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At least 1,045 records · Page 58
All sourcesNASA NTRSDOE OSTI
NASA NTRS1989

Wet spinning of solid polyamic acid fibers

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solution of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4'-benzo phenone tetracarboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'oxydianiline (4,4'-ODA). By utilizing the interrelationship between coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Dorogy, William E., Jr.↗
NASA NTRS1989

Bis(4-(3,4-dimethylenepyrrolidyl)-phenyl) methane

It is the primary object of the present invention to prepare high temperature polymeric materials, especially linear aromatic polyimides, which maintain their integrity and toughness during long exposure times at elevated temperatures. According to the present invention, this object is achieved, and the attending benefits are obtained, by first providing the bis(exocyclodiene) bis(4-(3,4-dinethylene pyrrolidyl) phenyl) methane, which is formed from the monomer N-phenyl 3,4-dimethylene pyrrolidine. This bis-(exocyclodiene) undergoes Diels-Alder reaction with a bismaleimide without the evolution of gaseous by-products, to form the aromatic polyimide.

Ottenbrite, Raphael M.↗
NASA NTRS1990

Use of unbalanced laminates as a screening method for microcracking

State-of-the-art, high temperature polyimide matrix composites, reinforced with continuous graphite fibers are known to be susceptible to intraply cracking when thermally cycled over their useful service temperature range. It is believed that the transply cracking, in part, results from residual stresses caused by differences in coefficients of thermal expansion (CTE) between the polymer matrix and the reinforcement. Thermal cycling tests to investigate this phenomenon involve expensive time and energy consuming programs which are not economically feasible for use as a part of a materials screening process. As an alternative to thermal cycling studies, a study of unbalanced crossply graphite fiber reinforcement composites was conducted to assess the effect of the composite ply layup and surface condition on the residual stresses that remain after the processing of these materials. The residual stresses were assessed by measuring the radii of curvature of the types of laminates that were studied. The temperature at which stress-free conditions existed were determined and a dye penetrant method was used to observe surface damage resulting from excessive residual stress buildup. These results are compared with some published results of thermal cycling tests that were previously conducted on balanced polyimide composites.

Papadopoulos, Demetrios S.↗
NASA NTRS1989

Interlaminar fracture toughness of thermoplastic composites

Edge delamination tension and double cantilever beam tests were used to characterize the interlaminar fracture toughness of continuous graphite-fiber composites made from experimental thermoplastic polyimides and a model thermoplastic. Residual thermal stresses, known to be significant in materials processed at high temperatures, were included in the edge delamination calculations. In the model thermoplastic system (polycarbonate matrix), surface properties of the graphite fiber were shown to be significant. Cricital strain energy release rates for two different fibers having similar nominal tensile properties differed by 30 to 60 percent. The reason for the difference is not clear. Interlaminar toughness values for the thermoplastic polyimide composites (LARC-TPI and polyimidesulfone) were 3 to 4 in-lb/sq in. Scanning electron micrographs of the EDT fracture surfaces suggest poor fiber/matrix bonding. Residual thermal stresses account for up to 32 percent of the strain energy release in composites made from these high-temperature resins.

Hinkley, Jeffrey A.↗
NASA NTRS1989

Molecular weight characterization of advanced thermoplastic resins

Analytical techniques including low angle laser light scattering photometry (LALLS), differential viscometry (DV), gel permeation chromatography (GPC), GPC-LALLS and GPC-DV, were used to characterize the molecular weight and molecular weight distribution of several advanced thermoplastics. A discussion is presented of various molecular-weight-related parameters obtained by these techniques on an experimental polyimide and poly(arylene ether ketone) and a commercially available polysulfone. Where possible, these parameters are correlated with processability and selected mechanical properties. The molecular weight was found to vary during the thermal conversion of poly(amic acid) to polyimide. However, no change in composition of the polysulfone was noted in response to various processing procedures.

Young, Philip R.↗
NASA NTRS1990

Improving processing and toughness of a high performance composite matrix through an interpenetrating polymer network. VI

The use of a semiinterpenetrating polymer network (SIPN) of the high-performance polyimide NR-150B2 to reduce brittleness and improve processability in the highly crosslinked acetylene-terminated polyimides Thermid LR-600, AL-600, MC-600, and FA-700 is described. The theoretical basis of the SIPN process is reviewed; the preparation and characterization of the neat SIPN resins and unidirectional graphite-fiber composites are explained; and the results are presented in extensive tables, graphs, and micrographs and discussed in detail. Significant increases in fracture energy were observed with SIPN, from 93 J/sq m for unmodified LR-600 to 283-603 J/sq m for the SIPN materials; the room-temperature flexural strength of the unidirectional composites also increased, from 1344 MPa for an unmodified MC-600 composite to 2020-1751 MPa for the SIPN composites. The potential applicability of SIPN-based composites to aerospace structures and electronic components is indicated.

