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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.

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All sourcesNASA NTRSDOE OSTI
NASA NTRS2001

Polyimide Composites from 'Salt-Like' Solution Precursors

Four NASA Langley-developed polyimide matrix resins, LaRC(TM)-IA, LaRC(TM)-IAX, LaRC(TM)-8515 and LaRC(TM)-PETI-5, were produced via a 'saltlike' process developed by Unitika Ltd. The salt-like solutions (65% solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC multipurpose tape machine. Process parameters were determined and composite panels fabricated. The temperature dependent volatile depletion rates, the thermal crystallization behavior and the resin rheology were characterized. Composite molding cycles were developed which consistently yielded well consolidated, void-free laminated parts. Composite mechanical properties such as the short beam shear strength; the longitudinal and transverse flexural strength and flexural modulus; the longitudinal compression strength and modulus; and the open hole compression strength and compression after impact strength were measured at room temperature and elevated temperatures. The processing characteristics and the composite mechanical properties of the four intermediate modulus carbon fiber/polyimide matrix composites were compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (30-35% solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of the polyimide composites.

Cano, Roberto J.↗
NASA NTRS1983

Dynamic Mechanical Properties of N-Phenylnadimide Modified PMR Polyimide Composites

The rheological behavior of newly developd Celion 6000/N-phenylnadimide modified PMR polyimide and PMR-15 composites was investigated. The dynamic mechanical properties were correlated with the structure of N-phenylnadimide modified PMR polyimides. The storage modulus (G'), loss modulus (G''), and loss tangent (tan delta) of four composite systems were measured over a temperature range from -150 to 400 C. Three well defined peaks were seen in the regions of 360, 100, and -120 C, corresponding to the alpha, beta, and gamma relaxations, respectively, of the matrix resins. The activation energies of the alpha, beta, and gamma relaxations were estimated to be 232, 60, and 14 kcal/mole, respectively, for PMR-15. Addition of N-phenylnadimide to the PMR-15 composition lowered the glass transition temperature and the activation energies of PMR-15 polyimide. The dynamic mechanical data appear to be consistent with the formation of a copolymer from N-phenylnadimide and a PMR-15 prepolymer.

Pater, R. H.↗
NASA NTRS2004

Heat, Moisture and Chemical Resistant Polyimide Compositions and Methods for Making and Using Them

Polyimides having a desired combination of high thermo-oxidative stability, low moisture absorption and excellent chemical and corrosion resistance are prepared by reacting a mixture of compounds including (a) 3,3',4,4'- benzophenonetetracarboxylic dianhydride (BTDA), (b) 3,4'- oxydianiline (3,4'-ODA), and (c) 5-norbornene-2,3- dicarboxylic anhydride (NA) in a high boiling, aprotic solvent to give 5 to 35% by weight of polyamic acid solution. The ratio of (a), (b), and (c) is selected to afford a family of polyimides having different molecular weights and properties. The mixture first forms a polyamic acid precursor. Upon heating at or above 300 C, the polyamic acids form polyimides, which are particularly suitable for use as a high temperature coating, adhesive, thin film, or composite matrix resin.

