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At least 145 records · Page 8

Improved performance of silicon nitride-based high temperature ceramics

Recent progress in the production of Si3N4 based ceramics is reviewed: (1) high temperature strength and toughness of hot pressed Si3N4 were improved by using high purity powder and a stabilized ZrO2 additive, (2) impact resistance of hot pressed Si3N4 was increased by the use of a crushable energy absorbing layer, (3) the oxidation resistance and strength of reaction sintered Si3N4 were increased by impregnating reaction sintered silicon nitride with solutions that oxidize to Al2O3 or ZrO2, (4) beta prime SiA1ON compositions and sintering aids were developed for improved oxidation resistance or improved high temperature strength.

Ashbrook, R. L.↗

Study program to develop and evaluate die and container materials for the growth of silicon ribbons

Initial sessile drop experiments on SiC, Si3N4 and A1N were conducted. Very promising results were achieved on both SiC and Si3N4 where minimal penetration of these CNTD coatings by molten silicon was observed. More detailed characterization of the CNTD microstructures was accomplished as well as X-ray characterization of the third and fourth candidate materials system sets (i.e. A1N and altered Si3N4). Polished sections of post sessile drop specimens were also prepared and evaluated. The techniques of full scale crucible hot pressing were developed and die grinding development was initiated. The apparatus for measurement of oxygen partial pressure was reconstructed and calibrated. The sessile drop temperature measurement procedure was calibrated for absorption by the pyrex view-port and additional Auger electron analysis was performed at the interface of molten silicon with CNTD Si3N4 and A1N.

Source record↗

Development and Evaluation of Die Materials for Use in the Growth of Silicon Ribbons by the Inverted Ribbon Growth Process. Task 2: LSSA Project

Several ribbon growth experiments were performed from V-shaped dies coated with CVD Si3N4. The most significant result was the ability to perform five consecutive growth runs from the same die without mechanical degradation of the die through temperature cycling. The die was made from vitreous carbon coated with CVD Si3N4. Silicon oxynitride, Si2N2O, was examined with respect to thermal stability in contact with molten silicon. The results of X-ray analysis indicate that this material is converted to both alpha - and beta-Si3N4 in the presence of molten silicon. Experiments on the stability of CVD SiOxNy shoe that this material can be maintained in contact with molten silicon (sessile drop test) for greater than 30 h at 1450 C without total decompositon. These layers are converted mainly to beta-Si3N4.

Duffy, M. T.↗

Variations in pore structure of reaction-bonded silicon nitride /RBSN/

A discussion is presented relating the observed pore structures (sizes) to the reaction mechanisms in reaction-bonded silicon nitride (alpha- and beta-Si3N4) on the basis of information available from the literature. While the techniques for reducing the residual macroporosity are quite well-developed for reaction-bonded Si3N4 (RBSN), it is important to be aware of three other orders of magnitude for porosity present in RBSN as a result of the nitriding process itself, and how these types of nitridation-induced porosity can be controlled. For ease of description, these types of nitridation-induced porosity are called micropores, nanopores, and picopores in order of their decreasing size. A scanning electron micrograph is presented, showing nanopores isolated in the unreacted Si and picopores in the alpha-matte Si3N4. The assumption that an alpha-matte growth mechanism is active explains the occurrence of nanopores and their partial filling with alpha-Si3N4, leaving behind very fine-grained alpha-matte and picopores.

