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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 NTRS1991

Correlated Si isotope anomalies and large C-13 enrichments in a family of exotic SiC grains

A hypothesis is presented to the effect that the distinctive morphological characteristics and comparatively simple Si isotope systematics identify the platy SiC crystals as a genetically related family, formed around a single isotopically heterogeneous presolar star on an association of related stars. The enrichments in C-13 and the Si isotope systematics of the platy SiC are broadly consistent with theoretical models of nucleosynthesis in low-mass, carbon stars on the ASG. The Si isotope array most plausibly reflects mixing between (Si-28)-rich material, inherited from a previous generation of stars, and material enriched in Si-29 and Si-30, produced in intershell regions by neutron capture during He-burning. The absence of a correlation between the Si and C isotopic compositions of the SiC suggests either episodic condensation of SiC, extending over several thermal pulses, in the atmosphere of a single star, or the derivation of the SiC from several stars characterized by different rates of C-13 production.

Stone, J.↗

NASA NTRS1992

SiC lightweight telescopes for advanced space applications. II - Structures technology

A critical technology area for lightweight SiC-based telescope systems is the structural integrity and thermal stability over spaceborne environmental launch and thermal operating conditions. Note, it is highly desirable to have an inherently athermal design of both SiC mirrors and structure. SSG has developed an 8 inch diameter SiC telescope system for brassboard level optical and thermal testing. The brassboard telescope has demonstrated less than 0.2 waves P-V in the visible wavefront change over +50 C to -200 C temperature range. SSG has also fabricated a SiC truss structural assembly and successfully qualified this hardware at environmental levels greater than 3 times higher than normal Delta, Titan, and ARIES launch loads. SSG is currently developing two SiC telescopes; an 20 cm diameter off-axis 3 mirror re-imaging and a 60 cm aperture on-axis 3 mirror re-imager. Both hardware developments will be tested to flight level environmental, optical, and thermal specifications.

Anapol, Michael I.↗

NASA NTRS1992

CVD of SiC and AlN using cyclic organometallic precursors

The use of cyclic organometallic molecules as single-source MOCVD precursors is illustrated by means of examples taken from our recent work on AlN and SiC deposition, with particular focus on SiC. Molecules containing (AlN)3 and (SiC)2 rings as the 'core structure' were employed as the source materials for these studies. The organoaluminum amide, (Me2AlNH2)3, was used as the AlN source and has been studied in a molecular beam sampling apparatus in order to determine the gas phase species present in a hot-wall CVD reactor environment. In the case of SiC CVD, a series of disilacyclobutanes (Si(XX')CH2)2 (with X and X' = H, CH3, and CH2SiH2CH3), were examined in a cold-wall, hot-stage CVD reactor in order to compare their relative reactivities and prospective utility as single-source CVD precursors. The parent compound, disilacyclobutane, (SiH2CH2)2, was found to exhibit the lowest deposition temperature (ca. 670 C) and to yield the highest purity SiC films. This precursor gave a highly textured, polycrystalline film on the Si(100) substrates.

Interrante, L. V.↗

NASA NTRS1993

Direct observation of porous SiC formed by anodization in HF

A process for forming porous SiC from single-crystal SiC wafers has been demonstrated. Porous SiC can be fabricated by anodizing n-type 6H-SiC in HF under UV illumination. TEM reveals pores of sizes 10-30 nm with interpore spacings ranging from roughly 5 to 150 nm. This is the first reported direct observation of porous SiC formation.

Shor, Joseph S.↗

NASA NTRS1998

Study of Bulk and Elementary Screw Dislocation Assisted Reverse Breakdown in Low-Voltage (less than 250 V) 4H-SiC p(+)n Junction diodes: DC Properties - Part 1

Given the high density (approx. 10(exp 4)/sq cm) of elementary screw dislocations (Burgers vector = 1c with no hollow core) in commercial SiC wafers and epilayers, all appreciable current (greater than 1 A) SiC power devices will likely contain elementary screw dislocations for the foreseeable future. It is therefore important to ascertain the electrical impact of these defects, particularly in high-field vertical power device topologies where SiC is expected to enable large performance improvements in solid-state high-power systems. This paper compares the DC-measured reverse-breakdown characteristics of low-voltage (less than 250 V) small-area (less than 5 x 10(exp -4)/sq cm) 4H-SiC p(+)n diodes with and without elementary screw dislocations. Compared to screw dislocation-free devices, diodes containing elementary screw dislocations exhibited higher pre-breakdown reverse leakage currents, softer reverse breakdown I-V knees, and highly localized microplasmic breakdown current filaments. The observed localized 4H-SiC breakdown parallels microplasmic breakdowns observed in silicon and other semiconductors, in which space-charge effects limit current conduction through the local microplasma as reverse bias is increased.

