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All sourcesNASA NTRSDOE OSTI
NASA NTRS2004

Processing Techniques Developed to Fabricate Lanthanum Titanate Piezoceramic Material for High-Temperature Smart Structures

Piezoelectric ceramic materials are potential candidates for use as actuators and sensors in intelligent gas turbine engines. For piezoceramics to be applied in gas turbine engines, they will have to be able to function in temperatures ranging from 1000 to 2500 F. However, the maximum use temperature for state-of-the-art piezoceramic materials is on the order of 300 to 400 F. Research activities have been initiated to develop high-temperature piezoceramic materials for gas turbine engine applications. Lanthanum titanate has been shown to have high-temperature piezoelectric properties with Curie temperatures of T(sub c) = 1500 C and use temperatures greater than 1000 C. However, the fabrication of lanthanum titanate poses serious challenges because of the very high sintering temperatures required for densification. Two different techniques have been developed at the NASA Glenn Research Center to fabricate dense lanthanum titanate piezoceramic material. In one approach, lower sintering temperatures were achieved by adding yttrium oxide to commercially available lanthanum titanate powder. Addition of only 0.1 mol% yttrium oxide lowered the sintering temperature by as much as 300 C, to just 1100 C, and dense lanthanum titanate was produced by pressure-assisted sintering. The second approach utilized the same commercially available powders but used an innovative sintering approach called differential sintering, which did not require any additive.

Goldsby, Jon C.↗
NASA NTRS2016

Fabrication of High Thermal Conductivity NARloy-Z-Diamond Composite Combustion Chamber Liner for Advanced Rocket Engines

NARloy-Z alloy (Cu-3 percent, Ag-0.5 percent, Zr) is a state of the art alloy currently used for fabricating rocket engine combustion chamber liners. Research conducted at NASA-MSFC and Penn State – Applied Research Laboratory has shown that thermal conductivity of NARloy-Z can be increased significantly by adding diamonds to form a composite (NARloy-Z-D). NARloy-Z-D is also lighter than NARloy-Z. These attributes make this advanced composite material an ideal candidate for fabricating combustion chamber liner for an advanced rocket engine. Increased thermal conductivity will directly translate into increased turbopump power and increased chamber pressure for improved thrust and specific impulse. This paper describes the process development for fabricating a subscale high thermal conductivity NARloy-Z-D combustion chamber liner using Field Assisted Sintering Technology (FAST). The FAST process uses a mixture of NARloy-Z and diamond powders which is sintered under pressure at elevated temperatures. Several challenges were encountered, i.e., segregation of diamonds, machining the super hard NARloy-Z-D composite, net shape fabrication and nondestructive examination. The paper describes how these challenges were addressed. Diamonds coated with copper (CuD) appear to give the best results. A near net shape subscale combustion chamber liner is being fabricated by diffusion bonding cylindrical rings of NARloy-Z-CuD using the FAST process.

Bhat, Biliyar N.↗
NASA NTRS1973

Grain boundary mobility in anion doped MgO

Certain anions OH(-), F(-) and Gl(-) are shown to enhance grain growth in MgO. The magnitude of their effect decreases in the order in which the anions are listed and depends on their location (solid-solution, second phase) in the MgO lattice. As most anions exhibit relatively high vapor pressures at sintering temperatures, they retard densification and invariably promote residual porosity. The role of anions on grain growth rates was studied in relation to their effect on pore mobility and pore removal; the atomic process controlling the actual rates was determined from observed kinetics in conjunction with the microstructural features. With respect to controlling mechanisms, the effects of all anions are not the same. OH(-) and F(-) control behavior through creation of a defect structure and a grain boundary liquid phase while Cl(-) promotes matter transport within pores by evaporation-condensation. Studies on an additional anion, S to the minus 2nd power gave results which were no different from undoped MgO, possibly because of evaporative losses during hot pressing. Hence, the effect of sulphur is negligible or undetermined.