Pater, Ruth H.↗
NASA NTRS1990

Use of unbalanced laminates as a screening method for microcracking

State-of-the-art, high temperature polyimide matrix composites, reinforced with continuous graphite fibers are known to be susceptible to intraply cracking when thermally cycled over their useful service temperature range. It is believed that the transply cracking, in part, results from residual stresses caused by differences in coefficients of thermal expansion (CTE) between the polymer matrix and the reinforcement. Thermal cycling tests to investigate this phenomenon involve expensive time and energy consuming programs which are not economically feasible for use as a part of a materials screening process. As an alternative to thermal cycling studies, a study of unbalanced crossply graphite fiber reinforcement composites was conducted to assess the effect of the composite ply layup and surface condition on the residual stresses that remain after the processing of these materials. The residual stresses were assessed by measuring the radii of curvature of the types of laminates that were studied. The temperature at which stress-free conditions existed were determined and a dye penetrant method was used to observe surface damage resulting from excessive residual stress buildup. These results are compared with some published results of thermal cycling tests that were previously conducted on balanced polyimide composites.

Papadopoulos, Demetrios S.↗
NASA NTRS1991

Polyamide-Imides Made From BTDA

New synthesis results in improved class of tough, thermally stable polyimides containing amide linkages. Linear, aromatic, polyimide/amides synthesized from isomers of DABA with 3, 3', 4, 4'- BTDA. Mechanical properties better than those of LARC-TPI polyimide. Potentially useful as matrix resins in graphite-reinforced structures, and as fibers or coating films withstanding high temperatures.

Dezern, James F.↗
NASA NTRS1990

Bis (4-(3,4-dimethylene-pyrrolidyl)-phenyl) methane

The primary objective is to prepare high temperature polymeric materials, especially linear aromatic polyimides, which maintain their integrity and toughness during long exposure times at elevated temperatures. The attained benefits are obtained by first providing the bis (exocyclodiene) bis (4-(3,4-dimethylene-pyrrolidyl)-phenyl) methane, which is a novel material formed from the monomer N-phenyl-3,4-dimethylene-pyrrolidine. This compound undergoes Diels-Alder reaction with a bismaleimide, without the evolution of gaseous by-products, to form the aromatic polyimide bis (4-(3,4-dimethylene-pyrrolidyl)-phenyl) methane.

Ottenbrite, Raphael M.↗
NASA NTRS1991

Effect of fiber reinforcements on thermo-oxidative stability and mechanical properties of polymer matrix composites

A number of studies have investigated the thermo-oxidative behavior of polymer matrix composites. Two significant observations have been made from these research efforts: (1) fiber reinforcement has a significant effect on composite thermal stability; and (2) geometric effects must be considered when evaluating thermal aging data. A compilation of some results from these studies is presented, and this information shows the influence of the reinforcement fibers on the oxidative degradation of various polymer matrix composites. The polyimide PMR-15 was the matrix material that was used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-40R graphite fibers, along with some very stable ceramic fibers were selected as reinforcing fibers because of their high thermal stability. The ceramic fibers were Nicalon (silicon carbide) and Nextel 312 (alumina-silica-boron oxide). The mechanical properties of the two graphite fiber composites were significantly different, probably owing to variations in interfacial bonding between the fibers and the polyimide matrix. The Celion 6000/PMR-15 bond is very tight but the T-40/PMR-15 bond is less tight. Three oxidation mechanisms were observed: (1) the preferential oxidation of the Celion 6000 fiber ends at cut surfaces, leaving a surface of matrix material with holes where the fiber ends were originally situated; (2) preferential oxidation of the composite matrix; and (3) interfacial degradation by oxidation. The latter two mechanisms were also observed on fiber end cut surfaces. The fiber and interface attacks appeared to initiate interfiber cracking along these surfaces.

Bowles, Kenneth J.↗
NASA NTRS1991

Wet spinning of solid polyamic acid fibers

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solutions of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4' benzophenonetetra carboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'-oxydianiline (4,4'-ODA). By utilizing the relationship among coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Dorogy, William E., Jr.↗
NASA NTRS1991

Advanced thermoplastic resins, phase 2

High temperature structural resins are required for use on advanced aerospace vehicles as adhesives and composite matrices. NASA-Langley developed polyimide resins were evaluated as high temperature structural adhesives for metal to metal bonding and as composite matrices. Adhesive tapes were prepared on glass scrim fabric from solutions of polyamide acids of the semicrystalline polyimide LARC-CPI, developed at the NASA-Langley Research Center. Using 6Al-4V titanium adherends, high lap shear bond strengths were obtained at ambient temperature (45.2 MPa, 6550 psi) and acceptable strengths were obtained at elevated temperature (14.0 MPa, 2030 psi) using the Pasa-Jell 107 conversion coating on the titanium and a bonding pressure of 1.38 MPa (200 psi). Average zero degree composite tensile and compressive strengths of 1290 MPa (187 ksi) and 883 MPa (128 ksi) respectively were obtained at ambient temperature with unsized AS-4 carbon fiber reinforcement.

