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NASA NTRS1989

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↗

NASA NTRS1977

Effect of processing parameters on autoclaved PMR polyimide composites

A study was conducted to determine the effect of processing parameters on the processability and properties of autoclaved fiber reinforced PMR polyimide composites. Composites were fabricated from commercially available graphite fabric and glass fabric PMR polyimide prepreg materials. Process parameters investigated included degree of resin advancement, heating rate, and cure pressure. Composites were inspected for porosity by ultrasonic C scan and photomicrographic examination. Processing characteristics for each set of process parameters and the effect of process parameters on composite mechanical properties at room temperature and 600 F are described.

Vannucci, R. D.↗

NASA NTRS1977

Effect of processing parameters on autoclaved PMR polyimide composites

A study was conducted to determine the effect of processing parameters on the processability and properties of autoclaved fiber reinforced PMR polyimide composites. Composites were fabricated from commercially available graphite fabric and glass fabric PMR polyimide prepreg materials. Process parameters investigated included degree of resin advancement, heating rate, and cure pressure. Composites were inspected for porosity by ultrasonic 'C' scan and photomicrographic examination. Processing characteristics for each set of process parameters and the effect of process parameters on composite mechanical properties at room temperature and 600 F are described.

Vannucci, R. D.↗

NASA NTRS1977

Ultrasonic evaluation of the strength of unidirectional graphite-polyimide composites

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.

Vary, A.↗

NASA NTRS1969

Titanium reinforced boron-polyimide composite

Processing techniques for boron polyimide prepreg were developed whereby composites could be molded under vacuum bag pressure only. A post-cure cycle was developed which resulted in no loss in room temperature mechanical properties of the composite at any time during up to 16 hours at 650 F. A design utilizing laminated titanium foil was developed to achieve a smooth transition of load from the titanium attachment points into the boron-reinforced body of the structure. The box beam test article was subjected to combined bending and torsional loads while exposed to 650 F. Loads were applied incrementally until failure occurred at 83% design limit load.

Clark, G. A.↗

NASA NTRS1980

Characterization of PMR-15 polyimide composition in thermo-oxidatively exposed graphite fiber composites

The contributions of individual resin components to total resin weight loss in 600 F air aged Celion 6000/PMR-15 polyimide composites were determined from the overall resin weight loss in the composite by chemically separating the PMR-15 matrix resin into its monomeric components. The individual resin components were also analyzed by spectroscopic techniques in order to elucidate curing and degradation mechanisms of the PMR-15 matrix resin. The isothermal weight loss of the individual resin components during prolonged 600 F thermo-oxidative aging of the composite was correlated to the changes observed in the Fourier Transform infrared spectra and Fourier Transform nuclear magnetic resonance spectra of the individual resin components. The correlation was used to identify the molecular site of the thermo-oxidative changes in PMR-15 polyimide matrix resin during 600 F curing the prolonged 600 F thermo-oxidative aging.

Alston, W. B.↗

NASA NTRS2014

Evaluation of RTM370 Polyimide Composites by Resin Film Infusion (RFI)

RTM370 imide oligomer based on 2,3,3',4'-biphenyl dianhydride (a-BPDA), 3,4'-oxydianiline (3,4'-ODA) and terminated with the 4-phenylethynylphthalic (PEPA) endcap has been shown to exhibit a low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h and a high cured glass-transition temperature (Tg) of 370 C. RTM370 resin has been successfully infused into fiberglass-stitched T650-35 carbon-fabric preforms (ranged from 3- to 6-mm thick) by resin film infusion (RFI). The resulting composite panels were inspected by ultrasonic C-scan and by photomicrographs before and after post-curing as a quality control. Mechanical tests such as unnotched compression (UNC), open-hole compression (OHC), and short-beam shear strength (SBS) at ambient and elevated temperatures were performed before and after isothermal aging at 288 C for 1000 h to assess high-temperature performance. Thermal cycling of RTM370 stitched composites was also conducted from -54 C to 288 C for up to 1600 cycles to evaluate the microcrack resistance of RTM370 polyimide composites fabricated by RFI.

Polyimide↗

NASA NTRS1983

The effect of a coating on the thermo-oxidative stability of Celion 6000 graphite fiber/PMR 15 polyimide composites

The thermooxidative stability in air at 316 C of unidirectional, uncoated and aluminum-coated Celion 6000 graphite fiber/PMR 15 polyimide composites has been determined for exposure times up to nominally 2000 h. Comparison of the weight loss data and microstructural integrity reveals that a thin aluminum-foil coating can provide significant protection from oxidation. A quantitative description of the average depth of the reaction zone and the maximum length of cracks produced during oxidation as a function of time in uncoated Celion 6000/PMR 15 are given.

Hurwitz, F. I.↗

NASA NTRS1991

Dynamic mechanical properties of N-phenylnadimide modified PMR polyimide composites

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.

Pater, Ruth H.↗

NASA NTRS1984

PMR polyimide composites for aerospace applications

A novel class of addition-type polyimides has been developed in response to the need for high temperature polymers with improved processability. The new plastic materials are known as PMR (for in situ polymerization of monomer reactants) polyimides. The highly processable PMR polyimides have made it possible to realize much of the potential of high temperature resistant polymers. Monomer reactant combinations for several PMR polyimides have been identified. The present investigation is concerned with a review of the current status of PMR polyimides. Attention is given to details of PMR polyimide chemistry, the processing of composites and their properties, and aerospace applications of PMR-15 polyimide composites.

