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At least 739 records · Page 41
All sourcesNASA NTRSDOE OSTI
NASA NTRS1994

Phenylethynyl-Terminated Polyimides

Phenylethynyl-terminated polyimides exhibit properties suitable for films, moldings, adhesives, and composite-material matrices. Polyimides synthesized at various molecular weights, selected to obtain desirable properties for specific applications. Thermally cured to form cross-linked molecular structures typically increasing resistance to solvents, glass-transition temperatures, and moduli of elasticity. Also have low molecular weights and low melt viscosities for easier processing into composites and adhesive bonds.

Jensen, Brian J.↗
NASA NTRS1993

Di(hydroxyphenyl)- benzimidazole monomers

Di(hydroxyphenyl)benzimidazole monomers were prepared from phenyl-hydroxybenzoate and aromatic bis(o-diamine)s. These monomers were used in the synthesis of soluble polybenzimidazoles. The reaction involved the aromatic nucleophilic displacement of various di(hydroxyphenyl)benzimidazole monomers with activated aromatic dihalides or activated aromatic dinitro compounds in the presence of an alkali metal base. These polymers exhibited lower glass transition temperatures, improved solubility, and better compression moldability over their commercial counterparts.

Connell, John W.↗
NASA NTRS1993

Effects of physical aging on long-term behavior of composites

The HSCT plane, envisioned to have a lifetime of over 60,000 flight hours and to travel at speeds in excess of Mach 2, is the source of intensive study at NASA. In particular, polymer matrix composites are being strongly considered for use in primary and secondary structures due to their high strength to weight ratio and the options of property tailoring. However, an added difficulty in the use of polymer based materials is that their properties change significantly over time, especially at the elevated temperatures that will be experienced during flight, and prediction of properties based on irregular thermal and mechanical loading is extremely difficult. This study focused on one aspect of long-term polymer composite behavior: physical aging. When a polymer is cooled to below its glass transition temperature, the material is not in thermodynamic equilibrium and the free volume and enthalpy evolve over time to approach their equilibrium values. During this time, the mechanical properties change significantly and this change is termed physical aging. This work begins with a review of the concepts of physical aging on a pure polymer system. The effective time theory, which can be used to predict long term behavior based on short term data, is mathematically formalized. The effects of aging to equilibrium are proven and discussed. The theory developed for polymers is then applied first to a unidirectional composite, then to a general laminate. Comparison to experimental data is excellent. It is shown that the effects of aging on the long-term properties of composites can be counter-intuitive, stressing the importance of the development and use of a predictive theory to analyze structures.

Brinson, L. Catherine↗
NASA NTRS1994

Effects of physical aging on long-term creep of polymers and polymer matrix composites

For many polymeric materials in use below the glass transition temperature, the long term viscoelastic behavior is greatly affected by physical aging. To use polymer matrix composites as critical structural components in existing and novel technological applications, this long term behavior of the material system must be understood. Towards that end, this study applied the concepts governing the mechanics of physical aging in a consistent manner to the study of laminated composite systems. Even in fiber-dominated lay-ups the effects of physical aging are found to be important in the long-term behavior of the composite. The basic concepts describing physical aging of polymers are discussed. Several aspects of physical aging which have not been previously documented are also explored in this study, namely the effects of aging into equilibrium and a relationship to the time-temperature shift factor. The physical aging theory is then extended to develop the long-term compliance/modulus of a single lamina with varying fiber orientation. The latter is then built into classical lamination theory to predict long-time response of general oriented lamina and laminates. It is illustrated that the long term response can be counterintuitive, stressing the need for consistent modeling efforts to make long term predictions of laminates to be used in structural situations.

Brinson, L. Catherine↗
NASA NTRS1993

Effects of orbital exposure on RTV during the LDEF mission

Thermomechanical analysis (TMA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA) were performed on samples of RTV 511 exposed on the Long Duration Exposure Facility (LDEF) mission for 6 years in orbit and unexposed RTV 511 control samples. Slices 20- to 400-microns thick were removed from the exposed surface down to a depth of 1,500 microns through the 3-mm thick samples. The TMA and DSC results, which arise from the entire slice and not just its surface, showed no significant differences between the LDEF exposed and the control samples. TMA scans were run from ambient to 500 C; results were compared by a tabulation of the onset temperatures for flow. DSC scans were run from ambient to 600 C; no endotherms or exotherms occurred over the range observed. What appear to be glass transition temperatures were compared for the samples as a function of section depth within the sample and between the exposed and control samples. The TGA scans from 25 to 900 C, which arise from the surface of the sample initially, showed a slight increase in the top most 105-micron slice (the exposed, discolored side) in the weight loss at 600 C in oxygen. This weight loss dropped to bulk values at the next slice below the top section, a mean depth of 258 microns. The control sample also showed an increase in weight loss as the top surface was approached, but the 600 C weight losses were very inconsistent. The LDEF RTV sample appears to be mechanically undamaged, with a surface layer which oxidizes slightly faster as a result of orbital exposure.

