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NASA NTRS1998

High Temperature Mechanical Characterization of Ceramic Matrix Composites

A high temperature mechanical characterization laboratory has been assembled at NASA Lewis Research Center. One contribution of this work is to test ceramic matrix composite specimens in tension in environmental extremes. Two high temperature tensile testing systems were assembled. The systems were assembled based on the performance and experience of other laboratories and meeting projected service conditions for the materials in question. The systems use frames with an electric actuator and a center screw. A PC based data acquisition and analysis system is used to collect and analyze the data. Mechanical extensometers are used to measure specimen strain. Thermocouples, placed near the specimen, are used to measure the specimen gage section temperature. The system for testing in air has a resistance element furnace with molybdenum disilicide elements and pneumatic grips with water cooling attached to hydraulic alignment devices. The system for testing in an inert gas has a graphite resistance element furnace in a chamber with rigidly mounted, water cooled, hydraulically actuated grips. Unidirectional SiC fiber reinforced reaction bonded Si3N4 and triaxially woven, two dimensional, SiC fiber reinforced enhanced SiC composites were tested in unidirectional tension. Theories for predicting the Young's modulus, modulus near the ultimate strength, first matrix cracking stress, and ultimate strength were applied and evaluated for suitability in predicting the mechanical behavior of SiC/RBSN and enhanced SiC/SiC composites. The SiC/RBSN composite exhibited pseudo tough behavior (increased area under the stress/strain curve) from 22 C to 1500 C. The rule of mixtures provides a good estimate of the Young's modulus of the SiC/RBSN composite using the constituent properties from room temperature to 1440 C for short term static tensile tests in air or nitrogen. The rule of mixtures significantly overestimates the secondary modulus near the ultimate strength. The ACK theory provides the best approximation of the first matrix cracking stress when residual stresses are ignored. The theory of Cao and Thouless, based on Weibull statistics, gave the best prediction for the composite ultimate strength. The enhanced SiC/SiC composite exhibited nonlinear stress/strain behavior from 24 C to 1370 C in air with increased ultimate strain when compared to monolithic SiC. The theory of Yang and Chou with the assumption of a frictional fiber/matrix interface provided the best estimate of the Young's modulus. The theory of Cao and Thouless gave the best estimate for the ultimate strength.

Gyekenyesi, John Z.↗

NASA NTRS1984

Phosphorus-containing imide resins - Modification by elastomers

The syntheses and general features of addition-type maleimide resins based on bis(m-aminophenyl)phosphine oxide and tris(m-aminophenyl)phosphine oxide have been reported previously. These resins have been used to fabricate graphite cloth laminates having excellent flame resistance. These composites did not burn even in pure oxygen. However, these resins were somewhat brittle. This paper reports the modification of these phosphorus-containing resins by an amine-terminated butadiene-acrylonitrile copolymer (ATBN) and a perfluoroalkylene diaromatic amine elastomer (3F). An approximately two-fold increase in short beam shear strength and flexural strength was observed at 7 percent ATBN concentration. The tensile, flexural, and shear strengths were reduced when 18 percent ATBN was used. Anaerobic char yields of the resins at 800 C and the limiting oxygen indexes of the laminates decreased with increasing ATBN concentration. The perfluorodiamine (3F) was used with both imide resins at 6.4 percent concentration. The shear strength was doubled in the case of the bisimide with no loss of flammability characteristics. The modified trisimide laminate also had improved properties over the unmodified one. The dynamic mechanical analysis of a four-ply laminate indicated a glass transition temperature above 300 C. Scanning electron micrographs of the ATBN modified imide resins were also recorded.

Varma, I. K.↗

NASA NTRS1991

Temperature effects on high strain rate properties of graphite/epoxy composites

A unidirectional graphite epoxy material (AS4/3501-6) was characterized at strain rates ranging from 5 x 10(exp 6) s(exp -1) to 5(exp -1), at room temperature and at 128 C. Results are presented in the form of stress-strain curves to failure. The longitudinal properties remain nearly unchanged with strain rate and temperature. The transverse modulus increases with strain rate but decreases with temperature. The transverse strength and transverse ultimate tensile strain have a positive rate sensitivity at low rates, which changes to negative at intermediate rates and returns to positive rate sensitivity at the highest rates tested. A temperature-time equivalence principle was applied and master curves were obtained for the transverse mechanical properties. The in-plane shear modulus and in-plane shear strength have a positive rate sensitivity. The ultimate intralaminar shear strain has a positive rate sensitivity at low rates, which changes to negative at high rates. At the elevated temperature of 128 C, the ultimate shear strain is 25 to 30 percent higher than the room temperature value, but its strain rate dependence is moderate.