Serafini, T. T.↗

NASA NTRS1972

Graphite fiber polyimide composites for spherical bearings to 340 C (650 F)

Journal bearings with self-alining spherical elements of graphite-fiber-reinforced-polyimide composites were tested from 24 to 340 C (75 to 650 F) at unit loads up to 3.5 times 10 to the 7th power N/sq m (5000 psi). The journal oscillated in the cylindrical bore of the composite element + or - 15 deg at 1 hertz. Outer races and journals were metal hardened of Rockwell C-32 and finished to 10 to the minus 7th power m. A 45 wt. percent graphite-fiber composite gave low friction (0.08 to 0.13), low wear, and almost no plastic deformation under any of the test conditions. Composites with 15 and 25 wt. percent graphite fiber failed by plastic deformation at 315 C (600 F) and 3.5 times 10 to the 7th power N/sq m (5000 psi). A composite with 60 wt. percent graphite fiber failed by brittle fracture under the same conditions, but had very low friction coefficients (0.05 to 0.10) and may be a good bearing material at lighter loads.

Sliney, H. E.↗

NASA NTRS1998

Long Term Degradation of Polyimide Composites

The durability of polymer matrix composites exposed to harsh environments is a major concern. Surface degradation and damage are observed in polyimide composites used in air at 125-300 C. It is believed that diffusion of oxygen into the material and oxidative chemical reactions are responsible. Previous work has characterized and modeled diffusion behavior, and thermogravimetric analyses (TGAS) have been carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. However, the model developed using these data did not successfully extrapolate TGA data down to conditions seen in service. A test program that focuses on lower temperatures and makes use of isothermal tests was undertaken to achieve a better understanding of the degradation reactions under use conditions. A new, low-cost technique was developed to collect chemical degradation data for isothermal tests lasting over 200 hours in the temperature range 125-300 C. Results indicate complex behavior not captured by the previous model, including the presence of weight-adding reactions. Weight gain reactions dominated in the 125-225 C temperature range, while weight loss reactions dominated beyond 225 C. The data obtained from isothermal tests and earlier TGAs is used to develop an advanced model of the material behavior.

Patekar, Kaustubh A.↗

NASA NTRS1972

Development and evaluation of graphite and boron polyimide composites.

This paper covers the development and evaluation of the HT-S/710 graphite/polyimide system and initial evaluations of high modulus graphite and boron reinforced polyimide systems. Detail design properties of the HT-S/710 graphite/polyimide systems, test results of test sheet stringer components, and initial test evaluations of high modulus graphite and boron reinforced polyimide composites are presented. Preliminary design applications utilizing the basic processing and design data from this development program are presented as to their utilization in aircraft and space applications.

Scheck, W. G.↗

NASA NTRS1991

Crosslinking-property relationships in PMR polyimide composites. I

The effect of the crosslink density of the matrix on physical and mechanical properties of a graphite-fiber-reinforced PMR (for polymerization of monomer reactants) polyimide composites during isothermal aging was investigated in experiments where unidirectional composite specimens of Celion 6000/PMR-P1 were isothermally exposed at 288 C in air for various time periods up to 5000 hrs. It was found that, as the crosslink density increased, the glass transition temperature, density, and elevated-temperature interlaminar shear strength of a composite increased, while the initial moisture absorption and the coefficient of thermal expansion decreased. However, after reaching the highest possible matrix crosslink density, several of the composite properties began to deteriorate rapidly.

Pater, R. H.↗

NASA NTRS1980

Properties of PMR Polyimide composites made with improved high strength graphite fibers

High strength, intermediate modulus graphite fibers were obtained from various commercial suppliers, and were used to fabricate PMR-15 and PMR-2 polyimide composites. The effects of the improved high strength graphite fibers on composite properties after exposure in air at 600 F were investigated. Two of the improved fibers were found to have an adverse effect on the long term performance of PMR composites. The influence of various factors such as fiber physical properties, surface morphology and chemical composition were also examined.

Vannucci, R. D.↗

NASA NTRS1978

Fiber reinforced PMR polyimide composites

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.

Cavano, P. J.↗

NASA NTRS1980

Properties of PMR polyimide composites made with improved high strength graphite fibers

Recent graphite fiber developments have resulted in high strength, intermediate modulus graphite fibers having improved thermo-oxidative resistance. These improved fibers, obtained from various commercial suppliers, were used to fabricate PMR-15 and PMR-11 polyimide composites. Studies were performed to investigate the effects of the improved high strength graphite fibers on composite properties after exposure in air at 600 F. The use of the more oxidatively resistant fibers did not result in improved performance at 600 F. Two of the improved fibers were found to have an adverse effect on the long-term performance of PMR composites. The influence of various factors such as fiber physical properties, surface morphology and chemical composition are also discussed.

Vannucci, R. D.↗

NASA NTRS1977

The correlation of ultrasonic attenuation and shear strength in graphite-polyimide composites

The buffer rod technique for measuring attenuation in thin specimens is modified here to apply to specimens having intermediate thicknesses and high attenuation. The described procedure, which requires only one accessible surface of the material, was used to determine the initial attenuation values of ultrasonic waves in short beam shear specimens of graphite-polyimide composite material. It is shown that there is good correlation between the initial attenuation values and the shear strengths of the specimens determined by the standard short beam shear test method. The modified ultrasonic buffer block technique offers much potential for service as a quantitative, nondestructive, quality assurance test for composite materials.

Hayford, D. T.↗