Brower, William E., Jr.↗
NASA NTRS1994

Space flight printed wiring board measling investigation

A flight printed wiring board (PWB) for a satellite project was observed to have a high incidence of measling. Other PWB's produced for the program by the same manufacturer did not exhibit the degree of measling as did the 'measle-prone' board. Measling susceptibility during hand soldering and measling effects on PWB insulation resistance were investigated for three production PWB's. Measling resistance was significantly different between the three boards: the 'worst' exhibited five times the number of measles as the 'best' board. 'Severe' measling (that which is likely to affect board reliability) did not exist on the 'best' board, even under extreme soldering conditions (399 degrees C for 12-15 sec.), whereas the 'worst' board showed an average of one 'severe' measle for every two pads under more normal soldering conditions (288-343 degrees C for 2-5 sec.). Both soldering time and temperature affected measling, with time having a slightly greater influence (2 percent versus 12 percent). Measling effects on PWB insulation resistance were inconclusive. These were evaluated by in situ resistance measurements on the same three boards at elevated temperature and humidity. The measured resistance for all three boards decreased for exposures greater than 50 degrees C and 50 percent relative humidity. The 'measle-prone' board showed a resistance decrease at only 25 degrees C and 50 percent relative humidity. However, no definitive difference was detected between measled and not-measled (control) samples. The boards evaluated were production boards, so the effect of interlayer traces connecting the plated-through holes was not controlled. It is likely the resistance measurements were over different volumes of PWB laminate, which would account for the widely varying resistances measured. Thermomechanical measurements on board laminate materials did not reveal any differences attributed to measling. Differences in glass transition temperature were significantly different when measured by DTA, but not by SDT. Laminate thermal expansion differences were significant for the 35 degrees C evaluations, but not for any higher temperatures.

Thomas, Walter B., III↗
NASA NTRS1994

A solvent resistant copolyimide

A solvent resistant copolyimide was prepared by reacting 4,4'-oxydiphthalic anhydride with a diamine blend comprising, based on the total amount of the diamine blend, about 75 to 90 mole percent of 3,4'-oxydianiline and about 10 to 25 mole percent p-phenylene diamine. The solvent resistant copolyimide had a higher glass transition temperature when cured at 350 C, 371 C and 400 C than LaRC(TM)-IA. The composite prepared from the copolyimide had similar mechanical properties to LaRC(TM)-IA. Films prepared from the copolyimide were resistant to immediate breakage when exposed to solvents such as dimethylacetamide and chloroform. The adhesive properties of the copolyimide were maintained even after testing at 23 C, 150 C, 177 C and 204 C.

Chang, Alice C.↗
NASA NTRS1995

LDEF polymeric materials: A summary of Langley characterization

The NASA Long Duration Exposure Facility (LDEF) enabled the exposure of a wide variety of materials to the low earth orbit (LEO) environment. This paper provides a summary of research conducted at the Langley Research Center into the response of selected LDEF polymers to this environment. Materials examined include graphite fiber reinforced epoxy, polysulfone, and additional polyimide matrix composites, films of FEP Teflon, Kapton, several experimental high performance polyimides, and films of more traditional polymers such as poly(vinyl toluene) and polystyrene. Exposure duration was either 10 months or 5.8 years. Flight and control specimens were characterized by a number of analytical techniques including ultraviolet-visible and infrared spectroscopy, thermal analysis, scanning electron and scanning tunneling microscopy, x-ray photoelectron spectroscopy, and, in some instances, selected solution property measurements. Characterized effects were found to be primarily surface phenomena. These effects included atomic oxygen-induced erosion of unprotected surfaces and ultraviolet-induced discoloration and changes in selected molecular level parameters. No gross changes in molecular structure or glass transition temperature were noted. The intent of this characterization is to increase our fundamental knowledge of space environmental effects as an aid in developing new and improved polymers for space application. A secondary objective is to develop benchmarks to enhance our methodology for the ground-based simulation of environmental effects so that polymer performance in space can be more reliably predicted.

