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NASA NTRS1986

Specimen geometry effects on graphite/PMR-15 composites during thermo-oxidative aging

Studies were conducted to establish the effects of specimen geometry on the thermo-oxidative stability and the mechanical properties retention of unidirectional Celion 12000 graphite fiber reinforced PMR-15 polyimide composites. Weight loss, flexural strength and interlaminar shear strength are measured at isothermal aging times as long as 1639 hr at a temperature of 316 C for three different specimen geometries. It is found that the three different types of specimen surfaces exhibit different values of weight loss/unit area. The mechanical properties retention is also found to be dependent on geometry for these composites. The interlaminar shear strength decreases significantly over the complete range of aging times. The flexural strength retention starts showing geometric dependency after about 1000 hr of aging at 316C. Weight loss fluxes, associated with the three different types of exposed surfaces, are calculated and used to develop an empirical mathematical model for predicting the weight loss behavior of unidirectional composites of arbitrary geometries. Data are presented comparing experimentally determined weight loss with weight loss values predicted using the empirical model.

Bowles, K. J.↗

NASA NTRS1986

Specimen geometry effects on graphite/PMR-15 composites during thermo-oxidative aging

Studies were conducted to establish the effects of specimen geometry on the thermo-oxidative stability and the mechanical properties retention of unidirectional Celion 12000 graphite fiber reinforced PMR-15 polyimide composites. Weight loss, flexural strength and interlaminar shear strength are measured at isothermal aging times as long as 1639 hr at a temperature of 316 C for three different specimen geometries. It is found that the three different types of specimen surfaces exhibit different values of weight loss/unit area. The mechanical properties retention is also found to be dependent on geometry for these composites. The interlaminar shear strength decreases significantly over the complete range of aging times. The flexural strength retention starts showing geometric dependency after about 1000 hr of aging at 316 C. Weight loss fluxes, associated with the three different types of exposed surfaces, are calculated and used to develop an empirical mathematical model for predicting the weight loss behavior of unidirectional composites of arbitrary geometries. Data are presented comparing experimentally determined weight loss with weight loss values predicted using the empirical model.

Bowles, K. J.↗

NASA NTRS1994

Mechanical Tests For Monitoring Aging Of Composites

Experimental study addresses related topics of thermo-oxidative aging of PMR-15 (polyimide matrix/graphite-fiber composite materials) strengths of interfacial bonds, effects of various surface treatments, and relative merits of mechanical tests yielding measures of strengths of materials.

Bowles, Kenneth J.↗

NASA NTRS1992

Transverse flexural tests as a tool for assessing damage to PMR-15 composites from isothermal aging in air at elevated temperatures

To date, the effect of thermo-oxidative aging on unidirectional composite mechanical properties has been monitored by the measurement of interlaminar shear strength (ILSS) and either three or four point longitudinal flexural strength (LFS) of the composites being tested. Both results are affected by the fiber-to-matrix bonding, the former being dependent on the shear resistance of the interface and the latter on the degree of load sharing by the fibers through the fiber/matrix interface. Recently, fiber/matrix interfacial bond strengths have been monitored using a transverse flexural strength (TFS) test method. This test method was used to evaluate the effect of fiber surface treatment on the fiber/matrix bond. The interface bonding was varied in these tests using Hercules A-fibers with three-types of surfaces that produce bonds of poor, better, and good quality. The TFS was found not only to be sensitive to the bonding, but also to the aging time of unidirectional A-fiber/PMR-15 composites. This relationship reflects the mechanism by which the PMR-15 degrades during thermal aging.

Bowles, Kenneth J.↗

NASA NTRS1993

Transverse flexural tests as a tool for assessing damage to PMR-15 composites from isothermal aging in air at elevated temperatures

Bowles, Kenneth J.↗

NASA NTRS1979

Resin/fiber thermo-oxidative interactions in PMR polymide/graphite composites

The amounts of resin weight loss and fiber weight loss in four PMR-polyimide graphite fiber composites were calculated from the composite weight losses and the fiber/resin ratios of the composites after long term thermo-oxidative aging in 600 F air. The accelerating effect of graphite fiber on resin weight loss, compared to neat resin weight loss, indicated the presence of a deleterious resin/fiber thermo-oxidative interaction, presumably due to fiber impurities. Similarly, the decelerating effect of the protective matrix resin on fiber weight loss, compared to bare fiber weight loss, was also demonstrated. The amount of hydrazine-indigestible resin and the amount of loose surface graphite fiber that formed during 600 deg F exposure of the composites were quantitatively determined. The indigestible residual resin was also qualitatively studied by scanning electron microscopy.

