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Gray, Hugh R.

Publications and source records attributed to Gray, Hugh R..

At least 37 records · Page 2

Morphological Evolution and Weak Interface Development within CVD-Zirconia Coating Deposited on Hi-Nicalon Fiber

The phase contents and morphology of a ZrO2 fiber coating deposited at 1050 C on Hi-Nicalon(Tm) by chemical vapor deposition were examined as a function of deposition time from 5 to 120 min. The morphological evolution in the ZrO2 coating was correlated to the development of delamination within the ZrO2 coating. The delamination appears to occur as a result of: (1) continuous formation of tetragonal ZrO2 nuclei on the deposition surface; (2) martensitic transformation of the tetragonal phase to a monoclinic phase upon reaching a critical grain size; and (3) development of significant compressive hoop stresses due to the volume dilation associated with the transformation. Our observations suggest that it will be of critical importance to further understand and eventually control the nucleation and grain growth behavior of CVD ZrO2 and its phase transformation behavior for its potential applications for composites.

Li, Hao↗

The Role of Ceramics and Ceramic Matrix Composites in NASA's Advanced Space Propulsion Programs

In recent years, NASA has embarked on several new and exciting efforts in the exploration and use of space. The successful accomplishment of many planned missions and projects is dependent upon the development and deployment of previously unproven propulsion systems. Key to many of the propulsion systems is the use of structural ceramics and ceramic matrix composites. In spite of their promise, a number of programmatic and technical hurdles remain before the potential of ceramic materials can be realized. A programmatic environment which focuses on relatively short term hardware demonstration programs precludes traditional longer term material's development efforts. The challenge oftentimes becomes one of engineering ceramics into proposed missions. This is dependent upon a fundamental understanding of processing, degradation and design issues unique to space vehicle design and operations. A review of the general missions and benefits of utilizing ceramics and ceramic matrix composites will be presented. The design parameters and operating conditions will be presented for both specific missions/vehicles and classes of components. Key technical challenges and opportunities are identified along with suggested paths for addressing them.

Eckel, Andrew J.↗

High Temperature Si-doped BN Interphases for Woven SiC/SiC Composites

The hydrolytic stability of high-temperature deposited Si-doped BN has been shown in the past to be superior in comparison to "pure" BN processed at similar or even higher temperatures. This type of material would be very desirable as a SiC/SiC composite interphase that is formed by chemical infiltration into multi-ply woven preform. However, due to rapid deposition on the preform outer surface at the high processing temperature, this has proven very difficult. To overcome this issue, single plies of woven fabric were infiltrated with Si-doped BN. Three composite panels of different SiC fiber types were fabricated with Si-doped BN interphases including Sylramic, Hi-Nicalon Type S and Sylramic-iBN fiber-types. The latter fiber-type possesses a thin in-situ grown BN layer on the fiber surface. High Si contents (approx. 7 to 10 a/o) and low oxygen contents (less than 1 a/o) were achieved. All three composite systems demonstrated reasonable debonding and sliding properties. The coated Sylramic fabric and composites were weak due to fiber degradation apparently caused during interphase processing by the formation of TiN crystals on the fiber surface. The Hi-Nicalon Type S composites with Si-doped BN interphase were only slightly weaker than Hi-Nicalon Type S composites with conventional BN when the strength on the load-bearing fibers at failure was compared. On the other hand, the Sylramic-iBN fabric and composites with Si-doped BN showed excellent composite and intermediate temperature stress-rupture properties. Most impressive was the lack of any significant interphase oxidation on the fracture surface of stress-ruptured specimens tested well above matrix cracking at 815C.

Morscher, Gregory N.↗

Mechanical Properties and Microstructure of Biomorphic Silicon Carbide Ceramics Fabricated from Wood Precursors

Silicon carbide based, environment friendly, biomorphic ceramics have been fabricated by the pyrolysis and infiltration of natural wood (maple and mahogany) precursors. This technology provides an eco-friendly route to advanced ceramic materials. These biomorphic silicon carbide ceramics have tailorable properties and behave like silicon carbide based materials manufactured by conventional approaches. The elastic moduli and fracture toughness of biomorphic ceramics strongly depend on the properties of starting wood preforms and the degree of molten silicon infiltration. Mechanical properties of silicon carbide ceramics fabricated from maple wood precursors indicate the flexural strengths of 3441+/-58 MPa at room temperature and 230136 MPa at 1350C. Room temperature fracture toughness of the maple based material is 2.6 +/- 0.2 MPa(square root of)m while the mahogany precursor derived ceramics show a fracture toughness of 2.0 +/- 0.2 Mpa(square root of)m. The fracture toughness and the strength increase as the density of final material increases. Fractographic characterization indicates the failure origins to be pores and chipped pockets of silicon.

