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Two aromatic polyimides and an aromatic polyamide-imide were tested in single edge notched tension. Fracture toughnesses, normalized to 25 micron film thickness ranged from 1.65 to 5.4 MPa m sup 1/2. LARC-TPI, a thermoplastic polyimide, showed evidence of crazing ahead of a growing crack whereas the other materials formed a shear yielded zone.
A high-temperature stable, optically transparent, low dielectric aromatic polyimide is prepared by chemically combining equimolar quantities of an aromatic dianhydride reactant and an aromatic diamine reactant, which are selected so that one reactant contains at least one Si(CH3)2 group in its molecular structure, and the other reactant contains at least one -CF3 group in its molecular structure. The reactants are chemically combined in a solvent medium to form a solution of a high molecular weight polyamic acid, which is then converted to the corresponding polyimide.
NASA-Langley studies of polymer structure-property relationships have led to the development of a method for the reduction of dielectric constants in polyimides through chemical alterations of polymer backbone composition to reduce chain-chain electronic interactions, as well as through the incorporation of fluorine atoms into the polymer molecular structure. Still-greater dielectric constant reductions are obtainable by means of a physical incorporation of diamic acid additives into these low-dielectric polyimide systems; the resulting thermoplastic resins are applicable to polymer matrices for composite structural materials.
As part of a program on high performance/high temperature structural resins for aerospace applications, work was performed with a new semi-crystalline polyimide (LARC-CPI) to improve the compression moldability while retaining high mechanical properties and thermooxidative stability. Various molecular weight versions of LARC-CPI polyamide acid were prepared, end-capped with different groups, converted to polyimide and evaluated for film properties, thermooxidative stability and melt flow. One controlled molecular weight, end-capped version of LARC-CPI was evaluated more comprehensively in adhesive and composite work and exhibited good compression moldability, reasonable crystallization rates and high mechanical properties.
Polyimide matrix composites were fabricated from unidirectional unsized AS-4 carbon fiber and a doped 1:1 blend of two polyimides: PISO2 and LARC-TPI. To enhance melt flow properties, the molecular weight of the PISO2 was controlled by end-capping with phthalic anhydride and addition of 5 percent by weight p-phenylenediamine-phthalic anhydride bisamic acid dopant. Prepreg was drum-wound using a diglyme slurry comprised of the soluble polyamideacid of PISO2, the soluble bisamideacid of the dopant, and the insoluble imidized LARC-TPI powder. Melt flow studies with a rotary rheometer and parallel plate plastometer on neat resin and prepreg helped develop an optimum cure cycle. Composite mechanical properties at room and elevated temperatures, dry and moisture-saturated, were evaluated, including short beam shear strength and flexure, tensile, shear, and compression properties. Two 18 x 24-inch skin-stringer panels were fabricated, one of which was tested in compression to failure.
Improved wet-spinning process makes aromatic polyamic acid fibers containing no voids, and converts to polyimide fibers also free of voids. Elimination of voids found to improve tensile strength and other tensile properties. Improved polyimide fibers prove useful in protective clothing, sealing materials, filters for harsh chemical and/or thermal environments, and other applications taking advantage of excellent chemical resistance, high thermal stability, and good tensile properties.
Polyimide resins having improved thermo-oxidative stability are provided having aromatic vinyl end-caps. The polyimides are prepared by the reaction of a mixture of monomers comprising (1) a diamine, (2) an ester of tetracarboxylic acid and (3) an aromatic vinyl compound in a molar ratio of 1:2:3 of n: (n + 1):2 when the aromatic vinyl compound contains nitrogen and in a ratio of (n + 1):n:2 when the aromatic vinyl compound does not contain nitrogen, wherein n ranges from about 5 to about 20.
Composite materials with matrices of tough, thermoplastic aromatic polyimides are obtained by blending semi-crystalline polyimide powders with polyamic acid solutions to form slurries, which are used in turn to prepare prepregs, the consolidation of which into finished composites is characterized by excellent melt flow during processing.
A new thermoplastic polyimide designated LaRC-I-TPI has been prepared from 4,4'-isophthaloyldiphthalic anhydride (IDPA) and 1,3-phenylenediamine (m-PDA), phthalic anhydride endcapped or unendcapped. It is closely related to the well-known commercial LaRC-TPI. A survey of the synthesis and some thermal, film, adhesive, fracture toughness, and composite properties of this new polyimide is presented. While both materials have similar properties at comparable stages of development, LaRC-I-TPI should be less expensive to manufacture as a result of the use of lower cost readily available monomers.
Temperature-frequency dependence of alpha, beta, and gamma transitions was determined using a Rheometrics dynamic spectrometer on a series of unidirectional Celion 6000/N-phenylnadimide (PN) modified PMR polyimide composites. The objective was to see if any correlations exist between crosslinked network structure and dynamic mechanical properties. Variation in crosslinked network structures was achieved by altering the polyimide formulation through addition of various quantities of PN into the standard PMR-15 composition. As a control, PMR-15 composite system exhibited well-defined alpha, beta, and gamma transitions in the regions of 360, 100, and -120 C, respectively. Their activation energies were estimated to be 232, 60, and 14 kcal/mole, respectively. Increasing the amount of PN concentration caused lowering of the activation energies of the three relaxations, a decrease of the glass transition temperature, and increasing intensities of the three damping peaks, compared to the control PMR-15 counterpart. These dynamic mechanical responses were in agreement with formation of a more flexible copolymer from PN and PMR-15 prepolymer.