Alston, W. B.↗

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 NTRS1994

Thermo-Oxidative Stability of Graphite/PMR-15 Composites: Effect of Fiber Surface Modification on Composite Shear Properties

Experiments were conducted to establish a correlation between the weight loss of a polyimide (PMR- 15) matrix and graphite fibers and the in-plane shear properties of their unidirectional composites subjected to different isothermal aging times up to 1000 hr at 316 C. The role of fiber surface treatment on the composite degradation during the thermo-oxidative aging was investigated by using A4 graphite fibers with three surface modifications: untreated (AU-4), surface treated (AS-4), and surface treated and sized with an epoxy-compatible sizing (AS-4G). The weight loss of the matrix fibers, and composites was determined during the aging. The effect of thermal aging was seen in all the fiber samples in terms of weight loss and reduction in fiber diameter. Calculated values of weight loss fluxes for different surfaces of rectangular unidirectional composite plates showed that the largest weight loss occurred at those cut surfaces where fibers were perpendicular to the surface. Consequently, the largest amount of damage was also noted on these cut surfaces. Optical observation of the neat matrix and composite plates subjected to different aging times revealed that the degradation (such as matrix microcracking and void growth) occurred in a thin surface layer near the specimen edges. The in-plane shear modulus of the composites was unaffected by the fiber surface treatment and the thermal aging. The shear strength of the composites with the untreated fibers was the lowest and it decreased with aging. A fracture surface examination of the composites with untreated fibers suggested that the weak interface allowed the oxidation reaction to proceed along the interface and thus expose the inner material to further oxidation. The results indicated that the fiber-matrix interface affected the composite degradation process during its thermal aging and that the the weak interface accelerated the composite degradation.

Madhukar, Madhu S.↗

NASA NTRS1985

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.↗

NASA NTRS1988

Thermo-oxidative stability studies of Celion 6000/PMR-15 unidirectional composites, PMR-15, and Celion 6000 fiber

Experimental results on the influence of the thermooxidative resistance characteristics of the fiber and matrix resin on the thermal stability of isothermally aged Celion 6000/PMR-15 matrix resin composites are presented. SEM studies reveal that extreme oxidative erosion of the graphite fiber occurs at elevated temperatures in the presence of the polyimide matrix. The activation energy of oxidation of the composite was shown to be greater than those of the fiber and the matrix resin.

Bowles, Kenneth J.↗

NASA NTRS1991

A comparison of fiber effects on polymer matrix composite oxidation

A number of thermo-oxidative stability studies addressing the effects of fiber reinforcement on composite thermal stability and influence of geometry on the results of aging studies were performed at NASA-Lewis. The information presented herein, a compilation of some results from these studies, shows the influence of the reinforcement fibers on the oxidative degradation of various PMR-15 composites. Reinforcement of graphite and ceramics were studied and three composite oxidation mechanisms were observed. One was a dominant attack of the reinforcement fiber, the second was the aggressive oxidation of the matrix material, and the third was interfacial degradation.

Bowles, Kenneth J.↗

NASA NTRS1992

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

A number of studies have investigated the thermooxidative 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. The polyimide PMR-15 was the matrix material used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-4OR 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. 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, K. J.↗

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 NTRS1993

Thermal stability relationships between PMR-15 resin and its composites

A study was conducted to investigate the relationship between the thermo-oxidative stability of PMR-15 matrix resin and the stability of graphite-fiber-reinforced composites that contain this resin as the matrix material. Three areas were investigated. The first was the effect of fiber/matrix interfacial bond strength on the isothermal aging weight loss of composites. By using type-A graphite fibers produced by Hercules, it was possible to study composites reinforced with fibers that were processed to receive different surface treatments. One of the fibers was untreated, a second fiber was treated by oxidation to enhance fiber/matrix bonding, and the third type of fiber was coated with an epoxy sizing. These treatments produced three significantly different interfacial bond strengths. The epoxy sizing on the third fiber was quickly oxidized from the bare fiber surfaces at 288, 316, and 343 C. The weight loss due to the removal of the sizing was constant at 1.5 percent. This initial weight loss was not observed in thermo-oxidative stability studies of composites. The PMR-15 matrix satisfactorily protected the reinforcemnt at all three temperatures.

