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NASA NTRS1980

Coatings for Graphite Fibers

Several approaches for applying high resistance coatings continuously to graphite yarn were investigated. Two of the most promising approaches involved (1) chemically vapor depositing (CVD) SiC coatings on the surface of the fiber followed by oxidation, and (2) drawing the graphite yarn through an organo-silicone solution followed by heat treatments. In both methods, coated fibers were obtained which exhibited increased electrical resistances over untreated fibers and which were not degraded. This work was conducted in a previous program. In this program, the continuous CVD SiC coating process used on HTS fiber was extended to the coating of HMS, Celion 6000, Celion 12000 and T-300 graphite fiber. Electrical resistances three order of magnitude greater than the uncoated fiber were measured with no significant degradation of the fiber strength. Graphite fibers coated with CVD Si3N4 and BN had resistances greater than 10(exp 6) ohm/cm. Lower pyrolysis temperatures were used in preparing the silica-like coatings also resulting in resistances as high as three orders of magnitude higher than the uncoated fiber. The epoxy matrix composites prepared using these coated fibers had low shear strengths indicating that the coatings were weak.

Galasso, F. S.↗

NASA NTRS1980

Properties of PMR polyimide composites made with improved high strength graphite fibers

Recent graphite fiber developments have resulted in high strength, intermediate modulus graphite fibers having improved thermo-oxidative resistance. These improved fibers, obtained from various commercial suppliers, were used to fabricate PMR-15 and PMR-11 polyimide composites. Studies were performed to investigate the effects of the improved high strength graphite fibers on composite properties after exposure in air at 600 F. The use of the more oxidatively resistant fibers did not result in improved performance at 600 F. Two of the improved fibers were found to have an adverse effect on the long-term performance of PMR composites. The influence of various factors such as fiber physical properties, surface morphology and chemical composition are also discussed.

Vannucci, R. D.↗

NASA NTRS1997

First Single-Crystal Mullite Fibers

Ceramic-matrix composites strengthened by suitable fiber additions are being developed for high-temperature use, particularly for aerospace applications. New oxide-based fibers, such as mullite, are particularly desirable because of their resistance to high-temperature oxidative environments. Mullite is a candidate material in both fiber and matrix form. The primary objective of this work was to determine the growth characteristics of single-crystal mullite fibers produced by the laser-heated floating zone method. Directionally solidified fibers with nominal mullite compositions of 3Al2O3 2SiO2 were grown by the laser-heated floating zone method at the NASA Lewis Research Center. SEM analysis revealed that the single-crystal fibers grown in this study were strongly faceted and that the facets act as critical flaws, limiting fiber strength. The average fiber tensile strength is 1.15 GPa at room temperature. The mullite fibers exhibit superior strength retention (80 percent of their room temperature tensile strength at 1450 C). Examined by transmission electron microscopy, these mullite single crystals are free of dislocations, low-angle boundaries, and voids. In addition, they show a high degree of oxygen vacancy ordering. High-resolution digital images from an optical microscope furnish evidence of the formation of a liquid-liquid miscibility gap during crystal growth. These images represent the first experimental evidence of liquid immiscibility for these compositions and temperatures. Continuing investigation with controlled seeding of mullite single crystals is planned.

Source record↗

NASA NTRS1977

Graphite/epoxy pressure vessels lined with ultra-thin titanium

Filament-wound, titanium-lined, fiber/epoxy pressure vessels were made using a very high-strength graphite fiber (3570-MPa typical fiber strength). The 0.254-mm-thick titanium liner was used to improve burst performance. The pressure vessels achieved an average burst performance of 241 kPa.cu m/kg, and the fatigue life of titanium liners with good welds (cycled to 50% of the average expected burst pressure) was in excess of 2000 cycles.

Hamstad, M. A.↗

NASA NTRS2012

Reliability of COPVs Accounting for Margin of Safety on Design Burst

In this paper, the stress rupture reliability of Carbon/Epoxy Composite Overwrapped Pressure Vessels (COPVs) is examined utilizing the classic Phoenix model and accounting for the differences between the design and the actual burst pressure, and the liner contribution effects. Stress rupture life primarily depends upon the fiber stress ratio which is defined as the ratio of stress in fibers at the maximum expected operating pressure to actual delivered fiber strength. The actual delivered fiber strength is calculated using the actual burst pressures of vessels established through burst tests. However, during the design phase the actual burst pressure is generally not known and to estimate the reliability of the vessels calculations are usually performed based upon the design burst pressure only. Since the design burst is lower than the actual burst, this process yields a much higher value for the stress ratio and consequently a conservative estimate for the reliability. Other complications arise due to the fact that the actual burst pressure and the liner contributions have inherent variability and therefore must be treated as random variables in order to compute the stress rupture reliability. Furthermore, the model parameters, which have to be established based on stress rupture tests of subscale vessels or coupons, have significant variability as well due to limited available data and hence must be properly accounted for. In this work an assessment of reliability of COPVs including both parameter uncertainties and physical variability inherent in liner and overwrap material behavior is made and estimates are provided in terms of degree of uncertainty in the actual burst pressure and the liner load sharing.