Danforth, S. C.↗

Friction and Wear of Monolithic and Fiber Reinforced Silicon-Ceramics Sliding Against IN-718 Alloy at 25 to 800 C in Atmospheric Air at Ambient Pressure

The friction and wear of monolithic and fiber reinforced Si-ceramics sliding against the nickel base alloy IN-718 at 25 to 800 C was measured. The monolithic materials tested were silicon carbide (SiC), fused silica (SiO2), syalon, silicon nitride (Si3N4) with W and Mg additives, and Si3N4 with Y2O3 additive. At 25 C fused silica had the lowest friction while Si3N4 (W,Mg type) had the lowest wear. At 800 C syalon had the lowest friction while Si3N4 (W,Mg type) and syalon had the lowest wear. The SiC/IN-718 couple had the lowest total wear at 25 C. At 800 C the fused silica/IN-718 couple exhibited the least total wear. SiC fiber reinforced reaction bonded silicon nitride (RBSN) composite material with a porosity of 32 percent and a fiber content of 23 vol percent had a lower coefficient of friction and wear when sliding parallel to the fiber direction than in the perpendicular at 25 C. The coefficient of friction for the carbon fiber reinforced borosilicate composite was 0.18 at 25 C. This is the lowest of all the couples tested. Wear of this material was about two decades smaller than that of the monolithic fused silica. This illustrates the large improvement in tribological properties which can be achieved in ceramic materials by fiber reinforcement. At higher temperatures the oxidation products formed on the IN-718 alloy are transferred to the ceramic by sliding action and forms a thin, solid lubricant layer which decreases friction and wear for both the monolithic and fiber reinforced composites.

Deadmore, Daniel L.↗

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.↗

Hot isostatic pressing of silicon nitride with boron nitride, boron carbide, and carbon additions

Si3N4 test bars containing additions of BN, B4C, and C, were hot isostatically pressed in Ta cladding at 1900 and 2050 C to 98.9 percent to 99.5 percent theoretical density. Room-temperature strength data on specimens containing 2 wt pct BN and 0.5 wt pct C were comparable to data obtained for Si3N4 sintered with Y2O3, Y2O3 and Al2O3, or ZrO2. The 1370 C strengths were less than those obtained for additions of Y2O3 or ZrO2 but greater than those obtained from a combination of Y2O3 and Al2O3. SEM fractography indicated that, as with other types of Si3N4, room-temperature strength was controlled by processing flaws. The decrease in strength at 1370 C was typical of Si3N4 having an amorphous grain-boundary phase. The primary advantage of nonoxide additions appears to be in facilitating specimen removal from the Ta cladding.

Mieskowski, Diane M.↗

Indirect measurement of the viscosity of the intergranular glass phase in yttria-sintered silicon nitride

Dense, sintered Si3N4 possesses a residual intergranular glass phase which softens at high temperatures, resulting in degradation of the ceramic's mechanical properties at high temperatures. An important parameter in the determination of the high temperature mechanical properties of sintered Si3N4 is the temperature-viscosity relationship of the intergranular glass. A method for indirectly measuring the intergranular glass viscosity at a given temperature using physical modelling of a two phase glass crystal microstructure and beam bending viscometry measurements of Si3N4 is described. Intergranular glass viscosities obtained by this method are presented for a yttria sintered Si3N4.

Dittmar, Mark B.↗

Diamond and diamondlike carbon as wear-resistant, self-lubricating coatings for silicon nitride

Recent work on the friction and wear properties of as-deposited fine-grain diamond, polished coarse-grain diamond, and as-deposited diamondlike carbon (DLC) films in humid air at a relative humidity of approximately 40 percent and in dry nitrogen is reviewed. Two types of chemical vapor deposition (CVD) processes are used to deposit diamond films on silicon nitride (Si3N4) substrates: microwave-plasma and hot-filament. Ion beams are used to deposit DLC films of Si3N4 substrates. The diamond and DLC films in sliding contact with hemispherical bare Si3N4 pins have low steady-state coefficients of friction (less than 0.2) and low wear rates (less than 10(exp -7) mm(exp 2)/N-m), and thus, can be used effectively as wear-resistant, self-lubricating coatings for Si3N4 in the aforementioned two environments.