Kapadia, C. M.↗
NASA NTRS1991

Thermochemical analysis of chemical processes relevant to the stability and processing of SiC-reinforced Si3N4 composite

Chemical processes relevant to the stability and processing of SiC-reinforced Si3N4 composites have been examined from thermochemical considerations. The thermodynamic stabilities of various interfaces, such as SiC-Si3N4, SiC-Si3N4-Si2ON2, and SiC-Si3N4-SiO2, have been examined as a function of temperature, and the temperatures above which these interfaces become unstable have been calculated. The degradation of SiC during the processing of the composite has been examined. The processing routes considered in this study include the reaction bonded silicon nitride (RBSN) process and the pressure-assisted sintering processes with suitable sintering additives.

Misra, Ajay K.↗
NASA NTRS1993

Radial basis function network learns ceramic processing and predicts related strength and density

Radial basis function (RBF) neural networks were trained using the data from 273 Si3N4 modulus of rupture (MOR) bars which were tested at room temperature and 135 MOR bars which were tested at 1370 C. Milling time, sintering time, and sintering gas pressure were the processing parameters used as the input features. Flexural strength and density were the outputs by which the RBF networks were assessed. The 'nodes-at-data-points' method was used to set the hidden layer centers and output layer training used the gradient descent method. The RBF network predicted strength with an average error of less than 12 percent and density with an average error of less than 2 percent. Further, the RBF network demonstrated a potential for optimizing and accelerating the development and processing of ceramic materials.

Cios, Krzysztof J.↗
NASA NTRS1993

Fuzzy sets predict flexural strength and density of silicon nitride ceramics

In this work, we utilize fuzzy sets theory to evaluate and make predictions of flexural strength and density of NASA 6Y silicon nitride ceramic. Processing variables of milling time, sintering time, and sintering nitrogen pressure are used as an input to the fuzzy system. Flexural strength and density are the output parameters of the system. Data from 273 Si3N4 modulus of rupture bars tested at room temperature and 135 bars tested at 1370 C are used in this study. Generalized mean operator and Hamming distance are utilized to build the fuzzy predictive model. The maximum test error for density does not exceed 3.3 percent, and for flexural strength 7.1 percent, as compared with the errors of 1.72 percent and 11.34 percent obtained by using neural networks, respectively. These results demonstrate that fuzzy sets theory can be incorporated into the process of designing materials, such as ceramics, especially for assessing more complex relationships between the processing variables and parameters, like strength, which are governed by randomness of manufacturing processes.

Cios, Krzysztof J.↗
NASA NTRS2003

Silicon Carbide Fiber-Reinforced Silicon Nitride Composites

The fabrication and thermo-mechanical properties of SiC monofilament- and SiC fiber tow-reinforced reaction-bonded silicon nitride matrix composites (SiC/RBSN) and fully dense SiC monofilament-reinforced silicon nitride matrix composites (SiC/Si3N4) have been reviewed. The SiC/RBSN composites display high strength and toughness, and low thermal conductivity in the as-fabricated condition, but are susceptible to internal oxidation and mechanical property degradation in the intermediate temperature range from 400 to 1100 C. The internal oxidation problem can be avoided by applying functionally graded oxidation resistant coatings on external surfaces of the composite. On the other hand, the fully dense SiC/SiC3N4 composites fabricated by using SiC monofilaments and pressure assisted sintering methods display moderate strength and limited strain capability beyond matrix cracking stress. Advantages, disadvantages, and potential applications of SiC fiber-reinforced silicon nitride matrix composites fabricated using various fiber types and processing methods are discussed.

Bhatt, Ramakrishna T.↗
NASA NTRS1982

Study of phenomena related to the sintering process of silicon nitride at atmospheric pressure

A procedure was perfected for the production of components used in engineering applications of silicon nitride. Particles of complex geometry that combine remarkable mechanical properties with a high density are obtained. The process developed, in contrast to the "hot pressing" method, does not use external pressures, and in contrast to the reaction bonding method, final densities close to the theoretical value are obtained.