Murthy, Pappu L.N.↗

NASA NTRS1994

High-Hot-Strength Ceramic Fibers

Continuous fibers consisting of laminae of alumina and yttrium aluminum garnet offer exceptionally high strength, resistance to creep, and chemical stability at high temperatures. These fibers exceed tensile strength of sapphire fibers. Leading candidates for reinforcement of intermetallic-matrix composites in exhaust nozzles of developmental high-speed civil transport aircraft engines. Other applications are in aerospace, automotive, chemical-process, and power-generation industries.

Sayir, Ali↗

NASA NTRS1990

Factors which influence tensile strength of a SiC/Ti-24Al-11Nb (at. pct) composite

Tensile and fiber pullout tests were used in conjunction with SEM to investigate structural and processing effects on SiC fiber, a neat Ti-24Al-11Nb matrix alloy, and a composite fabricated from the two. The effects of oxygen content, fiber spacing, fiber volume fraction, fiber-matrix reaction thickness, Teflon content, and matrix powder size, appear to be smaller than the effects of variability in fiber strength. Fiber spacing did not influence radial crack formation, interfacial bond shear strength, or stress-strain behavior in the composite. The temperature dependence of composite properties was investigated over the 23-815 C range.

Brindley, P. K.↗

NASA NTRS1974

Compressive strength of fiber reinforced composite materials

Results of an experimental and analytical investigation of the compressive strength of unidirectional boron-epoxy composite material are presented. Observation of fiber coordinates in a boron-epoxy composite indicates that the fibers contain initial curvature. Combined axial compression and torsion tests were conducted on boron-epoxy tubes, and it was shown that the shear modulus is a function of axial compressive stress. An analytical model which includes initial curvature in the fibers and permits an estimate of the effect of curvature on compressive strength is proposed. Two modes of failure which may result from the application of axial compressive stress are analyzed, delamination and shear instability. Based on tests and analysis, failure of boron-epoxy under axial compressive load is due to shear instability.

Davis, J. G., Jr.↗

NASA NTRS2008

Processing and Structural Advantages of the Sylramic-iBN SiC Fiber for SiC/SiC Components

The successful high-temperature application of complex-shaped SiC/SiC components will depend on achieving as high a fraction of the as-produced fiber strength as possible during component fabrication and service. Key issues center on a variety of component architecture, processing, and service-related factors that can reduce fiber strength, such as fiber-fiber abrasion during architecture shaping, surface chemical attack during interphase deposition and service, and intrinsic flaw growth during high-temperature matrix formation and composite creep. The objective of this paper is to show that the NASA-developed Sylramic-iBN SiC fiber minimizes many of these issues for state-of-the-art melt-infiltrated (MI) SiC/BN/SiC composites. To accomplish this, data from various mechanical tests are presented that compare how different high performance SiC fiber types retain strength during formation of complex architectures, during processing of BN interphases and MI matrices, and during simulated composite service at high temperatures.

Yun, H. M.↗

NASA NTRS1999

Intermediate Temperature Stress Rupture of a Woven Hi-Nicalon, BN-Interphase, SiC Matric Composite in Air

Woven Hi-Nicalon (TM) reinforced melt-infiltrated SiC matrix composites were tested under tensile stress-rupture conditions in air at intermediate temperatures. A comprehensive examination of the damage state and the fiber properties at failure was performed. Modal acoustic emission analysis was used to monitor damage during the experiment. Extensive microscopy of the composite fracture surfaces and the individual fiber fracture surfaces was used to determine the mechanisms leading to ultimate failure. The rupture properties of these composites were significantly worse than expected compared to the fiber properties under similar conditions. This was due to the oxidation of the BN interphase. Oxidation occurred through the matrix cracks that intersected the surface or edge of a tensile bar. These oxidation reactions resulted in minor degradation to fiber strength and strong bonding of the fibers to one another at regions of near fiber-to-fiber contact. It was found that two regimes for rupture exist for this material: a high stress regime where rupture occurs at a fast rate and a low stress regime where rupture occurs at a slower rate. For the high stress regime, the matrix damage state consisted of through thickness cracks. The average fracture strength of fibers that were pulled-out (the final fibers to break before ultimate failure) was controlled by the slow-crack growth rupture criterion in the literature for individual Hi-Nicalon (TM) fibers. For the low stress regime, the matrix damage state consisted of microcracks which grew during the rupture test. The average fracture strength of fibers that were pulled-out in this regime was the same as the average fracture strength of individual fibers pulled out in as-produced composites tested at room temperature.