Singh, Mrityunjay↗

Environment Conscious, Biomorphic Ceramics from Pine and Jelutong Wood Precursors

Environment conscious, biomorphic ceramics have been fabricated from pine and jelutong wood precursors. A carbonaceous preform is produced through wood pyrolysis and subsequent infiltration with oxides (ZrO2 sols) and liquid silicon to form ceramics. These biomorphic ceramics show a wide variety of microstructures, densities, and hardness behavior that are determined by the type of wood and infiltrants selected.

Singh, Mrityunjay↗

Oxidation and Volatilization of Silica-Formers in Water Vapor

At high temperatures SiC and Si3N4 react with water vapor to form a silica scale. Silica scales also react with water vapor to form a volatile Si(OH)4 species. These simultaneous reactions, one forming silica and the other removing silica, are described by paralinear kinetics. A steady state, in which these reactions occur at the same rate, is eventually achieved, After steady state is achieved, the oxide found on the surface is a constant thickness and recession of the underlying material occurs at a linear rate. The steady state oxide thickness, the time to achieve steady state, and the steady state recession rate can all be described in terms of the rate constants for the oxidation and volatilization reactions. In addition, the oxide thickness, the time to achieve steady state, and the recession rate can also be determined from parameters that describe a water vapor-containing environment. Accordingly, maps have been developed to show these steady state conditions as a function of reaction rate constants, pressure, and gas velocity. These maps can be used to predict the behavior of silica formers in water-vapor containing environments such as combustion environments. Finally, these maps are used to explore the limits of the paralinear oxidation model for SiC and Si3N4

Opila, E. J.↗

High Temperature Corrosion of Silicon Carbide and Silicon Nitride in Water Vapor

Silicon carbide (SiC) and silicon nitride (Si3N4) are proposed for applications in high temperature combustion environments containing water vapor. Both SiC and Si3N4 react with water vapor to form a silica (SiO2) scale. It is therefore important to understand the durability of SiC, Si3N4 and SiO2 in water vapor. Thermogravimetric analyses, furnace exposures and burner rig results were obtained for these materials in water vapor at temperatures between 1100 and 1450 C and water vapor partial pressures ranging from 0.1 to 3.1 atm. First, the oxidation of SiC and Si3N4 in water vapor is considered. The parabolic kinetic rate law, rate dependence on water vapor partial pressure, and oxidation mechanism are discussed. Second, the volatilization of silica to form Si(OH)4(g) is examined. Mass spectrometric results, the linear kinetic rate law and a volatilization model based on diffusion through a gas boundary layer are discussed. Finally, the combined oxidation and volatilization reactions, which occur when SiC or Si3N4 are exposed in a water vapor-containing environment, are presented. Both experimental evidence and a model for the paralinear kinetic rate law are shown for these simultaneous oxidation and volatilization reactions.

Opila, E. J.↗

HOTPC PMC Project Overview

A review of NASA GRCs Higher Operating Temperature Propulsion Components Project (HOTPC) on polymer matrix composites (PMCs) will be described. The summary includes research from NASA GRC in-house, university and industry's cooperative programs. Current research emphasis focuses on developing high temperature PMCs used in rapidly heated structures, erosion coatings for PMCs, nano-materials compatible with polyimide resins, and development of more durable high temperature PMCs.

Sutter, Jim↗

High-Temperature Mechanical Properties of Cr(3+) Doped Sapphire Fibers

High-temperature slow-crack growth of single crystal 10 wt% Cr2O3 - Al2O3 (nominal composition) fibers has been studied by tensile rupture experiments at 1400 C, under different stressing rates (0.5 to 41.5 MPa/s). Slow-crack growth (SCG) is less pronounced with increasing Cr2O3. Rupture stresses increased with the stressing rate from 397 MPa to 515 MPa, resulting in a SCG exponent, N=19. The Cr2O3 composition was analyzed by Energy Dispersed X-Ray Spectra (EDS) and fracture surfaces were studied by scanning electron microscopy (SEM). Results are compared with previous studies on 100-300 ppm Cr3(+) doped sapphire fibers and on commercial sapphire fibers.