Bowles, Kenneth J.↗

NASA NTRS1992

Cyclopentadiene evolution during pyrolysis-gas chromatography of PMR polyimides

The effect of formulated molecular weight (FMW), extent of cure, and cumulative aging on the amount of cyclopentadiene (CPD) evolved from Polymerization of Monomeric Reactants (PMR) polyimides were investigated by pyrolysis-gas chromotography (PY-GC). The PMR polyimides are additional crosslinked resins formed from an aromatic diamine, a diester of an aromatic tetracarboxylic acid and a monoester of 5-norbornene-2, 3-dicarboxylic acid. The PY-GC results were related to the degree of crosslinking and to the thermo-oxidative stability (weight loss) of PMR polyimides. Thus, PY-GC has shown to be a valid technique for the characterization of PMR polyimide resins and composites via correlation of the CPD evolved versus the thermal history of the PMR sample.

Alston, William B.↗

NASA NTRS1992

Structure-to-property relationships in addition cured polymers. 4: Correlations between thermo-oxidative weight losses of norbornenyl cured polyimide resins and their composites

Relationships are identified between the thermo-oxidative stability (TOS) at 316 C of a wide variety of PMR (polymerization of monomeric reactants) addition cured polyimide resins and their corresponding graphite fiber composites. Weight loss results at 316 C confirmed the expected relationship of increasing aliphatic endcap content with decreasing TOS. Moreover, the resin TOS study also showed an unexpected linear correlation of decreasing weight loss to increasing ratio of benzylic diamine to aliphatic endcap in the range of the stoichiometries studied. Only after long term 316 C aging does the dianhydride used with the benzylic diamines become an additional factor in influencing the amount of PMR resin and composite weight losses. Also, the benzylic systems consistently showed much lower resin and composite weight losses at 316 C than the corresponding nonbenzylic norbornenyl resins and composites, except when the nonbenzylic diamine monomer does not contain a connecting group. Instead, this diamine resulted in a 316 C resin and composite weight loss that was only competitive with benzylic type diamines. Results show excellent correlation between TOS of all graphite fiber PMR composites and resins.

Alston, William B.↗

NASA NTRS1979

Second generation PMR polyimide/fiber composites

A second generation polymerization monomeric reactants (PMR) polyimdes matrix system (PMR 2) was characterized in both neat resin and composite form with two different graphite fiber reinforcements. Three different formulated molecular weight levels of laboratory prepared PMR 2 were examined, in addition to a purchased experimental fully formulated PMR 2 precurser solution. Isothermal aging of graphite fibers, neat resin samples and composite specimens in air at 316 C were investigated. Humidity exposures at 65 C and 97 percent relative humidity were conducted for both neat resin and composites for eight day periods. Anaerobic char of neat resin and fire testing of composites were conducted with PMR 15, PMR 2, and an epoxy system. Composites were fire tested on a burner rig developed for this program. Results indicate that neat PMR 2 resins exhibit excellent isothermal resistance and that PMR 2 composite properties appear to be influenced by the thermo-oxidative stability of the reinforcing fiber.

Cavano, P. J.↗

NASA NTRS1990

Autoclavable addition polyimides for 371 C composite applications

Studies were conducted to improve the thermo-oxidative stability (TOS) of PMR type polyimides by the substitution of para-aminostyrene (PAS) for the nadic ester endcap in second generation PMR polyimides (PMR-2). The nadic endcap which provides the PMR polyimides with their relative ease of fabrication, both by limiting the molecular weight of the prepolymer and by undergoing the final addition cure without volatiles, is also the weak link with regard to TOS. A polyimide formulated with PAS endcaps, called V-CAP, utilizes a two step reaction sequence similar to that of the PMR polyimides and can be easily autoclave molded into low void composite materials. Resin studies included two formulations of both PMR-2 and V-CAP, corresponding to n=9 and n=14 prepolymer stoichiometry. Unidirectional reinforced T40R graphite fiber laminates were fabricated from each of the resins was post-cured in either air at 385 C or nitrogen at 400 C. Composite specimens were aged in air at 371 C and mechanical properties were measured at 371 C before and after exposure.

Vannucci, R. D.↗