Morscher, Gregory N.↗

NASA NTRS1991

Mechanical behavior of high strength ceramic fibers at high temperatures

The mechanical behavior of commercially available and developmental ceramic fibers, both oxide and nonoxide, has been experimentally studied at expected use temperatures. In addition, these properties have been compared to results from the literature. Tensile strengths were measured for three SiC-based and three oxide ceramic fibers for temperatures from 25 C to 1400 C. The SiC-based fibers were stronger but less stiff than the oxide fibers at room temperature and retained more of both strength and stiffness to high temperatures. Extensive creep and creep-rupture experiments have been performed on those fibers from this group which had the best strengths above 1200 C in both single filament tests and tests of fiber bundles. The creep rates for the oxides are on the order of two orders of magnitude faster than the polymer derived nonoxide fibers. The most creep resistant filaments available are single crystal c-axis sapphire filaments. Large diameter CVD fabricated SiC fibers are the most creep and rupture resistant nonoxide polycrystalline fibers tested to date.

Tressler, R. E.↗

NASA NTRS2018

High Strength Ceramic Fibers and Methods of Fabrication

A method and apparatus for forming a plurality of fibers from (e.g., CVD) precursors, including a reactor adapted to grow a plurality of individual fibers; and a plurality of independently controllable lasers, each laser of the plurality of lasers growing a respective fiber. A high performance fiber (HPF) structure, including a plurality of fibers arranged in the structure; a matrix disposed between the fibers; wherein a multilayer coating is provided along the surfaces of at least some of the fibers with an inner layer region having a sheet-like strength; and an outer layer region, having a particle-like strength, such that any cracks propagating toward the outer layer from the matrix propagate along the outer layer and back into the matrix, thereby preventing the cracks from approaching the fibers. A method of forming an interphase in a ceramic matrix composite material having a plurality of SiC fibers, which maximizes toughness by minimizing fiber to fiber bridging, including arranging a plurality of SiC fibers into a preform; selectively removing (e.g., etching) silicon out of the surface of the fibers resulting in a porous carbon layer on the fibers; and replacing the porous carbon layer with an interphase layer (e.g., Boron Nitride), which coats the fibers to thereby minimize fiber to fiber bridging in the preform.

Pegna, Joseph↗

NASA NTRS1999

Comparison of the Tensile, Creep, and Rupture Strength Properties of Stoichiometric SiC Fibers

Tensile strength, creep strength, and rupture strength properties were measured for the following types of polymer-derived stoichiometric SiC fibers: Hi-Nicalon Type S from Nippon Carbon, Tyranno SA from Ube, and Sylramic from Dow Corning. Also included in this study were an earlier version of the SA fiber plus two recent developmental versions of the Sylramic fiber. The tensile strength measurements were made at room temperature on as-received fibers and on fibers after high-temperature inert exposure. The creep-rupture property data were obtained at 1400 deg C in air as well as, argon. Some fiber types showed strong effects of environment on their strength properties. These results are compared and discussed in terms of underlying mechanisms and implications for ceramic composites.