Sayir, A.↗

Bn and Si-Doped Bn Coatings on Woven Fabrics

A computer controlled, pulsed chemical vapor infiltration (CVI) system has been developed to deposit BN from a liquid borazine (B3N3H6) source, as well as silicon doped BN coatings using borazine and a silicon source, into 2-D woven ceramic fabric preforms. The coating process was evaluated as a function of deposition temperature, pressure, and precursor flow rate. Coatings were characterized by field emission scanning electron microscopy, electron dispersive spectroscopy and Auger spectroscopy. By controlling the reactant feed ratios, Si incorporation could be controlled over the range of 6-24 atomic percent.

Hurwitz, Frances I.↗

Properties of M40J Carbon/PMR-II-50 Composites Fabricated with Desized and Surface Treated Fibers. Characterization of M40J Desized and Finished Fibers

To increase performance and durability of high temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high temperature polyimide resins. It has been previously demonstrated that the electro-oxidative shear treatments used by fiber manufacturers are not effective on higher modulus fibers that have fewer edge and defect sites in the surface crystallites. In addition, sizings commercially supplied on most carbon fibers are not compatible with polyimides. This study was an extension of prior work characterizing the surface chemistry and energy of high modulus carbon fibers (M40J and M60J, Torray) with typical fluorinated polyimide resins, such as PMR-II-50. A continuous desizing system which utilizes environmentally friendly chemical- mechanical processes was developed for tow level fiber and the processes were optimized based on weight loss behavior, surface elemental composition (XPS) and morphology (FE-SEM) analyses, and residual tow strength of the fiber, and the similar approaches have been applied on carbon fabrics. Both desized and further treated with a reactive finish were investigated for the composite reinforcement. The effects of desizing and/or subsequent surface retreatment on carbon fiber on composite properties and performance including fiber-matrix interfacial mechanical properties, thermal properties and blistering onset behavior will be discussed in this presentation.

Allred, Ronald E.↗

Evaluation of Graphite Fiber/Polyimide PMCs from Hot Melt versus Solution Prepreg

Carbon fiber reinforced high temperature polymer matrix composites (PMC) have been extensively investigated as potential weight reduction replacements of various metallic components in next generation high performance propulsion rocket engines. The initial phase involves development of comprehensive composite material-process-structure-design-property in-service performance correlations and database, especially for a high stiffness facesheet of various sandwich structures. Overview of the program plan, technical approaches and current multi-team efforts will be presented. During composite fabrication, it was found that the two large volume commercial prepregging methods (hot-melt vs. solution) resulted in considerably different composite cure behavior. Details of the process-induced physical and chemical modifications in the prepregs, their effects on composite processing, and systematic cure cycle optimization studies will be discussed. The combined effects of prepregging method and cure cycle modification on composite properties and isothermal aging performance were also evaluated.

Shin, Eugene E.↗

The Influence of Interfacial Roughness on Fiber Sliding in Oxide Composites with La-Monazite Interphases

Room temperature debonding and sliding of La-Monazite coated fibers is assessed using a composite with a polycrystalline alumina matrix and fibers of several different single crystal (mullite, sapphire) and directionally solidified eutectic (Al2O3/Y3Al5O12 and Al2O3/Y-ZrO2) compositions. These fibers provide a range of residual stresses and interfacial roughnesses. Sliding occurred over a debond crack at the fiber-coating interface when the sliding displacement and surface roughness were relatively small. At large sliding displacements with relatively rough interfaces, the monazite coatings were deformed extensively by fracture, dislocations and occasional twinning, whereas the fibers were undamaged. Dense, fine-grained (10 nm) microstructures suggestive of dynamic recrystallization were also observed in the coatings. Frictional heating during sliding is assessed. The possibility of low temperature recrystallization is discussed in the light of the known resistance of monazite to radiation damage. The ability of La-Monazite to undergo plastic deformation relatively easily at low temperatures may be enabling for its use as a composite interface.

Davis, J. B.↗

Characterization of C/SiC Ceramic Matrix Composites (CMCs) with Novel Interface Fiber Coatings

Ceramic Matrix Composites (CMCs) are attractive candidate materials in the aerospace industry due to their high specific strength, low density and higher temperature capabilities. The National Aeronautics and Space Administration (NASA) is pursuing the use of CMC components in advanced Reusable Launch Vehicle (RLV) propulsion applications. Carbon fiber-reinforced silicon carbide (C/SiQ is the primary material of interest for a variety of RLV propulsion applications. These composites offer high-strength carbon fibers and a high modulus, oxidation-resistant matrix. For comparison, two types of carbon fibers were processed with novel types of interface coatings (multilayer and pseudoporous). For RLV propulsion applications, environmental durability will be critical. The coatings show promise of protecting the carbon fibers from the oxidizing environment. The strengths and microstructures of these composite materials are presented.

