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At least 19 records

Fabrication of LARC 160/NR150B2 hybrid matrix polyimide composites

Graphite-polyimide composite materials exhibit high performance, low weight, and good thermal-oxidative stability, making them promising candidates for Space Shuttle applications. However, no single material is excellent in all respects: processibility, thermal-oxidative stability, toughness, and mechanical properties. This paper describes the development of hybrid matrix composite laminates that combine the attributes of two polyimide resins, NR150B2 and LARC 160, while avoiding their drawbacks. High quality laminates were fabricated from each resin system, and hybrid laminates were successfully co-cured, evaluated, and optimized.

Bergren, O. D.↗

Design Analysis and Thermo-Mechanical Fatigue of a Polyimide Composite for Combustion Chamber Support

Polyimide composites are being evaluated for use in lightweight support structures designed to preserve the ideal flow geometry within thin shell combustion chambers of future space launch propulsion systems. Principles of lightweight design and innovative manufacturing techniques have yielded a sandwich structure with an outer face sheet of carbon fiber polyimide matrix composite. While the continuous carbon fiber enables laminated skin of high specific stiffness; the polyimide matrix materials ensure that the rigidity and durability is maintained at operation temperatures of 316 C. Significant weight savings over all metal support structures are expected. The protypical structure is the result of ongoing collaboration, between Boeing and NASA-GRC seeking to introduce polyimide composites to the harsh environmental and loads familiar to space launch propulsion systems. Design trade analyses were carried out using relevant closed form solutions, approximations for sandwich beams/panels and finite element analysis. Analyses confirm the significant thermal stresses exist when combining materials whose coefficients of thermal expansion (CTEs) differ by a factor of about 10 for materials such as a polymer composite and metallic structures. The ramifications on design and manufacturing alternatives are reviewed and discussed. Due to stringent durability and safety requirements, serious consideration is being given to the synergistic effects of temperature and mechanical loads. The candidate structure operates at 316 C, about 80% of the glass transition temperature T(sub g). Earlier thermomechanical fatigue (TMF) investigations of chopped fiber polyimide composites made this near to T(sub g), showed that cyclic temperature and stress promoted excessive creep damage and strain accumulation. Here it is important to verify that such response is limited in continuous fiber laminates.

Thesken, J. C.↗

Thermal Cycling of Thermal Control Paints on Carbon-Carbon and Carbon-Polyimide Composites

Carbon-carbon composites and carbon-polyimide composites are being considered for space radiator applications owing to their light weight and high thermal conductivity. For those radiator applications where sunlight will impinge on the surface, it will be necessary to apply a white thermal control paint to minimize solar absorptance and enhance infrared emittance. Several currently available white thermal control paints were applied to candidate carbon-carbon and carbon-polyimide composites and were subjected to vacuum thermal cycling in the range of -100 C to +277 C. The optical properties of solar absorptance and infrared emittance were evaluated before and after thermal cycling. In addition, adhesion of the paints was evaluated utilizing a tape test. The test matrix included three composites: resin-derived carbon-carbon and vapor infiltrated carbon-carbon, both reinforced with pitch-based P-120 graphite fibers, and a polyimide composite reinforced with T-650 carbon fibers, and three commercially available white thermal control paints: AZ-93, Z-93-C55, and YB-71P.

Jaworske, Donald A.↗

Electron Beam Exposure of Thermal Control Paints on Carbon-Carbon and Carbon-Polyimide Composites

Carbon-carbon and carbon-polyimide composites are being considered for use as radiator face sheets or fins for space radiator applications. Several traditional white thermal control paints are being considered for the surface of the composite face sheets or fins. One threat to radiator performance is high energy electrons. The durability of the thermal control paints applied to the carbon-carbon and carbon-polyimide composites was evaluated after extended exposure to 4.5 MeV electrons. Electron exposure was conducted under argon utilizing a Mylar(TradeMark) bag enclosure. Solar absorptance and infrared emittance was evaluated before and after exposure to identify optical properties degradation. Adhesion of the paints to the carbon-carbon and carbon-polyimide composite substrates was also of interest. Adhesion was evaluated on pristine and electron beam exposed coupons using a variation of the ASTM D-3359 tape test. Results of the optical properties evaluation and the adhesion tape tests are summarized.