Bertani, A.↗
NASA NTRS2015

Methodology for Producing a Uniform Distribution of UO2 in a Tungsten Matrix

Current work at NASA's Marshall Space Flight Center (MSFC) is focused on the development CERMET fuel materials for Nuclear Thermal Propulsion (NTP). The CERMETs consist of uranium dioxide (UO2) fuel particles embedded in a tungsten (W) metal matrix. Initial testing of W-UO2 samples fabricated from fine angular powders performed reasonably well, but suffered from significant fuel loss during repeated thermal cycling due to agglomeration of the UO2 (1). The blended powder mixtures resulted in a non-uniform dispersion of the UO2 particles in the tungsten matrix, which allows rapid vaporization of the interconnected UO2 from the sample edges into the bulk material. Also, the angular powders create areas of stress concentrations due to thermal expansion mismatch, which eventually cracks the tungsten matrix. Evenly coating spherical UO2 particles with chemical vapor deposited (CVD) tungsten prior to consolidation was previously demonstrated to provide improved performance. However, the CVD processing technology is expensive and not currently available. In order to reduce cost and enhance performance, a powder coating process has been developed at MSFC to produce a uniform distribution of the spherical UO2 particles in a tungsten matrix. The method involves utilization of a polyethylene binder during mixing which leads to fine tungsten powders clinging to the larger UO2 spherical particles. This process was developed using HfO2 as a surrogate for UO2. Enough powder was mixed to make 8 discs (2cm diameter x 8mm thickness) using spark plasma sintering. A uniaxial pressure of 50 MPa was used at four different temperatures (2 samples at each temperature). The first two samples were heated to 1400C and 1500C respectively for 5 minutes. Densities for these samples were less than 85% of theoretical, so the time at temperature was increased to 20 minutes for the remaining samples. The highest densities were achieved for the two samples sintered at 1700C (approx. 92% of theoretical). Scanning electron microscopy (SEM) of the mixed powders and the sintered samples along with energy dispersive x-ray analysis was obtained. The SEM of the powders clearly show the fine W powder adhered to the larger HfO2 particles and a uniform distribution of HfO2 particles in a tungsten matrix upon densification. Vicker's Microhardness testing was also performed on all samples using 0.5, 1.0 and 2.0 kg loads. Five indents were made at each load level. All indents were placed in the tungsten matrix to assist as a proxy in measuring densification. The highest hardness value was obtained for the 1700C specimens. The hardness average for these samples was 312.14 MPa. This powder processing method has been applied to W/UO2 powders with the SEM of the powders appearing similar to the W/HfO2 powder images.

Tucker, Dennis S.↗
NASA NTRS1993

Cold press sintering of simulated lunar basalt

In order to predict the conditions for which the lunar regolith may be adequately sintered, experiments were conducted in which samples of simulated lunar basalt (MLS-1) were pressed at high pressures and then heated in an electric furnace. This sintering process may be referred to as cold press sintering since the material is pressed at room temperature. Although test articles were produced which possessed compressive strengths comparable to that of terrestrial concrete, the cold press sintering process requires very high press pressures and sintering temperatures in order to achieve that strength. Additionally, the prospect of poor internal heat transfer adversely affecting the quality of sintered lunar material is a major concern. Therefore, it is concluded that cold press sintering will most likely be undesirable for the production of lunar construction materials.

Altemir, D. A.↗
NASA NTRS1974

Preliminary results of experiments to duplicate Boulder textures by thermal sintering of powders

Experiments seem to indicate that at the low pressures characteristic of an ejecta blanket, sintering or sintering/devitrification could have lithified boulder 1 matrix materials and produced the textural types observed in 72255 and 72275. This very preliminary conclusion is consistent with other observations that granitic clasts have undergone a slight degree of partial melting (and have therefore experienced temperatures on the order of 1000 C). It is concluded that maskelynite in the boulder is completely devitrified.

