificing the desirable thermo-oxidative characteristics. The new approach is based on the utilization of a chemically compatible flow modifying agent. This agent is N-phenylnadimide (PN). The determination of the processing characteristics and properties of PN modified PMR/Celion 6000 composites is discussed.
A linear thermoplastic polyimide, LARC-TPI, has been characterized and developed for a variety of high-temperature applications. In its fully imidized form, this new material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI is being evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100% void-free laminates for flexible circuit applications. The further development of LARC-TPI as a potential molding powder, composite matrix resin, high-temperature film and fiber is also discussed.
Addition polyimode oligomers have been synthesized from 3,3 prime, 4,4 prime-benzophenone tetracarboxylic acid dianhydride and 3,3 prime-methylenedianiline using a variety of latent crosslinking groups as end-caps. The nominal 1300 molecular weight imide prepolymers were isolated and characterized for solubility in amide, chlorinated and ether solvents, melt-flow and cure properties, glass transition temperature, and thermal stability on heating in an air atmosphere. Adhesive strengths of the polyimides were obtained both at ambient and elevated temperatures before and after aging at 232 C. Properties of the novel addition polyimides were compared to a known nadic end-capped adhesive, LARC-13.
Polymer synthesis programs involve the development of Novel thermoplastics, pseudothermoplastics, and thermosets. These systems are prepared to elucidate structure-property relationships involving thermal capabilities, toughness, processability and environmental stability. Easily processable polyimides, solvent-resistant polysulfones and polyphenylquinoxalines, and tougher high and intermediate temperature polymers were developed. Characterization efforts included high pressure liquid chromatography methodology, the development of toughness tests for fiber reinforced composites, a study of electrical properties of metal ion filled polyimides, and a study of the mutagenicity of aromatic diamines. Also the mechanism of cure/degradation of experimental polymers was studied by rheology, mechanical behavior, separation techniques and spectroscopy. The degradative crosslinking of alkyl-containing polyimides, the separation and identification of crosslinked phenylquinoxalines, the rheological behavior of hot-melt polyimides, and the elucidation of the cure of norbornene endcapped imides were also studied.
The materials, production processes, testing procedures, and repair techniques for composite structures on the Orbiter are reviewed. The Orbiter currently features graphite/epoxy payload bay doors, as well as graphite/polyimide elevons, vertical tail, and aft body flap, which can withstand up to 600 F temperatures. Graphite/polyimide is also being considered for areas of the baseline aluminum structure and the thermal protection system in order to achieve a 20-30% weight reduction, i.e., over 7.5 tons. An analysis of the allowable stresses on FRC imide thermal protection system tiles bonded directly to the structure has shown satisfactory performances in high temperature and cryogenic conditions, although failure modes are yet to be determined. Ultrasonic emissions have been used for defect detection in nondestructive evaluations, together with tension, notch, shear, and compression tests. Field repairs have not been perfected, and require the evolution of high temperature adhesives that are curable under vacuum pressure and heat blankets.
The invention relates to an incombustible resin composition produced by blending a compound with a specific ester bond and imide bond in a combustible resin.
Synthesis, moldability and chloroform, acetone and tricresyl phosphate resistance of 16 polymer compositions are described. These aliphatic heterocyclic polymers include polyimides, polybenzimidazoles, and N-arylenepolybenzimidazoles. A solution condensation (cresol) method to prepare imidized aliphaic polyimides is described. Two polyimides and one polybenzimidazole demonstrate no crazing or cracking during 500 hr exposure to the cited solvents under stress. Modification of one aliphatic polyimide with several aromatic amines suggests that m-phenylenediamine is singular in its behavior to improve the chloroform resistance of that class of polyimides.
The detailed characterization of an experimental thermoplastic polyimidesulfone adhesive based on 3,3 prime-diaminodiphenylsulfone and 3,3 prime,4,4 prime-benzophenone tetracarboxylic dianhydride was studied. Model compounds were also examined. Thermal cyclization of the amide-acid to the imide was studied by a variety of techniques including DSC, TGA, MS, in situ diffuse reflectance-FTIR, and flow mearsurement. Characterizations were continued during the processing of adhesive tapes and the fabrication, bonding, and testing of lap shear specimens. Results provide fundamental insights into the role of cure chemistry, and the effects of residual solvent and volatile produces on processing and performance. These insights and the resulting chemical models should lead to more efficient processing cycles for these and other related thermoplastic adhesive systems.