Jaworske, Donald A.↗

Effect of counterface material type and its topography on the tribological properties of polyimide composites

Graphite fiber reinforced polyimide composite pins were slid against seven different counterfaces to determine the effect of material type on the tribological properties of polymer composites. In addition, the effect of sliding a new pin on a pre-established transfer film was investigated. The results indicated that almost a five order of magnitude difference in composite wear rate can occur just by varying the counterface material. An attempt to make all surfaces as smooth as possible was made, but due to differences in material composition this was not possible and a range of surface roughnesses were obtained. The results indicate that the smoother the surface, the lower the composite wear rate; but that small protrusions (not discernible with arithmetic surface roughness measurements) can markedly increase wear rates. A pre-established transfer film improved both run in and steady state wear rates.

Fusaro, R. L.↗

Counterface effects on the tribological properties of polyimide composites

Graphite fiber reinforced polyimide composite pins were slid against seven different counterfaces to determine the effect of material type on the tribological properties of polymer composites. In addition, the effect of sliding a new pin on a pre-established transfer film was investigated. The results indicated that almost a five order of magnitude difference in composite wear rate can occur just by varying the counterface material. An attempt to make all surfaces as smooth as possible was made, but due to differences in material composition this was not possible and a range of surface roughnesses were obtained. The results indicate that the smoother the surface, the lower the composite wear rate; but that small protrusions (not discernible with arithmetic surface roughness measurements) can markedly increase wear rates. A pre-established transfer film improved both run in and steady state wear rates.

Fusaro, Robert L.↗

Processing and Properties of Fiber Reinforced Polymeric Matrix Composites: Processing Robustness of IM7/PETI Polyimide Composites - Part 2

The processability of a phenylethynyl terminated imide (PETI) resin matrix composite was investigated. Unidirectional prepregs were made by coating an N-methylpyrrolidone solution of the amide acid oligomer onto unsized IM7. Two batches of prepregs were used: one was made by NASA in-house, and the other was from an industrial source. The composite processing robustness was investigated with respect to the effect of B-staging conditions, the prepreg shelf life, and the optimal processing window. Rheological measurements indicated that PETI's processability was only slightly affected over a wide range of B-staging temperatures (from 250 C to 300 C). The open hole compression (OHC) strength values were statistically indistinguishable among specimens consolidated using various B-staging conditions. Prepreg rheology and OHC strengths were also found not to be affected by prolonged (i.e., up to 60 days) ambient storage. An optimal processing window was established using response surface methodology. It was found that IM7/PETI composite is more sensitive to the consolidation temperature than to the consolidation pressure. A good consolidation was achievable at 371 C/100 Psi, which yielded an OHC strength of 62 Ksi at room temperature. However, processability declined dramatically at temperatures below 350 C.

Hou, Tan-Hung↗

Analysis of the Effect of Surface Modification on Polyimide Composites Coated with Erosion Resistant Materials

The aim of this research is to enhance performance of composite coatings through modification of graphite-reinforced polyimide composite surfaces prior to metal bond coat/ hard topcoat application for use in the erosive and/or oxidative environments of advanced engines. Graphite reinforced polyimide composites, PMR-15 and PMR-II-50, formed by sheet molding and pre-pregging will be surface treated, overlaid with a bond coat and then coated with WC-Co. The surface treatment will include cleaning, RF plasma or ultraviolet light- ozone etching, and deposition of SiO(x) groups. These surface treatments will be studied in order to investigate and improve adhesion and oxidation resistance. The following panels were provided by NASA-Glenn Research Center(NASA-GRC): Eight compression molded PMR-II-50; 6 x 6 x 0.125 in. Two vacuum-bagged PMR-II-50; 12 x 12 x 0.125 in. Eight compression molded PMR-15; 6 x 6 x 0.125 in. One vacuum-bagged PMR-15; 12 x 12 x 0.125 in. All panels were made using a 12 x 12 in. T650-35 8HS (3K-tow) graphite fabric. A diamond-wafering blade, with deionized water as a cutting fluid, was used to cut PMR-II-50 and PMR-15 panels into 1 x 1 in. pieces for surface tests. The panel edges exhibiting delamination were used for the preliminary surface preparation tests as these would be unsuitable for strength and erosion testing. PMR-15 neat resin samples were also provided by NASA GRC. Surface profiles of the as-received samples were determined using a Dektak III Surface profile measuring system. Two samples of compression molded PMR-II-50 and PMR-15, vacuum-bagged PMR-II-50 and PMR-15 were randomly chosen for surface profile measurement according to ANSI/ASME B46.1. Prior to each measurement, the samples were blasted with compressed air to remove any artifacts. Five 10 mm-long scans were made on each sample. The short and long wavelength cutoff filter values were set at 100 and 1000 m, diamond stylus radius was 12.5 microns. Table 1 is a summary of the arithmetic average roughness (Ra) and waviness (Wa) for the composite surfaces.