Young, Philip R.↗
NASA NTRS1995

Structure and properties of polymeric composite materials during 1501 days outer space exposure at Salyut-7 orbital station

Specimens of polymeric composite materials for aviation and space applications such as glass fiber reinforced plastics (GFRP), carbon fiber reinforced plastics (CFRP), organic fiber reinforced plastics (OFRP), and hybrid plastics (HP) based on epoxy compounds were exposed to the space environment on the surface of Salyut-7 orbital station. The space exposure lasted 1501 days as a maximum. The data relating to the change in mechanical properties, mass losses, glass transition temperature, linear thermal expansion coefficient, and microstructure after various periods of exposure are given. It has been found that the change in properties is caused by the processes of binder postcuring and microerosion of the exposed surface of plastics. The phenomenon of strengthening of the surface layer of hybrid composites, due to which the nature of destruction changes at bending loads, has been revealed.

Startsev, Oleg V.↗
NASA NTRS1994

Structure-property relationships in addition polyimides. 1: Resins from four-ring aromatic diamines containing carbonyl and methylene groups

In an effort to improve the processing characteristics of addition-type polyimide resins the use of flexibilized four-ring aromatic diamine moieties was investigated. A series of 12 diamines containing carbonyl and methylene, as well as oxo and thio bridging groups, was synthesized. The diamines were polymerized with the dimethyl ester of 3.3', 4.4' - benzophenonetetracarboxylic acid (BTDE), using the monomethyl ester of nadic acid (NE) as an end-cap. The effect of diamine structure on the solubility and rheological properties during cure was determined. This paper also describes the effect of diamine structure and formulated molecular weight on the glass transition temperature and thermo-oxidative stability at elevated temperatures after various post-cure regimes. The results indicate that polyimides from some of the diamines containing methylene connecting groups have potential as matrix resins for long-term applications at temperatures up to 300 C.

Delvigs, Peter↗
NASA NTRS1994

Preparation and characterization of poly (arylene ether isoxazole)s by fluoride ion-mediated aromatic nucleophilic displacement reactions

As part of a continuing effort to prepare novel thermally stable high-performance polymers, poly(arylene ether isoxazole)s have been prepared by fluoride ion-catalyzed aromatic nucleophilic substitution reactions with bis(trimethylsiloxyphenyl) isoxazoles and activated bisarylhalides in diphenyl sulfone. Initial investigation involving the preparation of these materials with isoxazole bisphenols and activated bisarylhalides in the presence of potassium carbonate indicated that, under reaction conditions necessary to prepare high-molecular-weight materials, the isoxazole monomer was converted to an enamino ketone. This side reaction was avoided by using fluoride as a base. However, trimethylsilyl ether derivatives of the isoxazole bisphenols were required in these polymerizations for the preparation of high-molecular-weight materials. Moderate to high inherent viscosity eta(sub inh): 0.43-0.87 dl/g) materials with good thermal stability (air: 409-477 C, helium: 435-512 C) can be prepared by the silyl ether method. Glass transition temperatures ranged from 182 to 225 C for polymers with phenyl pendants and from 170 to 214 C for those without. Molecular weight control by 2% endcapping and the incorporation of a phenyl pendant at the 4 position of the isoxazole is necessary to yield polymers soluble in polar aprotic solvents at room temperature. There is evidence, however, indicating the existence of crosslinks between the polymer chains when the silyl ether approach is utilized.

Herbert, C. G.↗
NASA NTRS1995

Poly(Arylene Ether)s Containing Pendent Ethynyl Groups

Poly(arylene ether)s containing pendent ethynyl groups synthesized. Offer advantage over linear poly(arylene ether)s in upon heating, pendent ethynyl groups react to form cross-linked molecular structures exhibiting greater resistance to solvents and higher glass-transition temperatures and tensile moduli. Polymers useful as adhesives, moldings, films, and matrices of composite materials.

Hergenrother, Paul M.↗
NASA NTRS1995

Polyimides Made From 3,5-Diaminobenzotrifluoride

Polyimides synthesized from 3,5-diaminobenzotrifluoride (DABTF). One monomer of major importance in preparing these high-temperature polymers is 1,3-phenylenediamine (mPDA). Fluorinated polyimides exhibit characteristics potentially attractive for aerospace and electronic applications. Includes optical transparency, solubility in common polar solvents, enhanced thermo-oxidative stability, low dielectric constants, and high glass-transition temperatures. Polyimides also used to form free-standing films, coatings, and moldings.