Neudeck, Philip G.↗

NASA NTRS1999

Study of Bulk and Elementary Screw Dislocation Assisted Reverse Breakdown in Low-Voltage (<250 V) 4H-SiC p+n Junction Diodes - Part 1: DC Properties

Given the high density (approx. 10(exp 4)/sq cm) of elementary screw dislocations (Burgers vector = lc with no hollow core) in commercial SiC wafers and epilayers, all appreciable current (greater than 1 A) SiC power devices will likely contain elementary screw dislocations for the foreseeable future. It is therefore important to ascertain the electrical impact of these defects, particularly in high-field vertical power device topologies where SiC is expected to enable large performance improvements in solid-state high-power systems. This paper compares the DC-measured reverse-breakdown characteristics of low-voltage (less than 250 V) small-area (less than 5 x 10(exp -4) sq cm) 4H-SiC p(+)n diodes with and without elementary screw dislocations. Compared to screw dislocation-free devices, diodes containing elementary screw dislocations exhibited higher pre-breakdown reverse leakage currents, softer reverse breakdown I-V knees, and highly localized microplasmic breakdown current filaments. The observed localized 4H-SiC breakdown parallels microplasmic breakdowns observed in silicon and other semiconductors, in which space-charge effects limit current conduction through the local microplasma as reverse bias is increased.

Neudeck, Philip G.↗

NASA NTRS1998

"Un-annealed and Annealed Pd Ultra-Thin Film on SiC Characterized by Scanning Probe Microscopy and X-ray Photoelectron Spectroscopy"

Pd/SiC has been used as a hydrogen and a hydrocarbon gas sensor operated at high temperature. UHV (Ultra High Vacuum)-Scanning Tunneling Microscopy (STM), Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS) techniques were applied to study the relationship between the morphology and chemical compositions for Pd ultra-thin films on SiC (less than 30 angstroms) at different annealing temperatures. Pd ultra-thin film on 6H-SiC was prepared by the RF sputtering method. The morphology from UHV-STM and AFM shows that the Pd thin film was well deposited on SiC substrate, and the Pd was partially aggregated to round shaped participates at an annealing temperature of 300 C. At 400 C, the amount of surface participates decreases, and some strap shape participates appear. From XPS, Pd2Si was formed on the surface after annealing at 300 C, and all Pd reacted with SiC to form Pd2Si after annealing at 400 C. The intensity of the XPS Pd peak decreases enormously at 400 C. The Pd film diffused into SiC, and the Schottky barrier height has almost no changes. The work shows the Pd sicilides/SiC have the same electronic properties with Pd/SiC, and explains why the Pd/SiC sensor still responds to hydrogen at high operating temperatures.

Lu, W. J.↗

NASA NTRS1994

The Influence of SiC on the Ablation Response of Advanced Refractory Composite Materials

In continuing our studies of advanced refractory composite materials we have recently completed an arc-jet test series of a diverse group of ceramics and ceramic matrix composites. The compositions range from continuous fiber reinforced ceramics to monoliths. Many of these materials contain SiC and one objective of this test series was to identify the influence of SiC oxidation mechanisms on material performance. Hence the arc heater was operated at two conditions; one in which the passive oxidation of SiC would be dominant and the other where the active oxidation of SiC would be dominant. It is shown here that the active oxidation mechanism of SiC does not dominate material performance when it is present at levels equal to or below 20 volume percent.