Petko, Jeanne F.↗

Paralinear Oxidation of Silicon Nitride in a Water Vapor/Oxygen Environment

Three silicon nitride materials were exposed to dry oxygen flowing at 0.44 cm/s at temperatures between 1200 and 1400 C. Reaction kinetics were measured with a continuously recording microbalance. Parabolic kinetics were observed. When the same materials were exposed to a 50% H2O - 50% O2 gas mixture flowing at 4.4 cm/s, all three types exhibited paralinear kinetics. The material is oxidized by water vapor to form solid silica. The protective silica is in turn volatilized by water vapor to form primarily gaseous Si(OH)4. Nonlinear least squares analysis and a paralinear kinetic model were used to determine both parabolic and linear rate constants from the kinetic data. Volatilization of the protective silica scale can result in accelerated consumption of Si3N4. Recession rates under conditions more representative of actual combustors are compared to the furnace data.

Fox, Dennis S.↗

Mullite+CAS Bond Coat for Environmental Barrier Coatings for Si-Based Ceramics

Current environmental barrier coatings (EBCs) for silicon-based ceramics consist of a bond coat and a top coat. Mullite bond coat modified by adding low CTE glass ceramics, such as BSAS (xBaO.1xSrO.Al2O3.2SiO2) or CAS (CaO.Al2O3.2SiO2), was developed in the NASA Enabling Propulsion Materials (EPM) Program. EBCs based on mullite+CAS bond coat were characterized using high steam thermal cycling test and high steam isothermal thermogravemitry (TGA) at 1225 C - 13,000 C. The Mullite+CAS bond coat showed far superior durability compared to mullite bond coat, due to enhanced crack resistance. A BSAS top coat provided further improved durability compared to EBCs with a yttria-stabilized zirconia (YSZ) top coat. Still further improvement in the durability was achieved by adding a silicon bond coat between the mullite and the substrate. However, the silicon/mullite+CAS/BSAS EBC showed inferior long-term durability compared to the current state-of-the art EBC (silicon/mullite+BSAS/BSAS EBC), presumably due to the higher CAS-silica chemical reactivity.

Lee, Kang N.↗

Oxidation Behavior of Copper Alloy Candidates for Rocket Engine Applications (Technical Poster)

A rocket engine's combustion chamber is lined with material that is highly conductive to heat in order to dissipate the huge thermal load (evident in a white-hot exhaust plume). Because of its thermal conductivity copper is the best choice of liner material. However, the mechanical properties of pure copper are inadequate to withstand the high stresses, hence, copper alloys are needed in this application. But copper and its alloys are prone to oxidation and related damage, especially "blanching" (an oxidation-reduction mode of degradation). The space shuttle main engine combustion chamber is lined with a Cu-Ag-Zr alloy, "NARloy-Z", which exhibits blanching. A superior liner is being sought for the next generation of RLVs (Reusable Launch Vehicles) It should have improved mechanical properties and higher resistance to oxidation and blanching, but without substantial penalty in thermal conductivity. GRCop84, a Cu-8Cr-4Nb alloy (Cr2Nb in Cu matrix), developed by NASA Glenn Research Center (GRC) and Case Western Reserve University, is a prime contender for RLV liner material. In this study, the oxidation resistance of GRCop-84 and other related/candidate copper alloys are investigated and compared

Ogbuji, Linus U. J.↗

Characterization of Ceramic Matrix Composite Fasteners Exposed in a Combustion Liner Rig Test

Combustion tests on SiC/SiC CMC (Ceramic Matrix Composite) components were performed in an aircraft combustion environment using the Rich-burn, Quick-quench, Lean-burn (RQL) sector rig. SiC/SiC fasteners were used to attach several of these components to the metallic rig structure. The effect of combustion exposure on the fastener material was characterized via microstructural examination. Fasteners were also destructively tested, after combustion exposure, and the failure loads of fasteners exposed in the sector rig were compared to those of as-manufactured fasteners. Combustion exposure reduced the fastener failure load by 50% relative to the as-manufactured fasteners for exposure times ranging from 50 to 260 hours. The fasteners exposed in the combustion environment demonstrated failure loads that varied with failure mode. Fasteners that had the highest average failure load, failed in the same manner as the unexposed fasteners.

Verrilli, Michael J.↗