St. Clair, Terry L.↗
NASA NTRS1995

LaRC(TM)-IA Copolyimides

Copolyimides modified versions of LaRC(TM)-IA thermoplastic polyimide formulated by incorporating moieties of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) and, alternatively, isophthaloyldiphthalic anhydride (IDPA) into LaRC(TM)-IA polymer backbones. Exhibit higher glass-transition temperatures and retain greater fractions of lower-temperature shear moduli at higher temperatures. Copolyimides spun into fibers or used as adhesives, molding powders, or matrix resins in many applications, especially in fabrication of strong, lightweight structural components of aircraft.

St. Clair, Terry L.↗
NASA NTRS1995

Integrated optical components in thin films of polymers

The results will be reported on the study of integrated optical components based on nonlinear optical polymeric films. Polymers poly(methyl methacrylate) (PMMA) and polyimide (PI) doped with organic laser dyes 4-dicyanomethylene-2-methyl-6-p dimethylaminostyryl-4H pyran (DCM) and 1, 3, 5, 7, 8 - pentamethyl-2,6 -diethyl-pyrromethene -BF2-complex (Pyrommethene 567, PM-567) were selected as materials for light guiding films. Additionally, UV polymerized polydiacetylene (PDA) on glass substrate was used as a waveguide material. Optical waveguides were fabricated using spin coating of preoxidized silicon wafers (1.5 micrometer silicon oxide layer) with organic dye/polymer solution followed by soft baking. the modes in slab waveguides were studied using prism coupling techniques. Measured values of mode coupling angles in multimode waveguides were used to calculate film thickness and refractive index for different polarizations. Refractive index anisotropy was found in PDA waveguide. The optimal conditions of spin coating for single mode waveguide fabrication were estimated. Propagation losses were measured by collecting the light scattered from the trace of a propagating mode either by scanning photo detector or by CCD camera. Different types of light coupling techniques were used including end-dire coupling, prism and grating coupling. Mechanical printing technique was developed for coupling grating fabrication resulting in gratings with 4% diffraction efficiency. The gratings demonstrated good stability with diffraction efficiency relaxation rate 2.4 dB/hour at a temperature approximately 15-20 C below glass transition point. Dye doped waveguides were transversally pumped with frequency doubled Nd:YAG Q-switched laser producing intensive light emission with apparent 6 kW/sq cm pump threshold and spectrum narrowing near 617 nm peak in the case of DCM doped waveguide. PM-567 doped waveguide pumped with CW Ar(+) laser (514 nm wavelength) far below threshold (0.1 W/sq.cm pump power) demonstrated emission spectrum narrowing near 616 nm peak with 18% power conversion slope efficiency. In this case emission spectrum modification was caused by the enhanced light absorption along the direction of propagating waveguide modes. Changing length, thickness, and other morphlogical waveguide parameters one can modify emission spectrum in predictable direction. The results show that polymeric waveguides, especially based on high temperature polymers such as Pl, can be used to produce a varietiy of active and passive silicon compatible integrated optical components for aerospace applications.

Sarkisov, Sergey↗
NASA NTRS1995

Crystalline imide/arylene ether copolymers

Crystalline imide/arylene ether block copolymers are prepared by reacting anhydride terminated poly(amic acids) with amine terminated poly)arylene ethers) in polar aprotic solvents and chemically or thermally cyclodehydrating the resulting intermediate poly(amic acids). The block copolymers of the invention have one glass transition temperature or two, depending on the particular structure and/or the compatibility of the block units. Most of these crystalline block copolymers for tough, solvent resistant films with high tensile properties. While all of the copolymers produced by the present invention are crystalline, testing reveals that copolymers with longer imide blocks or higher imide content have increased crystallinity.

Jensen, Brian J.↗
NASA NTRS1995

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↗
NASA NTRS1995

Physical aging effects on the compressive linear viscoelastic creep of IM7/K3B composite

An experimental study was undertaken to establish the viscoelastic behavior of 1M7/K3B composite in compression at elevated temperature. Creep compliance, strain recovery and the effects of physical aging on the time dependent response was measured for uniaxial loading at several isothermal conditions below the glass transition temperature (T(g)). The IM7/K3B composite is a graphite reinforced thermoplastic polyimide with a T(g) of approximately 240 C. In a composite, the two matrix dominated compliance terms associated with time dependent behavior occur in the transverse and shear directions. Linear viscoelasticity was used to characterize the creep/recovery behavior and superposition techniques were used to establish the physical aging related material constants. Creep strain was converted to compliance and measured as a function of test time and aging time. Results included creep compliance master curves, physical aging shift factors and shift rates. The description of the unique experimental techniques required for compressive testing is also given.

Veazie, David R.↗