Bull, Jeffrey D.↗

NASA NTRS1999

Sensor Lead Wires Positioned on SiC-based Monolithic Ceramic and Fiber- reinforced Ceramic Matrix Composite Subcomponents with Flat and Curved Surfaces

There is strong interest in the development of silicon carbide-based monolithic ceramic and composite materials and components for demanding, high-temperature applications. Thorough characterization of material properties, including high-temperature testing under simulated or actual operating conditions, is a high priority for programs involved in developing these silicon carbide- (SiC) based materials and components. Members of the Sensors and Electronics Technology Branch at the NASA Lewis Research Center are developing minimally intrusive methods of measuring the properties (such as the surface temperature, strain, and heat flux characteristics) of components and subelements that are being tested or operated in hostile, high-temperature environments. Their primary goal is to instrument the test article or operating component with durable sensors that have a minimal effect on test conditions such as the gas flow across the surface of the item and the material response (including the through-thickness conduction of heat). Therefore, the main thrust of their work has been the development of thin-film sensors (e.g., thermocouples or strain gauges) for use on various advanced material test articles, including SiC/SiC composite components. There was a need for a better method of securing sensor lead wires on SiC-based components and subelements that would be tested at temperatures to 1000 C (or higher), to enhance the durability of the overall minimally intrusive sensor system. To address this need, Lewis researchers devised an alternative approach for positioning the sensor lead wires (which are connected to the thin-film sensors) on SiC or SiC/SiC components. A reaction-forming method of joining was used to strongly bond hoop-shaped monolithic SiC and SiC/SiC composite attachments of various sizes to both flat and curved surfaces of SiC/SiC composite subelements (see the photos). This approach is based on an affordable, robust ceramic joining technology, named ARCJoinT, which was developed at Lewis for the joining of SiC-based ceramics and fiber-reinforced composites.

Kiser, James D.↗

NASA NTRS2003

Packaging Technology Designed, Fabricated, and Assembled for High-Temperature SiC Microsystems

A series of ceramic substrates and thick-film metalization-based prototype microsystem packages designed for silicon carbide (SiC) high-temperature microsystems have been developed for operation in 500 C harsh environments. These prototype packages were designed, fabricated, and assembled at the NASA Glenn Research Center. Both the electrical interconnection system and the die-attach scheme for this packaging system have been tested extensively at high temperatures. Printed circuit boards used to interconnect these chip-level packages and passive components also are being fabricated and tested. NASA space and aeronautical missions need harsh-environment, especially high-temperature, operable microsystems for probing the inner solar planets and for in situ monitoring and control of next-generation aeronautical engines. Various SiC high-temperature-operable microelectromechanical system (MEMS) sensors, actuators, and electronics have been demonstrated at temperatures as high as 600 C, but most of these devices were demonstrated only in the laboratory environment partially because systematic packaging technology for supporting these devices at temperatures of 500 C and beyond was not available. Thus, the development of a systematic high-temperature packaging technology is essential for both in situ testing and the commercialization of high-temperature SiC MEMS. Researchers at Glenn developed new prototype packages for high-temperature microsystems using ceramic substrates (aluminum nitride and 96- and 90-wt% aluminum oxides) and gold (Au) thick-film metalization. Packaging components, which include a thick-film metalization-based wirebond interconnection system and a low-electrical-resistance SiC die-attachment scheme, have been tested at temperatures up to 500 C. The interconnection system composed of Au thick-film printed wire and 1-mil Au wire bond was tested in 500 C oxidizing air with and without 50-mA direct current for over 5000 hr. The Au thick-film metalization-based wirebond electrical interconnection system was also tested in an extremely dynamic thermal environment to assess thermal reliability. The I-V curve1 of a SiC high-temperature diode was measured in oxidizing air at 500 C for 1000 hr to electrically test the Au thick-film material-based die-attach assembly.

Chen, Liang-Yu↗

NASA NTRS2006

Deep Reactive Ion Etching (DRIE) of High Aspect Ratio SiC Microstructures using a Time-Multiplexed Etch-Passivate Process

High aspect ratio silicon carbide (SiC) microstructures are needed for microengines and other harsh environment micro-electro-mechanical systems (MEMS). Previously, deep reactive ion etching (DRIE) of low aspect ratio (AR less than or = 1) deep (greater than 100 micron) trenches in SiC has been reported. However, existing DRIE processes for SiC are not well-suited for definition of high aspect ratio features because such simple etch-only processes provide insufficient control over sidewall roughness and slope. Therefore, we have investigated the use of a time-multiplexed etch-passivate (TMEP) process, which alternates etching with polymer passivation of the etch sidewalls. An optimized TMEP process was used to etch high aspect ratio (AR greater than 5) deep (less than 100 micron) trenches in 6H-SiC. Power MEMS structures (micro turbine blades) in 6H-SiC were also fabricated.