Miyoshi, Kazuhisa↗

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.↗

Joining and Integration of Silicon Nitride Ceramics for Aerospace and Energy Systems

Light-weight, creep-resistant silicon nitride ceramics possess excellent high-temperature strength and are projected to significantly raise engine efficiency and performance when used as turbine components in the next-generation turbo-shaft engines without the extensive cooling that is needed for metallic parts. One key aspect of Si3N4 utilization in such applications is its joining response to diverse materials. In an ongoing research program, the joining and integration of Si3N4 ceramics with metallic, ceramic, and composite materials using braze interlayers with the liquidus temperature in the range 750-1240C is being explored. In this paper, the self-joining behavior of Kyocera Si3N4 and St. Gobain Si3N4 using a ductile Cu-based active braze (Cu-ABA) containing Ti will be presented. Joint microstructure, composition, hardness, and strength as revealed by optical microscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Knoop microhardness test, and offset compression shear test will be presented. Additionally, microstructure, composition, and joint strength of Si3N4/Inconel 625 joints made using Cu-ABA, will be presented. The results will be discussed with reference to the role of chemical reactions, wetting behavior, and residual stresses in joints.

Singh, M.↗

Low-Mass Planar Photonic Imaging Sensor

Continuing on the successful progress of NIAC Phase I, this report summarizes the technical progress achieved under NIAC Phase II during the performance period September 19, 2014-June 18, 2017. During this period, the research team has made the following accomplishments: designed and layout a silica photonic integrated circuit (PIC) as a two baseline interferometric imager; constructed an experiment to utilize the two baselines for complex visibility measurement on a point source and a variable width slit; analyzed and studied the testbed results. (in collaboration with Lockheed Martin); designed and layout Si3N4 PICs for the low-resolution and high-resolution SPIDER telescope; fabricated the multi-layer Si3N4 PIC for low and high resolution SPIDER telescope; characterize the optical throughput and heater response for Si3N4 PIC for low and high resolution SPIDER telescopes; carried out imaging experiments using the Si3N4 PIC low-resolution version (in collaboration with Lockheed Martin); investigated signal-to-noise (SNR) ratio of SPIDER imager compared to the conventional panchromatic imager (in collaboration with Lockheed Martin); fulfilled the SNR simulation upon SPIDER imager (in collaboration with Lockheed Martin).

Yoo, S. J. Ben↗

Low-Mass Planar Photonic Imaging Sensor

Continuing on the successful progress of NIAC (NASA Innovative Advanced Concepts) Phase I, this report summarizes the technical progress achieved under NIAC Phase II during the performance period September 19, 2014 to June 18, 2017. During this period, the research team has made the following accomplishments: designed and layout a silica photonic integrated circuit (PIC) as a two baselineinterferometric imager; constructed an experiment to utilize the two baselines for complex visibility measurementon a point source and a variable width slit; analyzed and studied the testbed results (in collaboration with Lockheed Martin); designed and layout Si3N4 PICs for the low-resolution and high-resolution SPIDER (Segmented Planar Imaging Detector for Electro-Optical Reconnaissance) telescope; fabricated the multi-layer Si3N4 PIC for low and high resolution SPIDER telescope; characterized the optical throughput and heater response for Si3N4 PIC for low and highresolution SPIDER telescopes; carried out imaging experiments using the Si3N4 PIC low-resolution version (in collaboration with Lockheed Martin); investigated signal-to-noise (SNR) ratio of SPIDER imager compared to the conventional panchromatic imager (in collaboration with Lockheed Martin); fulfilled the SNR simulation upon SPIDER imager (in collaboration with Lockheed Martin).