A method of forming 4,4',4'',4''' -tetraamino phthalocyanines involves reducing 4,4',4'',4''' -tetranitro phthalocyanines, polymerizing the metal tetraamino phthalocyanines with a tetracarboxylic dianhydride (preferably aromatic) or copolymerizing with a tetracarboxylic dianhydride and a diamine (preferably also aromatic) to produce amic acids which are then dehydrocyclized to imides. Thermally and oxidatively stable polymers result which form tough, flexible films, varnishes, adhesives, and fibers.
The effects of electron radiation on Ultem, a polyetherimide were studied for doses from 2 x 10 to the 9th power to 6 x 10 to the 9th power rad. Specimens were studied for tensile property testing and for electron paramagnetic resonance and infrared spectroscopic measurements of molecular structure. A Faraday cup design and a method for remote temperature measurement were developed. The spectroscopic data show that radiation caused dehydrogenation of methyl groups, rupture of main-chain ether linkage, and opening of imide rings, all to form radicals and indicate that the so-formed atomic hydrogen attached to phenyl radicals, but not to phenoxyl radicals, which would have formed hydroxyls. The observed decays of the radiation-generated phenoxyl, gem-dimethyl, and carbonyl radicals were interpreted as a combining of the radicals to form crosslinking. This crosslinking is the probable cause of the major reduction in the elongation of the tensile specimens after irradiation. Subsequent classical solubility tests indicate that the irradiation caused massive crosslinking.
A series of tin-containing polyimide films derived from either 3,3',4,4'-benzophenone tetracarboxylic acid dianhydride or pyromellitic dianhydride and 4,4'-oxydianiline have been synthesized and their electrical properties examined. Highest quality materials (i.e., homogeneous, smooth surface, flexible) with the best electrical properties were doped with either SnCl2.2H2O or (n-Bu)2SnCl2. In all cases, extensive reactivity of the tin dopant with water, air or polyamic acid during imidization is observed. Lowered electrical surface resistivities appear to be correlatable with the presence of surface tin oxide on the film surface.
An in situ diffuse reflectance-Fourier transform infrared technique was developed to determine infrared spectra of graphite fiber prepregs as they were being cured. A bismaleimide, an epoxy, and addition polyimide matrix resin prepregs were studied. An experimental polyimide adhesive was also examined. Samples were positioned on a small heater at the focal point of diffuse reflectance optics and programmed at 15 F/min while FTIR spectra were being scanned, averaged, and stored. An analysis of the resulting spectra provided basic insights into changes in matrix resin molecular structure which accompanied reactions such as imidization and crosslinking. An endo-exothermal isomerization involving reactive end-caps was confirmed for the addition polyimide prepregs. The results of this study contribute to a fundamental understanding of the processing of composites and adhesives. Such understanding will promote the development of more efficient cure cycles.
The polymer program at NASA Langley Research Center involves exploratory studies in polymer science. These include the synthesis of novel polymers and their characterization. Polymer synthesis programs involve the development of novel thermoplastics, pseudothermoplastics, and thermosets. Recent investigations have led to the development of more easily processable polyimides, solvent-resistant polysulfones and polyphenylquinoxalines, and tougher high and intermediate-temperature polymers. Characterization efforts have included high-pressure liquid chromatography methodology, the development of toughness tests for fiber-reinforced composites, a study of electrical properties of metal-ion-filled polyimides, and a study of the mutagenicity of aromatic diamines. Also the mechanism of cure/degradation of experimental polymers has been studied by rheology, mechanical behavior, separation techniques and spectroscopy. Some of these programs have involved the degradation crosslinking of alkyl-containing polyimides, the separation and identification of crosslinked phenylquinoxalines, the rheological behavior of hot-melt polyimides, and the elucidation of the cure of norbornene endcapped imides.