Yun, H. M.↗

NASA NTRS1998

Effects of HF Treatments on Tensile Strength of Hi-Nicalon Fibers

Tensile strengths of as-received Hi-Nicalon fibers and those having a dual BN/SiC surface coating, deposited by chemical vapor deposition, have been measured at room temperature. These fibers were also treated with HF for 24 h followed by tensile strength measurements. Strengths of uncoated and BN/SiC coated Hi-Nicalon fibers extracted from celsian matrix composites, by dissolving away the matrix in HF for 24 h, were also determined. The average tensile strength of uncoated Hi-Nicalon was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. The Hi-Nicalon/BN/SiC fibers showed an average strength of 3.04 q 0.53 GPa and Weibull modulus of 6.66. After HF treatments, the average strengths of the uncoated and BN/SiC coated Hi-Nicalon fibers were 2.69 +/- 0.67 GPa and 2.80 +/- 0.53 GPa and the Weibull moduli were 4.93 and 5.96, respectively. The BN/SiC coated fibers extracted from the celsian matrix composite exhibited a strength of 2.38 +/- 0.40 GPa and a Weibull modulus of 7.15. The strength of the uncoated Hi-Nicalon fibers in the composite was so severely degraded that they disintegrated into small fragments during extraction with HF. The uncoated fibers probably undergo mechanical surface damage during hot pressing of the composites. Also, the BN layer on the coated fibers acts as a compliant layer which protects the fibers from mechanical damage during composite processing. The elemental composition and thickness of the fiber coatings were deten-nined using scanning Auger analysis. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy and transmission electron microscopy. Strengths of fibers calculated using average and measured fiber diameters were in good agreement. Thus, the strength of fibers can be evaluated using an average fiber diameter instead of the measured diameter of each filament.

Bansal, Narottam P.↗

NASA NTRS1973

Application of diffusion barriers to the refractory fibers of tungsten, columbium, carbon and aluminum oxide

A radio frequency powered ion-plating system was used to plate protective layers of refractory oxides and carbide onto high strength fiber substrates. Subsequent overplating of these combinations with nickel and titanium was made to determine the effectiveness of such barrier layers in preventing diffusion of the overcoat metal into the fibers with consequent loss of fiber strength. Four substrates, five coatings, and two metal matrix materials were employed for a total of forty material combinations. The substrates were tungsten, niobium, NASA-Hough carbon, and Tyco sapphire. The diffusion-barrier coatings were aluminum oxide, yttrium oxide, titanium carbide, tungsten carbide with 14% cobalt addition, and zirconium carbide. The metal matrix materials were IN 600 nickel and Ti 6/4 titanium. Adhesion of the coatings to all substrates was good except for the NASA-Hough carbon, where flaking off of the oxide coatings in particular was observed.

Douglas, F. C.↗

NASA NTRS1979

Development and fabrication of high strength alloy fibers for use in metal-metal matrix composites

Metal fiber reinforced superalloys are being considered for construction of critical components in turbine engines that operate at high temperature. The problems involved in fabricating refractory metal alloys into wire form in such a manner as to maximize their strength properties without developing excessive structural defects are described. The fundamental principles underlying the development of such alloy fibers are also briefly discussed. The progress made to date in developing tungsten, tantalum and columbium base alloys for fiber reinforcement is reported and future prospects for alloy fiber development considered.

King, G. W.↗

NASA NTRS1980

Effects of temperature, thermal exposure, and fatigue on an alumina/aluminum composite

An experimental investigation of the mechanical properties and microstructure of an aluminum matrix/polycrystalline alumina fiber composite material is discussed. The effects of fabrication, isothermal exposure (up to 10,000 hours at 590 K), thermal cycling (6000 cycles between 200 K and 590 K), fatigue (1,000,000 tension-tension cycles) were determined by mechanical testing and metallurgical analysis. The fabrication process severely degraded the fiber strength by reducing the alumina to a nonstoichiometric form and quenching in the resultant vacancies and stress fields. However, isothermal exposure, thermal cycling, and fatigue cycling all restored the fiber strength by enhancing vacancy annihilation. Comparison of the as-fabricated material with other aerospace materials shows that it is an attractive candidate for select applications. Long duration isothermal exposure weakened the matrix by overaging and through the diffusional loss of lithium to a surface reaction forming lithium carbonate. Thermal cycling initiated cracks in the matrix and fibers. Tension-tension fatigue cycling caused no apparent damage to the as-fabricated material but in fact, strengthened it to the rule-of-mixtures value. Fatigue cycling after thermal exposure did have a cumulative damage effect.

Olsen, G. C.↗

NASA NTRS1978

Use of an ultrasonic-acoustic technique for nondestructive evaluation of fiber composite strength

Details of the method used to measure the stress wave factor are described. Frequency spectra of the stress waves are analyzed in order to clarify the nature of the wave phenomena involved. The stress wave factor was measured with simple contact probes requiring only one-side access to a part. This is beneficial in nondestructive evaluations because the waves can run parallel to fiber directions and thus measure material properties in directions assumed by actual loads. The technique can be applied where conventional through transmission techniques are impractical or where more quantitative data are required. The stress wave factor was measured for a series of graphite/polyimide composite panels, and results obtained are compared with through transmission immersion ultrasonic scans.

Vary, A.↗