Yoo, S. J. Ben↗

Development and evaluation of die materials for use in the growth of silicon ribbons by the inverted ribbon growth process, task 2, LSSA project

Silicon sessile drop experiments were performed on a variety of commercially available refractory carbides, nitrides, oxides, and borides to examine the potential of these materials for applications involving either direct contact with molten silicon or as substrates for CVD coatings in the fabrication of dies and crucibles for containing molten silicon. Simultaneous experiments were also conducted with CVD layers of SiC, Si3N4, and SiOxNy. Silicon nitride layers, deposited with NH3:SiH4 ratios ranging from 100:1 down to 5:1, were examined in sessile drop experiments to determine if the layers are degraded as a result of using lower reagent ratios. Preliminary experiments were undertaken on the stability of CVD Si3N4 near the melting point of silicon. Silicon ribbon segments were grown from vitreous carbon dies which had been coated with CVD Si3N4. Depending upon the purity of the die materials, ribbon resistivity values up to 40 Omega cm were obtained.

Duffy, M. T.↗

Development and evaluation of die materials for use in the growth of silicon ribbons by the inverted ribbon growth process, task 2. LSSA project

The results of emission spectroscopic analysis indicate that molten silicon can remain in contact with hot-pressed Si3N4 (99.2 percent theoretical density) for prolonged periods without attaining the impurity content level of the nitride. Although MgO was used as binder, Mg was not found present in the silicon sessile drop in quantities much above the level initially present in the silicon source material. Preliminary experiments with EFG-type dies coated with CVD Si3N4 or CVD SiOxNy indicate that capillary rise does not occur readily in these dies. The same was found to be true of hot-pressed and reaction-sintered Si3N4 obtained commercially. However, when dies were formed by depositing CVD layers on shaped silicon slabs, a column of molten silicon was maintained in each CVD die while being heated in contact with a crucible of molten silicon. Preliminary wetting of dies appears necessary for EFG growth. Several ribbon growth experiments were performed from V-shaped dies.

Duffy, M. T.↗

Study Program to Develop and Evaluate Die and Container Materials for the Growth of Silicon Ribbons

The completion of a major hardware delivery milestone was accomplished with the delivery of three CNTD Si3N4 coated hot pressed Si3N4 crucibles. A limited characterization of the coating was performed at MRL prior to delivery. The coatings were fine grained alpha - Si3N4. It was determined that a two piece die design is required. The importance of the role of oxygen in influencing the attack of the CNTD materials by molten silicon was demonstrated. The stability is greatly enhanced by maintaining the oxygen partial pressure near or below the Si + O2 = SiO2 equilibrium.

Ounby, P. D.↗

Development of SiAlON materials

Cold pressing and sintering techniques were used to produce ceramic test specimens in which the major phase was either Si3N4 or a solid solution having the beta Si3N4 structure. Additional components were incorporated to promote liquid phase sintering. Glass and/or crystalline phase were consequently retained in boundaries between Si3N4 grains which largely determined the physical properties of the bodies. Systems investigated most extensively included R-Si-Al-O-N (R = rare earth element) Zr-Si-Al-O-N, Y-Si-Be-O-N, and R1-R2-Si-O-N. Room temperature and 1370 C modulus of ruptured, 1370 C creep, and oxidation behavior are discussed in terms of phase relationships in a parent quinery, and relavent oxide systems.

Layden, G. K.↗

Formation of porous surface layers in reaction bonded silicon nitride during processing

An effort was undertaken to determine if the formation of the generally observed layer of large porosity adjacent to the as-nitride surfaces of reaction bonded silicon nitrides could be prevented during processing. Isostatically pressed test bars were prepared from wet vibratory milled Si powder. Sintering and nitriding were each done under three different conditions:(1) bars directly exposed to the furnance atmosphere; (2) bars packed in Si powder; (3) bars packed in Si3N4 powder. Packing the bars in either Si of Si3N4 powder during sintering retarded formation of the layer of large porosity. Only packing the bars in Si prevented formation of the layer during nitridation. The strongest bars (316 MPa) were those sintered in Si and nitrided in Si3N4 despite their having a layer of large surface porosity; failure initiated at very large pores and inclusions. The alpha/beta ratio was found to be directly proportional to the oxygen content; a possible explanation for this relationship is discussed.

Shaw, N. J.↗