Ruth H Pater↗
NASA NTRS2001

Zr-Containing 4,4'-ODA/PMDA Polyimide Composites

The objective of this research is to improve the atomic oxygen resistance of Kapton(TM), a polyimide (PI) made from pyromellitic acid dianhydride (PMDA) and 4,4'-oxydianiline (ODA), while retaining or enhancing the desirable properties of the pure polymer. Toward this end, zirconium-containing complexes and polymers were used to make composites and blends. Tetra(acetylacetonato)zirconium(IV), Zr(acac)4, which is commercially available, was identified as the best zirconium-containing complex for enhancing the atomic oxygen resistance of polyimide composites of the 10 complexes screened. Films prepared from the commercially available polyamic acid (PAA) of PMDA-ODA (DuPont) have good uniformity, flexibility, and tensile strength. A 24-layer 10% (mol) Zr(acac)4/PI composite film showed significant improvement (ca. 20 fold) of atomic oxygen resistance over the pure polyimide. However, 10% (mol) Zr(acac)4 represents an upper concentration limit, above which films undergo cracking upon thermal imidization. In order to increase the Zr complex concentration in PMDA-ODA PI films, while retaining good film properties, [Zr(adsp)2-PMDA]n coordination polymer [bis(4-amino-N,N'-disalicylidene- 1,2-phenylenediamino)zirconium(IV)-pyromellitic dianhydride] and [Zr(adsp)2-PMDA-ODA-PMDA]n terpolymer were synthesized and blended with commercial PAA, respectively. Several techniques were used to characterize the films made from the polymer containing Zr(acac)4. Plasma studies of films having 2% (mol) incremental concentrations of Zr in the Kapton up to 10% (mol) show that the overall rate of erosion is reduced about 75 percent.

Illingsworth, M. L.↗
NASA NTRS1975

Performance of graphite fiber-reinforced polyimide composites in self-aligning plain bearings to 315 C

A 50/50 (weight percent) composite of graphite fibers and polyimide was studied in self-aligning plain bearings oscillating + or - 15 degrees at 1 hz. The friction coefficient was 0.15 + or - 0.05 at 250 C, and 0.05 + or - 0.02 at 315 C. Best results were obtained with a molded composite liner with chopped graphite fibers randomly oriented in the composite. The specific wear rate is given. It was found that the dynamic unit load capacity was higher for a composite bushing (thin liner), than for a composite ball.

Sliney, H. E.↗
NASA NTRS1987

Crosslinking-property relationships in PMR polyimide composites. I

The thermooxidatively-induced crosslinking/ physical and mechanical property relationships of graphite fiber-reinforced PMR polyimide-matrix composites were studied during isothermal exposure of the composite specimens at 288 C in air for periods of up to 5000 hr. The crosslinking densities due to this treatment were estimated on the basis of the kinetic theory of rubber elasticity and shifts in the glass transition temperature T(g). Several linear relationships are noted between crosslink density and physical and mechanical properties: T(g), initial weight loss, and elevated temperature interlaminar shear strength increase with crosslink density, while initial moisture absorption decreases. After achieving the highest crosslink density, several of the composite properties begin to decrease from their maximum values.

Pater, R. H.↗
NASA NTRS1982

PMR polyimide composites for aerospace applications

Fiber reinforced PMR polyimides are finding increased acceptance as engineering materials for high performance structural applications. Prepreg materials based on this novel class of highly processable, high temperature resistant polyimides, are commercially available and the PMR concept was incorporated in several industrial applications. The status of PMR polyimides is reviewed. Emphasis is given to the chemistry, processing, and applications of the first generation PMR polyimides known as PMR-15.

Serafini, T. T.↗
NASA NTRS1985

Polyimide composites: Application histories

Advanced composite hardware exposed to thermal environments above 127 C (260 F) must be fabricated from materials having resin matrices whose thermal/moisture resistance is superior to that of conventional epoxy-matrix systems. A family of polyimide resins has evolved in the last 10 years that exhibits the thermal-oxidative stability required for high-temperature technology applications. The weight and structural benefits for organic-matrix composites can now be extended by designers and materials engineers to include structures exposed to 316 F (600 F). Polyimide composite materials are now commercially available that can replace metallic or epoxy composite structures in a wide range of aerospace applications.

Poveromo, L. M.↗
NASA NTRS2008

Magnetic Property Measurements on Single Wall Carbon Nanotube-Polyimide Composites

Temperature and magnetic field dependent magnetization measurements were performed on polyimide nanocomposite samples, synthesized with various weight percentages of single wall carbon nanotubes. It was found that the magnetization of the composite, normalized to the mass of nanotube material in the sample, decreased with increasing weight percentage of nanotubes. It is possible that the interfacial coupling between the carbon nanotube (CNT) fillers and the polyimide matrix promotes the diamagnetic response from CNTs and reduces the total magnetization of the composite. The coercivity of the samples, believed to originate from the residual magnetic catalyst particles, was enhanced and had a stronger temperature dependence as a result of the composite synthesis. These changes in magnetic properties can form the basis of a new approach to investigate the interfacial properties in the CNT nanocomposites through magnetic property measurements.