Yaniv, G.↗

NASA NTRS1984

Space Radiation Effects on Graphite-Epoxy Composite Materials

Radiation effects on engineering properties, dimensional stability, and chemistry on state of the art composite systems were characterized. T300/934 graphite-epoxy composite was subjected to 1.0 MeV electron radiation for a total dose of 1.0 x 10(10) rads at a rate of 5.0 x 10(7) rads/hour. This simulates a worst case exposure equivalent to 30 years in space. Mechanical testing was performed on he 4-ply unidirectional laminates over the temperature range of -250 F (116K) to +250 F (394K). A complete set of in-plane tensile elastic and strength properties were obtained (E sub 1, E sub 2, nu sub 12, G sub 12, X sub T, Y sub T, and S). In addition electron microscopy was used to study and analyze the fracture surfaces of all specimens tested. Results indicate that little difference in properties is noted at room temperature, but significant differences are observed at both low and elevated temperatures.

Milkovich, S. M.↗

NASA NTRS1981

The effect of resin on the impact damage tolerance of graphite-epoxy laminates

The effect of the matrix resin on the impact damage tolerance of graphite-epoxy composite laminates was investigated. The materials were evaluated on the basis of the damage incurred due to local impact and on their ability to retain compression strength in the presence of impact damage. Twenty-four different resin systems were evaluated. Five of the systems demonstrated substantial improvements compared to the baseline system including retention of compression strength in the presence of impact damage. Examination of the neat resin mechanical properties indicates the resin tensile properties influence significantly the laminate damage tolerance and that improvements in laminate damage tolerance are not necessarily made at the expense of room temperature mechanical properties. Preliminary results indicate a resin volume fraction on the order of 40 percent or greater may be required to permit the plastic flow between fibers necessary for improved damage tolerance.

Williams, J. G.↗

NASA NTRS1988

Degradation of graphite-epoxy due to electron radiation

Experimental results are presented showing that electron irradiation has a variable effect on the properties of graphite-epoxy depending upon the test temperature and the property of interest. In general, compression properties are improved at cold temperature and degraded at elevated temperature. With the exception of some moduli, tensile and shear properties are degraded at both cold and elevated temperatures. Electron irradiation lowers the glass transition temperature of graphite/epoxy significantly. Property degradation of irradiated materials at the elevated temperature is associated with the reduction in Tg. It is shown that a (0) compression-strength test is the most sensitive test for exhibiting the effects of electron irradiation. Results from tests on neat resin also show that the bulk matrix is degraded after irradiation, and that the correlation between resin and composite response is good.

Herakovich, C. T.↗

NASA NTRS1986

Space radiation effects on the thermo-mechanical behavior of graphite-epoxy composites

This investigation of composite material properties utilized T300/934 graphite-epoxy that was subjected to 1.0 MeV electron radiation for a total dose of 1.0 x 10 to the 10th rads at a rate of 5.0 x 10 to the 7th rads/hour, simulating a worst-case exposure equivalent to 30 years in space. Mechanical testing was performed on 4-ply unidirectional laminates over the temperature range of -250 F (116 K) to +250 F (394 K). In-plane elastic tensile and shear properties as well as strength were obtained. The results show that electron radiation degrades the epoxy matrix and produces products that volatilize at the temperatures considered. These degradation products plasticize the epoxy at elevated temperatures and embrittle it at low temperatures, thereby altering the mechanical properties of the composite.

Milkovich, Scott M.↗

NASA NTRS1992

Mechanical properties of triaxially braided composites: Experimental and analytical results

This paper investigates the unnotched tensile properties of two-dimensional triaxial braid reinforced composites from both an experimental and analytical viewpoint. The materials are graphite fibers in an epoxy matrix. Three different reinforcing fiber architectures were considered. Specimens were cut from resin transfer molded (RTM) composite panels made from each braid. There were considerable differences in the observed elastic constants from different size strain gage and extensometer readings. Larger strain gages gave more consistent results and correlated better with the extensometer readings. Experimental strains correlated reasonably well with analytical predictions in the longitudinal, zero degree, fiber direction but not in the transverse direction. Tensile strength results were not always predictable even in reinforcing directions. Minor changes in braid geometry led to disproportionate strength variations. The unit cell structure of the triaxial braid was discussed with the assistence of computer analysis of the microgeometry. Photomicrographs of the braid geometry were used to improve upon the computer graphics representations of unit cells. These unit cells were used to predict the elastic moduli with various degrees of sophistication. The simple and the complex analyses were generally in agreement but none adequately matched the experimental results for all the braids.