Brown, A. M.↗
NASA NTRS1990

LaRC-TPI 1500 composites fabricated using an aqueous slurry process

Unidirectional composites from unsized carbon fiber and LaRC-TPI matrix material were fabricated using 'high flow' and'medium flow' grades of the LaRC-TPI 1500 series of polyimides. Prepreg was drum-wound from a slurry composed of the polyimide powder dispersed in an aqueous solution of LaRC-TPI poly(amide acid). The poly(amide acid) was found to be an effective binding agent in the prepregging process. Composite short beam shear and flexure properties were measured at room and elevated temperatures (to 177 C) with both dry and moisture-saturated specimens. The mechanical properties observed for composites fabricated from the high and medium flow materials were virtually identical. Additionally, double cantilever beam measurements showed nearly equivalent fracture toughness for the two composite materials.

Towell, Timothy W.↗
NASA NTRS1991

Advanced thermoplastic resins, phase 1

Eight thermoplastic polyimide resin systems were evaluated as composite matrix materials. Two resins were selected for more extensive mechanical testing and both were versions of LaRC-TPI (Langley Research Center - Thermoplastic Polyimide). One resin was made with LaRC-TPI and contained 2 weight percent of a di(amic acid) dopant as a melt flow aid. The second system was a 1:1 slurry of semicrystalline LaRC-TPI powder in a polyimidesulfone resin diglyme solution. The LaRC-TPI powder melts during processing and increases the melt flow of the resin. Testing included dynamic mechanical analysis, tension and compression testing, and compression-after-impact testing. The test results demonstrated that the LaRC-TPI resins have very good properties compared to other thermoplastics, and that they are promising matrix materials for advanced composite structures.

Hendricks, C. L.↗
NASA NTRS1991

A Process for Preparing 1,3-Diamino-5-Pentafluorosulfanylbenzene and Polymers Therefrom

Diamines have shown their utility in the formation of many polymers. Examples of these polymers include polyimides, polyamides, and epoxies. The properties of these polymers are often dependent on the diamine which is used to make the polymer. By the present invention, a process was developed to make a diamine containing pentafluorosulfanylbenzene moiety. This process involves two steps: the preparation of a dinitro precursor and the reduction of the dinitro compound to form the diamine. This diamine was then reacted with various dianhydrides, diacidchlorides, and epoxy resins to yield the corresponding polyimide, polyamide, and epoxy polymers. These polymers were then used to make films, a wire coating enamel, and a semi-permeable membrane. The novelty of this invention resides in the process to make the diamine. Traditionally, dinitro compounds are reduced with hydrazine or a catalyst such as palladium on charcoal. The catalyst which is used in this invention is platinum oxide. When this catalyst is used, it makes it possible to form a polymer-grade diamine.

St.clair, Anne K.↗
NASA NTRS1992

Synergistic effects of ultraviolet radiation, thermal cycling, and atomic oxygen on altered and coated Kapton surfaces

The photovoltaic (PV) power system for Space Station Freedom (SSF) uses solar array blankets which provide structural support for the solar cells and house the electrical interconnections. In the low Earth orbital (LEO) environment where SSF will be located, surfaces will be exposed to potentially damaging environmental conditions including solar ultraviolet (UV) radiation, thermal cycling, and atomic oxygen. It is necessary to use ground based tests to determine how these environmental conditions would affect the mass loss and optical properties of candidate SSF blanket materials. Silicone containing, silicone coated, and SiO(x) coated polyimide film materials were exposed to simulated LEO environmental conditions to determine there durability and whether the environmental conditions of UV, thermal cycling and oxygen atoms act synergistically on these materials. A candidate PV blanket material called AOR Kapton, a polysiloxane polyimide cast from a solution mixture, shows an improvement in durability to oxygen atoms erosion after exposure to UV radiation or thermal cycling combined with UV radiation. This may indicate that the environmental conditions react synergistically with this material, and the damage predicted by exposure to atomic oxygen alone is more severe than that which would occur in LEO where atomic oxygen, thermal cycling and UV radiation are present together.

Dever, Joyce A.↗
NASA NTRS1992

Orbital transfer rocket engine technology program: Soft wear ring seal technology

Liquid oxygen (LOX) compatibility tests, including autogenous ignition, promoted ignition, LOX impact tests, and friction and wear tests on different PV products were conducted for several polymer materials as verification for the implementation of soft wear ring seals in advanced rocket engine turbopumps. Thermoplastics, polyimide based materials, and polyimide-imide base materials were compared for oxygen compatibility, specific wear coefficient, wear debris production, and heat dissipation mechanisms. A thermal model was generated that simulated the frictional heating input and calculated the surface temperature and temperature distribution within the seal. The predictions were compared against measured values. Heat loads in the model were varied to better match the test data and determine the difference between the measured and the calculated coefficients of friction.

Lariviere, Brian W.↗
NASA NTRS1992

Semi-interpenetrating polymer network for tougher and more microcracking resistant high temperature polymers

This invention is a semi-interpenetrating polymer network which includes a high performance thermosetting polyimide having a nadic end group acting as a crosslinking site and a high performance linear thermoplastic polyimide. An improved high temperature matrix resin is provided which is capable of performing at 316 C in air for several hundreds of hours. This resin has significantly improved toughness and microcracking resistance, excellent processability and mechanical performance, and cost effectiveness.

Pater, Ruth H.↗