Consideration is given to an approach to provide a semi-IPN in which two constituent materials have nearly the same chemical structure and polymer chain length. A reactive endcapped LARC-TPI polyamic acid having a formulated molecular weight of 20,000 is prepared and then combined with various quantities of a commercial LARC-TPI polyamic acid solution. The polyimide films of semi-IPNs are tested along with two constituent materials. The physical and mechanical properties of the polyimide films are presented. The applicability of using this approach to minimize phase separation and to maximize long-term phase stability is discussed. The concept of controlling morphology by chemistry is proven for providing LARC-TPI based semi-2-IPNs. A very long chain LARC-TPI endcapped with a nadic group exhibits physical properties almost identical to unendcapped LARC-TPI.
Polyimides of new class, known as polyetherimides, used for composites and castings. Study undertaken to compare effects of electron radiation, in doses expected for 30-year missions in geosynchronous orbit, on molecular structures and tensile properties of two commercially available polyimides: polypyromellitimide and polyetherimide. Findings helpful in development of new polymers that endure radiation, leading to synthesis of polymers not having methyl groups or other moieties that are sources of hydrogen, inhibiting self-mending. Significance of study for polymer industry relating to structures in outer space considerable.
An assembly of an article and a polyimide composition is prepared. The assembly resists dimensional change, delamination, or debonding when exposed to changes to temperature. An article is provided. A polyamic acid solution which yields a polyimide having a low coefficient of thermal expansion (CTE) was prepared. Equimolar quantities of an aromatic diamine and an aromatic dianhydride were reacted in a solvent medium to form a polyamic acid solution. A metal ion containing additive was added to the solution. Examples of this additive are: TbCl3, DyCl3, ErCl3, TmCl3, Al(C5H7O2)3, and Er2S3. The polyamic acid solution was imidized and is combined with the article to form the assembly.
Kapton H (DuPont Trademark) polyimide specimens exposed to the low earth (LEO) space environment suffered significant weathering with surface erosions of approximately 8.0 microns. Despite these effects, no significant changes in bulk chemistry were observed. X-ray photoelectron spectroscopy (XPS) was used to determine local changes induced from approximately 25 percent in 1980 vintage ground control specimens to nearly 53 percent in space exposed specimens. The greatest increase was observed for the divalent oxygen moieties, although a slight increase in carbonyl oxygen was also measured. Furthermore, the chemical shifts of all XPS peaks of space-exposed Kapton are shifted to higher energy. This is consistent with a higher oxidation state of the space exposed surface. Finally, space exposed specimens had distinct silicon peaks (2p 100 eV and 2s 149 eV) in their XPS spectra in agreement with widespread reports of silicon contamination throughout the LDEF satellite. These results are discussed in terms of surface reactivity of the polyimide exposed to the LEO environment and the chemical nature of contaminants deposited on flight surfaces due to satellite outgassing.
New polyimides synthesized from reactions of aromatic hexafluoroisopropyl dianhydrides with asymmetric amide diamines. Soluble to extent of at least 10 percent by weight at temperature of about 25 degrees C in common amide solvents such as N-methylpyrrolidone, N,N-dimethylacetamide, and N,N-dimethylformamide. Polyimides form tough, flexible films, coatings, and moldings. Glass-transition temperatures ranged from 300 to 365 degrees C, and crystalline melting temperatures observed between 543 and 603 degrees C. Display excellent physical, chemical, and electrical properties. Useful as adhesives, laminating resins, fibers, coatings for electrical and decorative purposes, films, wire enamels, and molding compounds.
Aromatic polyimides are a class of polymers that show remarkable thermal stability, strength, and toughness. These properties make them attractive candidates for use in high-performance carbon fiber composites for airborne and spaceborne structural components. Our research centered on the development of an understanding of the underlying process of crystallite formation in a particular class of aryl polyimides for which there are some x-ray crystallographic data available. The ultimate aim of the project is to be able to develop a model sufficiently flexible to be able, on the basis of the chemical structure of a polymer in this class, to predict: (1) whether it will be prone to form crystallites; (2) crystallographic features of the crystallites; and (3) synthesis and/or processing conditions that will be favorable or unfavorable to crystallite formation. This will provide guidance to the laboratory chemists in their choice of candidate polymers and processing methods.
High performance, thermooxidatively stable polyimides are prepared by reacting aromatic diamines with pendant trifluoromethyl groups and dianhydrides in an amide solvent to form a poly(amic acid), followed by cyclizing the poly(amic acid) to form the corresponding polyimide.
A high temperature stable, highly optically transparent-to-colorless, low dielectic linear aromatic polyimide is prepared by reacting an aromatic diamine with 3,3'bis (3,4-dicarboxyphenoxy) diphenylmethane dianhydride in an amide solvent to form a linear aromatic polyamic acid. This polyamic acid is then cyclized to form the corresponding polyimide.