Masters, John E.↗

NASA NTRS1992

Mechanical properties of triaxially braided composites: Experimental and analytical results

The unnotched tensile properties of 2-D triaxial braid reinforced composites from both an experimental and an analytical viewpoint are studied. The materials are graphite fibers in an epoxy matrix. Three different reinforcing fiber architectures were considered. Specimens were cut from resin transfer molded (RTM) composite panels made from each braid. There were considerable differences in the observed elastic constants from different size strain gage and extensometer reading. Larger strain gages gave more consistent results and correlated better with the extensometer reading. Experimental strains correlated reasonably well with analytical predictions in the longitudinal, 0 degrees, fiber direction but not in the transverse direction. Tensile strength results were not always predictable even in reinforcing directions. Minor changes in braid geometry led to disproportionate strength variations. The unit cell structure of the triaxial braid was discussed with the assistance of computer analysis of the microgeometry. Photomicrographs of braid geometry were used to improve upon the computer graphics representations of unit cells. These unit cells were used to predict the elastic moduli with various degrees of sophistication. The simple and the complex analyses were generally in agreement but none adequately matched the experimental results for all the braids.

Masters, John E.↗

NASA NTRS1980

Creep rupture behavior of unidirectional advanced composites

A 'material modeling' methodology for predicting the creep rupture behavior of unidirectional advanced composites is proposed. In this approach the parameters (obtained from short-term tests) required to make the predictions are the three principal creep compliance master curves and their corresponding quasi-static strengths tested at room temperature (22 C). Using these parameters in conjunction with a failure criterion, creep rupture envelopes can be generated for any combination of in-plane loading conditions and ambient temperature. The analysis was validated experimentally for one composite system, the T300/934 graphite-epoxy system. This was done by performing short-term creep tests (to generate the principal creep compliance master curves with the time-temperature superposition principle) and relatively long-term creep rupture tensile tests of off-axis specimens at 180 C. Good to reasonable agreement between experimental and analytical results is observed.

Yeow, Y. T.↗

NASA NTRS1993

The effects of aircraft fuel and fluids on the strength properties of Resin Transfer Molded (RTM) composites

The resin transfer molding (RTM) process offers important advantages for cost-effective composites manufacturing, and consequently has become the subject of intense research and development efforts. Several new matrix resins have been formulated specifically for RTM applications in aircraft and aerospace vehicles. For successful use on aircraft, composite materials must withstand exposure to the fluids in common use. The present study was conducted to obtain comparative screening data on several state-ofthe-art RTM resins after environmental exposures were performed on RTM composite specimens. Four graphite/epoxy composites and one graphite/bismaleimide composite were tested; testing of two additional graphite epoxy composites is in progress. Zero-deg tension tests were conducted on specimens machined from eight-ply (+45-deg, -45-deg) laminates, and interlaminar shear tests were conducted on 32-ply 0-deg laminate specimens. In these tests, the various RTM resins demonstrated widely different strengths, with 3501-6 epoxy being the strongest. As expected, all of the matrix resins suffered severe strength degradation from exposure to methylene chloride (paint stripper). The 3501-6 epoxy composites exhibited about a 30 percent drop in tensile strength in hot, wet tests. The E905-L epoxy exhibited little loss of tensile strength (less than 8 percent) after exposure to water. The CET-2 and 862 epoxies as well as the bismaleimide exhibited reduced strengths at elevated temperature after exposure to oils and fuel. In terms of the percentage strength reductions, all of the RTM matrix resins compared favorably with 3501-6 epoxy.

Falcone, Anthony↗

NASA NTRS1985

Fatigue Damage in Notched Composite Laminates Under Tension-Tension Cyclic Loads

The results are given of an investigation to determine the damage states which develop in graphite epoxy laminates with center holes due to tension-tension cyclic loads, to determine the influence of stacking sequence on the initiation and interaction of damage modes and the process of damage development, and to establish the relationships between the damage states and the strength, stiffness, and life of the laminates. Two quasi-isotropic laminates were selected to give different distributions of interlaminar stresses around the hole. The laminates were tested under cyclic loads (R=0.1, 10 Hz) at maximum stresses ranging between 60 and 95 percent of the notched tensile strength.

Stinchcomb, W. W.↗

NASA NTRS1971

High performance filament wound composites for pressure vessel applications.

A new high modulus fiber was evaluated as a reinforcement for filament wound pressure vessels. Based on preliminary data it offers significant specific strength and modulus improvements over an S-glass reinforcement. Winding parameters and design data were established for the fiber with two different epoxy resin systems. NOL composite rings were evaluated for tensile strength, modulus and interlaminar shear strength at +70 F, -320 F and -423 F. Results showed that the fiber reinforced composite exhibited a specific strength of 4,100,000 inches and a specific modulus of 290,000,000 inches compared to 3,260,000 inches and 110,000,000 inches respectively for S-glass. Utilizing this data to design small filament wound pressure vessels, a performance factor of 806,000 inches was obtained experimentally with PRD 49-1 fiber compared to values of 632,000 inches and 501,000 inches for S-glass and high modulus graphite vessels, respectively.