Hallam, M. E.↗
NASA NTRS1988

Preparation and evaluation of silicon nitride matrices for silicon nitride-SiC fiber composites

Continuous silicon carbide (SiC) fiber was added to three types of silicon nitride (Si3N4) matrices. Efforts were aimed at producing a dense Si3N4 matrix from reaction-bonded silicon nitride (RBSN) by hot-isostatic-pressing (HIP) and pressureless sintering, and from Si3N4 powder by hot-pressing. The sintering additives utilized were chosen to allow for densification, while not causing severe degradation of the fiber. The ceramic microstructures were evaluated using scanning optical microscopy. Vickers indentation was used to determine the microhardness and fracture toughness values of the matrices. The RBSN matrices in this study did not reach more than 80 percent of theoretical density after sintering at various temperatures, pressures, and additive levels. Hot-pressing Si3N4 powder produced the highest density matrices; hardness and toughness values were within an order of magnitude of the best literature values. The best sintering aid composition chosen included Y2O3, SiO2, and Al2O3 or AlN. Photomicrographs demonstrate a significant reduction of fiber attack by this additive composition.

Axelson, Scott R.↗
NASA NTRS1999

The Oxidation Rate of SiC in High Pressure Water Vapor Environments

CVD SiC and sintered alpha-SiC samples were exposed at 1316 C in a high pressure burner rig at total pressures of 5.7, 15, and 25 atm for times up to 100h. Variations in sample emittance for the first nine hours of exposure were used to determine the thickness of the silica scale as a function of time. After accounting for volatility of silica in water vapor, the parabolic rate constants for Sic in water vapor pressures of 0.7, 1.8 and 3.1 atm were determined. The dependence of the parabolic rate constant on the water vapor pressure yielded a power law exponent of one. Silica growth on Sic is therefore limited by transport of molecular water vapor through the silica scale.

Opila, Elizabeth J.↗
NASA NTRS1990

In-situ resource utilization in the design of advanced lunar facilities

Resource utilization will play an important role in the establishment and support of a permanently manned lunar base. At the University of Houston - College of Architecture and the Sasakawa International Center for Space Architecture, a study team recently investigated the potential use of lunar in-situ materials in the design of lunar facilities. The team identified seven potential lunar construction materials; concrete, sulfur concrete, cast basalt, sintered basalt, glass, fiberglass, and metals. Analysis and evaluation of these materials with respect to their physical properties, processes, energy requirements, resource efficiency, and overall advantages and disadvantages lead to the selection of basalt materials as the more likely construction material for initial use on a lunar base. Basalt materials can be formed out of in-situ lunar regolith, with minor material beneficiation, by a simple process of heating and controlled cooling. The team then conceptualized a construction system that combines lunar regolith sintering and casting to make pressurized structures out of lunar resources. The design uses a machine that simultaneously excavates and sinters the lunar regolith to create a cylindrical hole, which is then enclosed with cast basalt slabs, allowing the volume to be pressurized for use as a living or work environment. Cylinder depths of up to 4 to 6 m in the lunar mare or 10 to 12 m in the lunar highlands are possible. Advantages of this construction system include maximum resource utilization, relatively large habitable volumes, interior flexibility, and minimal construction equipment needs. Conclusions of this study indicate that there is significant potential for the use of basalt, a lunar resource derived construction material, as a low cost alternative to Earth-based materials. It remains to be determined when in lunar base phasing this construction method should be implemented.