Ndalama, Tchinga↗

Tribological properties of graphite-fiber-reinforced, partially fluorinated polyimide composites

Graphite-fiber-reinforced polyimide (GFRPI) composites were formulated from three new partially fluorinated polyimides and three types of graphite fiber. Nine composites were molded into pins and evaluated in a pin-on-disk tribometer. Friction coefficients, wear rates, pin wear surface morphology, and transfer film formation were assessed at 25 and 300 C. Also assessed was the effect of sliding speed on friction. Wear was up to two orders of magnitude lower at 25 C and up to one order of magnitude lower at 300 C than with previously formulated NASA GFRPI composites.

Fusaro, R. L.↗

Tribological properties of graphite-fiber-reinforced, partially fluorinated polyimide composites

Graphite-fiber-reinforced polyimide (GFRPI) composites were formulated from three new partially fluorinated polyimides and three types of graphite fiber. Nine composites were molded into pins and evaluated in a pin-on-disk tribometer. Friction coefficients, wear rates, pin wear surface morphology, and transfer film formation were assessed at 25 and 300 C. Also assessed was the effect of sliding speed on friction. Wear was up to two orders of magnitude lower at 25 C and up to one order of magnitude lower at 300 C than with previously formulated NASA GFRPI composites.

Fusaro, R. L.↗

SEM/XPS analysis of fractured adhesively bonded graphite fibre-reinforced polyimide composites

The surfaces of the graphite fiber-reinforced polyimide composites presently pretreated prior to bonding with polyimide adhesive contained variable amounts of a fluoropolymer, as determined by X-ray photoelectron spectroscopy. Lap shear strengths were determined for unaged samples and for those aged over 500- and 1000-hour periods at 177 and 232 C. Unaged sample lap strengths, which were the highest obtained, exhibited no variation with surface pretreatment, but a significant decrease is noted with increasing aging temperature. These thermally aged samples, however, had increased surface fluorine concentration, while a minimal concentration was found in unaged samples. SEM demonstrated a progressive shift from cohesive to adhesive failure for elevated temperature-aged composites.

Devilbiss, T. A.↗

Friction and wear behavior of graphite fiber reinforced polyimide composites

The friction and wear rate characteristics of 50/50 (weight per cent) graphite fiber-polyimide composites were studied by sliding metallic hemispherically tipped riders against disks made from the composites. Two different polyimides and two different graphite fibers were evaluated. Also studied were such variables as the effect of adding 10 per cent weight additions of powdered (CF-1.1)n, CdI2, or CdO, the effect of moisture in an air atmosphere, the effect of temperature, and the effect of different sliding speeds. In general, wear to the metallic riders was negligible and composite wear increased at a constant rate as a function of number of sliding cycles.

Fusaro, R. L.↗

Processing and properties of fiber reinforced polymeric matrix composites: I. IM7/LARC(TM)-PETI-7 polyimide composites

A phenylethynyl terminated imide oligomer formed from the reaction of benzophenone tetracarboxylic acid dianhydride, an 75:25 molar ratio of 4,4'-oxydianiline and meta-phenylenediamine and 4-phenylethynylphthalic anhydride as the endcapper at a theoretical number average molecular weight (Mn) of approximately 3,700 g/mol was evaluated as a composite resin matrix. A glass transition temperature (Tg) of 315 deg C was reached after 250 deg C/1 hr annealing of the matrix resin. Unidirectional prepreg was made by coating an N-methylpyrrolidinone solution of the amide acid oligomer onto unsized IM7 graphite fibers. The thermal and rheological properties and the solvent/volatile depletion rates of the amide acid/NMP system were determined. This information was used to successfully design a molding cycle for composite fabrication. Composites molded under 800 Psi at 371 C consistently yielded good consolidation as measured by C-scan and optical photomicrography. The composite's short beam shear strength (SBS), longitudinal and transverse flexural strengths and moduli were measured at various temperatures. These composites exhibited excellent room temperature (RT) longitudinal flexural strength and modulus and RT SBS strength retention at 177 C.

