Soluble, thermally-stable aromatic polyimides
Solubility of aromatic polyimides in organic solvents is increased by additions of dianhydride monomers and substituted diamines. Thermal stability of polymers is retained.
SEARCH · Engineering Papers
Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.
Solubility of aromatic polyimides in organic solvents is increased by additions of dianhydride monomers and substituted diamines. Thermal stability of polymers is retained.
Addition polyimide for composite materials is based on liquid monomers and has significant advantages over most existing high-temperature resins. Essentially solventless prepreg has improved drape, tack.
Process economically separates gold from goldized polyimide film and other nonmetallic scrap without hazards of conventional processes. Technique uses nitric acid to destroy nonmetallic material, leaving gold intact.
Conducting layers of multi-layered thin-film ferroelectric device, such as is used in liquid crystal/ferroelectric display, can be electrically isolated using thin-film layer of polyimide. Ease of application and high electrical-breakdown strength allow dependable and economical means of providing dielectric for other thin-film microelectronic devices.
An acoustic-ultrasonic method is described that was successful in ranking unidirectional graphite-polyimide composite specimens according to variations in interlaminar shear strength. Using this method, a quantity termed the stress wave factor was determined. It was found that this factor increases directly with interlaminar shear strength. The key variables in this investigation were composite density, fiber weight fraction, and void content. The stress wave factor and other ultrasonic factors that were studied were found to provide a powerful means for nondestructive evaluation of mechanical strength properties.
A procedure was developed for fabricating short-fiber HTS graphite and NR150B2 polyimide resin into an isogrid configuration. After fabrication, the panels were subjected to structural analysis and testing. The testing program is described.
Friction and wear experiments conducted on polyimide films bonded to 440 C stainless steel disks indicated that a wear transition (from high wear to low wear) accompanied the friction transition (from high friction to low friction). The transition was found to be atmospheric dependent as well as temperature dependent. Wear rate calculations indicated that, at temperatures above the transition, wear could be up to 600 times less than at temperatures below the transition. Transfer to metallic riders was also investigated and found to be considerably different at temperatures above and below the transition.
A new addition polyimide, LaRC-160, based on liquid monomers has been prepared. The essentially solventless prepreg retains good drape and tack. Unidirectional HT-S composites were fabricated and tested before and after aging at temperatures between 505 K and 589 K (450 F and 600 F). Excellent retention of mechanical properties was realized after 2000 hours at 547 K (525 F). This material should be a candidate for solventless prepregging due to the liquid nature of the monomeric mixture.
The properties of laminated composite materials are strongly affected by many fabrication variables including temperature, time, and molding pressure. It is therefore necessary to have reliable quality control tests to check the properties of manufactured materials. The short-beam shear test is used widely by both manufacturers and researchers as a quality control test in the production of materials and development of new material systems. There are, however, several limitations to the standard test method. This paper presents the results of short-beam shear tests on graphite-polyimide laminates and reports on stiffness-strength relationships and nondestructive evaluation methods which aid in the interpretation of the test data.
Approach results in synthesis of addition polyimide adhesives with exceptional high temperature capabilities that show excellent potential for bonding titanium metal, polyimide/graphite composites, and combinations of these materials. Adhesives compatible with materials used in high performance aircraft and spacecraft structures also prove highly desirable in many other applications involving similar adherents.
Thin polyimide films are given excellent antistatic properties even at high temperature by low-level loading with lithium salts. Extremely hygroscopic, these salts absorb a layer of atmospheric water that provides conductive paths allowing charges to dissipate.
A low density polyimide foam material was tested in an arc tunnel to determine its potential for heat shield application on aerospace vehicles. The results show that the material has some reuse potential at surface temperatures as high as 750 K. When a black refractory paint was applied to the surface of the material, the surface recession was negligible at 750 K. An analytical thermal conductivity was derived for this material which, combined with measured thermal property values, can be used to make preliminary design thickness calculations for heat shield applications.
The addition polyimide, LARC-160, which was originally synthesized from low cost liquid monomers as a laminating resin in ethanol, was prepared as a solventless, high viscosity, neat liquid resin. The resin was processed by hot-melt coating techniques into graphite prepreg with excellent tack and drape. Comparable data on graphite reinforced laminates made from solvent-coated and various hot-melt coated prepreg were generated. LARC-160, because of its liquid nature, can be easily autoclave processed to produce low void laminates. Liquid chromatographic fingerprints indicate good reaction control on resin scale ups. Minor changes in monomer ratios were also made to improve the thermal aging performance of graphite laminates.