Sun, Keun J.↗
NASA NTRS2019

Manufacturing of Thermoset Polyimide Composites by Laser Sintering

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 computer-aided design (CAD) model. SLS generally uses thermoplastic polymeric powders such as polyamides. The resultant 3D-printed objects are often weaker in their strength compared to traditionally processed materials, due to their higher porosity. This paper described the process development of using melt-processable imide oligomers terminated with reactive 4-phenylethynylphthalic anhydride (4-PEPA) to conduct laser sintering (LS). The first successful 3D-printing of high temperature RTM370 thermoset polyimide carbon fiber composites were further post-cured to promote additional crosslinking for achieving higher temperature (T g = 370°C) capability. Another novel imide oligomer, RTM385-SLS, formulated with a complex melt viscosity [ƞ*] of ~104-105 poise is also suitable for LS. RTM385-SLS resin powder was mixed with 20-25% of hexagonal boron nitride (h-BN) and subjected to LS to print out “Green” specimens which could be further post-cured to afford a thermally conductive but electrically insulating composites with high T g of 385 °C. The cured composite specimens were then subjected to mechanical testing, thermal conductivity and porosity measurements as well as SEM characterization.

additive Manufacturing↗
NASA NTRS1972

Titanium reinforced boron polyimide composite

Program involves development of process technique for boron-polyimide prepeg, lay-up and curing procedures for prepegs when processed under vacuum bag pressure, and development and evaluation of titanium hard points for smooth transition of loads from titanium attach points into boron reinforced body of structure.

Clark, G. A.↗
NASA NTRS1996

Experiments Related to the Fabrication of Carbon Fiber/AMB-21 Polyimide Composite Tubes Using the RTM Process

AMB-21 is a new polymer developed by Mr. Ray Vannucci, NASA, LeRC as a noncarcinogenic polyimide matrix which may be suitable for fabricating composite parts by the Resin Transfer Modeling (RTM) process. The polyimide for this project was prepared at the Center of Composite Materials Research at N.C. A&T State University because it is not currently an item of commerce. The RTM process is especially suitable for producing geometrically complex composite parts at a low cost. Because of the high melting point and very high viscosity at the time of processing, polyimides have not been extensively used in the RTM process. The process for preparing AMB-21 as well as the process for fabricating composite plates will be described. The basic fabrication process consists of injecting a solvent solution of AMP-21 into a carbon fiber preform, evaporating the solvent, imidizing the polyimide, and vacuum/compression modeling the impregnated preform. All the above molding steps are preformed in a specially designed RTM mold which will be described. The results of this process have been inconsistent. Where as some experiments have resulted in a reasonably sound panels, others have not. Further refinements of the process are required to establish a reliable process.

Exum, Daniel↗
NASA NTRS2006

Solvent Free Low-Melt Viscosity Imide Oligomers And Thermosetting Polyimide Composites

This invention relates to the composition and a solvent-free process for preparing novel imide oligomers and polymers specifically formulated with effective amounts of a dianhydride such as 2,3,3',4-biphenyltetra carboxylic dianydride (a-BPDA), at least one aromatic diamine' and an endcapped of 4-phenylethynylphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260-280" C. When the imide oligomer melt is cured at about 371 C. in a press or autoclave under 100-500 psi, the melt resulted in a thermoset polyimide having a glass transition temperature (T(sub g)) equal to and above 310 C. A novel feature of this process is that the monomers; namely the dianhydrides, diamines and the endcaps, are melt processable to form imide oligomers at temperatures ranging between 232-280 C. (450-535 F) without any solvent. These low-melt imide oligomers can be easily processed by resin transfer molding (RTM), vacuum-assisted resin transfer molding (VARTM) or the resin infusion process with fiber preforms e.g. carbon, glass or quartz preforms to produce polyimide matrix composites with 288-343C (550-650 F) high temperature performance capability.