Source record↗
NASA NTRS2000

Corrosion Issues for Ceramics in Gas Turbines

The requirements for hot-gas-path materials in gas turbine engines are demanding. These materials must maintain high strength and creep resistance in a particularly aggressive environment. A typical gas turbine environment involves high temperatures, rapid gas flow rates, high pressures, and a complex mixture of aggressive gases. Figure 26.1 illustrates the requirements for components of an aircraft engine and critical issues [1]. Currently, heat engines are constructed of metal alloys, which meet these requirements within strict temperature limits. In order to extend these temperature limits, ceramic materials have been considered as potential engine materials, due to their high melting points and stability at high temperatures. These materials include oxides, carbides, borides, and nitrides. Interest in using these materials in engines appears to have begun in the 1940s with BeO-based porcelains [2]. During the 1950s, the efforts shifted to cermets. These were carbide-based materials intended to exploit the best properties of metals and ceramics. During the 1960s and 1970s, the silicon-based ceramics silicon carbide (SiC) and silicon nitride (Si3N4) were extensively developed. Although the desirable high-temperature properties of SiC and Si3N4 had long been known, consolidation of powders into component-sized bodies required the development of a series of specialized processing routes [3]. For SiC, the major consolidation routes are reaction bonding, hot-pressing, and sintering. The use of boron and carbon as additives which enable sintering was a particularly noteworthy advance [4]. For Si3N4 the major consolidation routes are reaction bonding and hot pressing [5]. Reaction-bonding involves nitridation of silicon powder. Hot pressing involves addition of various refractory oxides, such as magnesia (MgO), alumina (Al2O3), and yttria (y2O3). Variations on these processes include a number of routes including Hot Isostatic Pressing (HIP), gas-pressure sintering, sinter-HIPing, and Encapsulation-HIPing. It is important to note that each process involves the addition of secondary elements, which later were shown to dramatically influence oxidation and corrosion behavior. As dense bodies of silicon-based ceramics became more readily available, their desirable high temperature properties were confirmed. These materials retained strength to very high temperatures (i.e. 1300-1400 C). Further, they were lightweight and made from abundant materials. SiC and Si3N4 therefore emerged as leading ceramic candidates for components in heat engines, designed to operate at higher temperatures for better performance and fuel efficiency. The first US programs for ceramics in heat engines have been reviewed [6]. Selected programs on ceramic engine parts are summarized here in regard to their contributions to understanding the corrosion behavior of a heat engine environment.

Jacobson, Nathan S.↗
NASA NTRS1985

Capsulation of moldings made from silicon ceramic material

Ceramic articles are potted for hot isostatic pressing by porous glass and/or ceramic coating which is sintered to a pressure-tight coating in vacuo. Thus, a powdered SiO2 glass mixture with saturated alcohol sterin is sprayed on a SI3N4 ceramic, dried, introduced into the press which is evacuated to less than 0.013 mbar and heated to approximately 1200 C to drive off the organic binder and leave a powdered glass coating on the ceramic. The coating is sintered by heating to approximately 1200 C for 0.5 to 2 hours and forms a tight gass-impermeable layer. The press is heated to approximately 1700 C at 1000-300 bar and isostatic pressing is performed in the conventional manner.

Rossmann, A.↗
NASA NTRS1975

Sintering, crystallization, and breccia formation

The process of breccia formation by viscous sintering in the absence of pressure, advanced by Simonds (1973), is examined in detail. The limitations on the standard model for such sintering are considered. The competing process of crystallization is analyzed kinetically in terms of time-temperature-transformation curves corresponding to various degrees of crystallinity. The analysis is applied to Lunar Composition 15418 to illustrate the approach. The results indicate that close constraints can be placed on the thermal histories of lunar breccias, particularly breccias with modest degrees of crystallinity, from microstructural observations and kinetic measurements.

Uhlmann, D. R.↗
NASA NTRS1972

Electron petrography of Apollo 14 and 15 rocks.

Comparative optical and high-voltage electron petrographic analyses of igneous rocks and several types of breccias the Fra Mauro and Apennine sites of Apollo 14 and 15 are reported and interpreted. The crystalline rocks are found to differ substantially from the Apollo 11 and 12 basalts. Substructures in the Apollo 14 breccias are complex. At least two bonding mechanisms can be discerned from the electron petrographic examination: (a) 'shock sintering' due to high pressures and temperatures associated with the shock waves of meteoritic impacts; and (b) lithification by glass bonding.

Lally, J. S.↗