Hoggatt, J. T.↗

NASA NTRS1982

A compliant, high failure strain, fibre-reinforced glass-matrix composite

A glass-matrix composite reinforced by discontinuous graphite fibers was produced by hot pressing glass-powder-impregnated two-dimensional arrays of in-plane randomly oriented graphite fibers held together by approximately 5-10% by weight of organic binder (generally polyester). The composite tensile behavior is characterized by a highly nonlinear stress-strain curve which differs markedly from that of either unreinforced glass or a similarly reinforced epoxy-matrix composite. By virtue of this nonlinearity, the composite is able to redistribute applied stresses to achieve a high load-carrying capacity. The fibrous microstructure and the low fiber-matrix bond provide a mechanism for achieving high fracture toughness and unusually high compliance. For a 96%-silica-matrix composite, the strength is retained to over 1000 C.

Prewo, K. M.↗

NASA NTRS1986

Thermally induced transverse cracking in graphite-epoxy cross-ply laminates

Thermally induced transverse cracking in T300/5208 graphite-epoxy cross-ply laminates was investigated experimentally and theoretically. The six laminate configurations studied were: 0/90(3)s, 0(2)/90(2)s, 0(3)/90s, 90/0(3)s, 90(2)/0(2)s, and 90(3)/0s. The thermal load required to initiate transverse cracking was determined experimentally and compared to a theoretical prediction. Experimental results for the accumulation of transverse cracks under cyclic thermal loading between - 250 and 250 F for up to 500 thermal cycles are presented. The calculated in situ transverse-lamina strength was determined to be at least 1.9 times the unidirectional-lamina transverse tensile strength. All laminate configurations exhibited an increase in crack density with increasing thermal cycles.

Adams, D. S.↗

NASA NTRS1985

Fracture morphology of 2-D carbon-carbon composition

Out-of-plane tensile tests of a woven fabric carbon-carbon composite were performed in a scanning electron microscope equipped with a tensile stage and a videotape recording system. The composite was prepared from T-300 8-harness satin graphite fabric and a phenolic resin. The (0/90/0/90/0 sub 1/2) sub 2 laminate, with a Theta describing the orientation of the warp fibers of the fabric, was cured at 160 C and pyrolized at 871 C. This was followed by four cycles of resin impregnation, curing, and pyrolysis. A micrograph of the cross section of the composite is presented. Inspection of the specimen fracture surface revealed that the filaments had no residual matrix bonded to them. Further inspection revealed that the fracture was interlaminar in nature. Failure occurred where filaments of adjacent plies had the same orientation. Thus it is postulated that improvement in transverse tensile strength of 2-D carbon-carbon depends on the improvement of the filament-matrix bond strength.

Avery, W. B.↗

NASA NTRS1985

Response of thick, notched laminates subjected to tension-compression cyclic loads

The fatigue response of a (0/24/90/-45)s4 T300-5208 graphite-epoxy laminate with a drilled centerhole subjected to fully reversed tension-compression (R=-1, T-C) constant amplitude loading was investigated. Damage evaluation techniques such as stiffness monitoring, penetrant-enchanced X-ray radiography, C-scan, laminate deeply and residual strength were used to establish the mechanisms of damage development as well as the relations between this damage and the stiffness, strength and life of the laminate. Damage initiated at the hole as matrix cracking parallel to the fibers in all plies. Matrix cracks had a significant effect on delamination initiation and growth. Delaminations initiated near the surface in the densely cracked region at the hole and grew along major matrix cracks. Compressive properties degraded more rapidly than tensile properties. At the stress levels used, residual tensile strength increased early in the fatigue life and remained approximately constant to near the end of life, when failure was precipitated by excessive laminate instability during the compressive portion of the loading.

Bakis, C. E.↗

NASA NTRS1986

Response of thick, notched laminates subjected to tension-compression cyclic loads

The fatigue response of a (0/24/90/-45)s4 T300-5208 graphite-epoxy laminate with a drilled centerhole subjected to fully reversed tension-compression (R=-1, T-C) constant amplitude loading was investigated. Damage evaluation techniques such as stiffness monitoring, penetrant-enhanced X-ray radiography, C-scan, laminate deply and residual strength were used to establish the mechanisms of damage development as well as the relations between this damage and the stiffness, strength and life of the laminate. Damage initiated at the hole as matrix cracking parallel to the fibers in all plies. Matrix cracks had a significant effect on delamination initiation and growth. Delaminations initiated near the surface in the densely cracked region at the hole and grew along major matrix cracks. Compressive properties degraded more rapidly than tensile properties. At the stress levels used, residual tensile strength increased early in the fatigue life and remained approximately constant to near the end of life, when failure was precipitated by excessive laminate instability during the compressive portion of the loading.

Bakis, C. E.↗