Infrared spectroscopy and differential scanning calorimetry were employed to study the imidization and crosslinking kinetics of norbornenyl-capped, addition-type polyimide resins (designated PMR for polymerization of monomer reactants). The spectral and thermal analyses were performed on resin specimens which had been isothermally aged at temperatures appropriate for imidization (120 to 204 C) and crosslinking (275 to 325 C). Imidization occurs rapidly (approximately 0.01/min) at short times, while at times longer than approximately 0.5 hour, the rate decreases significantly (approximately 0.0001/min). The crosslinking reaction exhibits first order kinetics during the initial portion of the reaction and its rate appears to be limited by the reversion of the norbornenyl Diels-Alder adduct. The total heat evolved per mole of endcap during crosslinking shows an inverse dependence on the molecular weight of the imide prepolymers. This reflects the effect of endcap dilution and decreased mobility of the larger oligomers.
Commercially obtained PMR-15 polyimide prepregs with S-glass and graphite fiber reinforcements were evaluated along with in-house prepared glass and graphite cloth PMR 2 materials. A novel autoclave approach was conceived and used to demonstrate that both the PMR systems respond to 1.4 MPa (200 psi) autoclave pressures to produce void free composites equivalent to die molded laminates. Isothermal gravimetric analysis and subsequent mechanical property tests indicated that the PMR 2 system was significantly superior in thermo-oxidative stability, and that S-glass reinforcements may contribute to the accelerated degradation of composites at 316 C (600 F) when compared to graphite fiber reinforced composites. Fully reversed bending fatigue experiments were conducted with a type of fixture unused for organic matrix composites. These studies indicated that the graphite fiber composites were clearly superior in fatigue resistance to the glass fiber reinforced material and that PMR matrix composite systems yield performance of the same order as composite materials employing other families of matrices.
Oscillating, plain spherical bearings with graphite-fiber-reinforced polyimide (GFRPI) liners were tested for friction and wear from 25 to 315 C. A condensation polymer was compared with an addition polymer, and a high-modulus fiber was compared with a lower cost, low-modulus fiber. All polymer-fiber combinations gave friction coefficients from 0.05 to 0.18 and low wear. Adding CdO and CdI2 reduced the wear of degassed bearings in dry air. These additives were not needed when the bearing liners contained adsorbed moisture. Although, at 25 C, MoS2 reduced the friction and wear of the base composite at unit loads above 70,000,000 N/m squared (10,000 psi), it had no beneficial effect at lighter loads.
Plain spherical bearings with molded liners of self-lubricating graphite fiber-polyimide composite were developed and their dynamic load capacities were determined. Liners were prepared by transfer molding a prepolymer resin-fiber mix into the space between the ball and outer race, the completing polymerization under heat and pressure. Bearing dynamic load capacities were in excess of 140 MPa (20,000 psi) from room temperature to 260 C and about 70 MPa (10,000 psi) at 320 C. Friction coefficients were about 0.20 at room temperatures and light loads and tended to decrease with increasing temperatures and loads to about 0.15. Thermal expansion of the liner at uniform bearing temperatures of 200 C or higher produced a bearing preload which could be alleviated by providing an initial internal diametral clearance of 0.05 to 0.10 mm.
Polyimide membranes of a thickness range from under 0.01 micron m to greater than 1 micron m can be produced at an estimated cost of 50 cents per sq m (plus the cost of the polymer). The polymer of interest is dissolved in a solvent which is solube in water. The polymer or casting solution is allowed to flow down an inclined ramp onto a water surface where a pool of floating polymer develops. The solvent dissolves into the water lowering the surface tension of the water on equently, the contact angle of the polymer pool is very low and the edge of the pool is very thin. The solvent dissolves from this thin region too rapidly to be replenished from the bulk of the pool and a solid polymer film forms. Firm formation is rapid and spontaneous and the film spreads out unaided, many feet from the leading edge of the pool. The driving force for this process is the exothermic solution of the organic solvent from the polymer solution into the water.