Chuang, CHun-Hua↗
NASA NTRS2000

A High T(sub g) PMR Polyimide Composites (DMBZ-15)

A high T(sub g) thermosetting PMR-type polyimide, designated as DMBZ-15, was developed by replacing methylene dianline (MDA) in PMR-15 with 2,2'-dimethylbenzidine. Polyimide/carbon fiber (T650-35) composites were fabricated from a formulation of 3,3', 4,4'-benzophenonetetracarboxylic acid dimethyl ester (BTDE) and 2,2'-dimethylbenzidine (DMBZ), along with nadic ester (NE) as the endcap. DMBZ-15 displays a higher glass transition temperature (T(sub g) = 414 C) than PMR-15 (T(sub g) = 345 C), and thus retains better mechanical properties for brief exposure above 400 C. The physical properties and longterm thermo-oxidative stability of the DMBZ-15 polyimide/carbon fiber composites are also compared to that of PMR-15.

Chuang, Kathy C.↗
NASA NTRS1985

Graphite/PMR polyimide composites with improved toughness

The toughness of composites made with modified PMR (polymerization of monomer reactants) polyimides and Celion 6000 graphite fibers was studied. Various types/levels of monomer reactants containing flexible links were incorporated into PMR resin compositions used to prepare composites. The composites were evaluated for toughness using instrumented drop weight and 10 deg off axis tensile tests at room temperature, and for strength using flexure and short beam shear tests at room temperature and at elevated temperature. The effect of resin composition on composite processability, thermo-oxidative stability, toughness and mechanical properties are discussed.

Vannucci, R. D.↗
NASA NTRS1985

Graphite/PMR polyimide composites with improved toughness

The toughness of composites made with modified PMR (Polymerization of monomer reactants) polyimides and Celion 6000 graphite fibers was studied. Various types/levels of monomer reactants containing flexible links were incorporated into PMR resin compositions used to prepare composites. The composites were evaluated for toughness using instrumented drop weight and 10 deg off axis tensile tests at room temperature, and for strength using flexure and short beam shear tests at room temperature and at elevated temperature. The effect of resin composition on composite processability, thermo-oxidative stability, toughness and mechanical properties are discussed.

Vannucci, R. D.↗
NASA NTRS1976

Effects of tetraamine crosslinking agents on the thermomechanical properties of PMR polyimide composites

The effects were investigated of partial substitution of tetraamine crosslinking agents for diamine reactants on the thermomechanical properties of PMR polyimide resins and graphite fiber-reinforced composites. The effect of tetraamine content on isothermal weight loss, glass transition, and softening temperatures of neat resin samples is discussed. Composites were fabricated using PMR methodology. Monomeric solution of various stoichiometric ratios was used to impregnate Hercules HTS graphite fiber. The mechanical property retention characteristics of the composites at 316 C (600 F) are described.

Delvigs, P.↗
NASA NTRS1983

Surface analysis of grapite fiber reinforced polyimide composites. I

The results of experimental analyses of the effects of pretreatment on bonding between composite materials are reported. The materials comprised graphite fibers in a polyimide matrix. The surfaces were bonded as-received or subjected to grit blasting, bead blasting, hand sanding, washes with ethanolic KOH, NH2NH2-H2O or H2SO4 + 0.30 H2O2 or flashblasting. SEM and X-ray photoelectron spectroscopy revealed fluorine contents in the as-received samples. Contact angles were determined by means of five different liquids with various surface tensions. The flashblast technique removed all fluorine from the samples. Low critical surface tensions were found in the composite surfaces with high fluorine concentrations. The surface scanning techniques are concluded to be useful for studying factors influencing the strength and durability of adhesively bonded composites.

Messick, D. L.↗