Hou, Tan-Hung↗

Laser Sintering of Thermoset Polyimide Composites

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the CAD model. SLS generally uses thermoplastic polymeric powders, such as polyamides (i.e. Nylon), and the resultant 3D objects are often weaker in their strength compared to traditionally processed materials, due to the lack of polymer inter-chain connection in the z-direction. Our previous effort showed the challenges of printing a melt-processable RTM370 imide resin powder terminated with reactive 4-phenylethynylphthalic anhydride by LS, due to its inherently low viscosity of these oligomers. This paper presented the first successful 3D printing of high temperature carbon fiber filled thermoset polyimide composites, followed by post cure cycles to promote additional crosslinking for achieving higher temperature (Tg = 370 °C) capability. The processes to build tensile specimens and a component by LS, and the characterization of RTM370 imide resin by DSC and rheology as well as evaluation of the LS printed polyimide composite specimens by SEM and mechanical tests will be discussed.

Polyimide Composites↗

Thermo-oxidative stability of graphite fiber/PMR-15 polyimide composites at 350 deg C

A series of graphite fiber/PMR-15 polyimide composites were subjected to isothermal aging at 350 C in flowing air (100 cc/min and 1000 cc/min) over a 520 hr time period. The graphite fibers were analyzed by ISS/SIMS techniques before composite fabrication. Fibers exposed at the surface of the composite due to the isothermal aging process were also analyzed by the ISS/SIMS method. Component and composite weight less studies were also conducted for similarly exposed materials. Optical micrograph investigations of composites to follow the progress of the thermo-oxidative process were also conducted. Flexural and interlaminar shear strengths of the imaged and aged composites were measured. The relationship of component and composite properties as they relate to the thermo-oxidative behavior of the materials was discussed.

Scola, D. A.↗

Surface analysis of graphite fiber reinforced polyimide composites

Several techniques have been used to establish the effect of different surface pretreatments on graphite-polyimide composites. Composites were prepared from Celion 6000 graphite fibers and the polyimide LARC-160. Pretreatments included mechanical abrasion, chemical etching and light irradiation. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) were used in the analysis. Contact angle of five different liquids of varying surface tensions were measured on the composites. SEM results showed polymer-rich peaks and polymer-poor valleys conforming to the pattern of the release cloth used durng fabrication. Mechanically treated and light irradiated samples showed varying degrees of polymer peak removal, with some degradation down to the graphite fibers. Minimal changes in surface topography were observed on concentrations of surface fluorine even after pretreatment. The light irradiation pretreatment was most effective at reducing surface fluorine concentrations whereas chemical pretreatment was the least effective. Critical surface tensions correlated directly with the surface fluorine to carbon ratios as calculated from XPS.

Messick, D. L.↗

The 371 deg C(700 deg F) properties of celion 6000/n-phenylnadimide modified PMR polyimide composites

The 371 C (700 F) properties of Celion 6000/N-phenylnadimide modified PMR-15 polyimide composites were investigated to determine the feasibility of using these materials at a 371 C (700 F) service temperature. The processing characteristics and physical and mechanical properties of the composite systems are presented. The results of the 371 C (700 F) thermo-oxidation stability study suggest that the composite materials can be considered for short term (at least 100 hours) application at 371 C (700 F).

Pater, R. H.↗

Aerospace applications of PMR polyimide composites

The current status of the novel class of processable, addition-type polyimides known as PMR (for in situ polymerization of monomer reactants) polyimides, developed by NASA at the Lewis Research Center, is reviewed. Highlights of PMR technology studies conducted at NASA Lewis are presented. Several examples of industrial applications of PMR-15 polyimide composites to aerospace structural components are examined.

Serafini, T. T.↗