Evans, Laura J.↗

NASA NTRS1994

Porous silicon carbide (SiC) semiconductor device

A semiconductor device employs at least one layer of semiconducting porous silicon carbide (SiC). The porous SiC layer has a monocrystalline structure wherein the pore sizes, shapes, and spacing are determined by the processing conditions. In one embodiment, the semiconductor device is a p-n junction diode in which a layer of n-type SiC is positioned on a p-type layer of SiC, with the p-type layer positioned on a layer of silicon dioxide. Because of the UV luminescent properties of the semiconducting porous SiC layer, it may also be utilized for other devices such as LEDs and optoelectronic devices.

Shor, Joseph S.↗

NASA NTRS2009

SiC Optically Modulated Field-Effect Transistor

An optically modulated field-effect transistor (OFET) based on a silicon carbide junction field-effect transistor (JFET) is under study as, potentially, a prototype of devices that could be useful for detecting ultraviolet light. The SiC OFET is an experimental device that is one of several devices, including commercial and experimental photodiodes, that were initially evaluated as detectors of ultraviolet light from combustion and that could be incorporated into SiC integrated circuits to be designed to function as combustion sensors. The ultraviolet-detection sensitivity of the photodiodes was found to be less than desired, such that it would be necessary to process their outputs using high-gain amplification circuitry. On the other hand, in principle, the function of the OFET could be characterized as a combination of detection and amplification. In effect, its sensitivity could be considerably greater than that of a photodiode, such that the need for amplification external to the photodetector could be reduced or eliminated. The experimental SiC OFET was made by processes similar to JFET-fabrication processes developed at Glenn Research Center. The gate of the OFET is very long, wide, and thin, relative to the gates of typical prior SiC JFETs. Unlike in prior SiC FETs, the gate is almost completely transparent to near-ultraviolet and visible light. More specifically: The OFET includes a p+ gate layer less than 1/4 m thick, through which photons can be transported efficiently to the p+/p body interface. The gate is relatively long and wide (about 0.5 by 0.5 mm), such that holes generated at the body interface form a depletion layer that modulates the conductivity of the channel between the drain and the source. The exact physical mechanism of modulation of conductivity is a subject of continuing research. It is known that injection of minority charge carriers (in this case, holes) at the interface exerts a strong effect on the channel, resulting in amplification of the photon-detection signal. A family of operating curves characterizing the OFET can be generated in a series of measurements performed at different intensities of incident ultraviolet light.

Tabib-Azar, Massood↗

NASA NTRS2011

Active Oxidation of SiC

The high temperature oxidation of silicon carbide occurs in either a passive or active mode, depending on temperature and oxygen potential. Passive oxidation forms a protective oxide film which limits attack of the SiC:SiC(s) + 3/2 O2(g) = SiO2(s) + CO(g.) Active oxidation forms a volatile oxide and leads to extensive attack of the SiC: SiC(s) + O2(g) = SiO(g) + CO(g). The transition points and rates of active oxidation are a major issue. Previous studies are reviewed and the leading theories of passive/active transitions summarized. Comparisons are made to the active/passive transitions in pure Si, which are relatively well-understood. Critical questions remain about the difference between the active-to-passive transition and passive-to-active transition. For Si, Wagner [2] points out that the active-to-passive transition is governed by the criterion for a stable Si/SiO2 equilibria and the passive-to-active transition is governed by the decomposition of the SiO2 film. This suggests a significant oxygen potential difference between these two transitions and our experiments confirm this. For Si, the initial stages of active oxidation are characterized by the formation of SiO(g) and further oxidation to SiO2(s) as micron-sized rods, with a distinctive morphology. SiC shows significant differences. The active-to-passive and the passive-to-active transitions are close. The SiO2 rods only appear as the passive film breaks down. These differences are explained in terms of the reactions at the SiC/SiO2 interface. In order to understand the breakdown of the passive film, pre-oxidation experiments are conducted. These involve forming dense protective scales of 0.5, 1, and 2 microns and then subjecting the samples with these scales to a known active oxidation environment. Microstructural studies show that SiC/SiO2 interfacial reactions lead to a breakdown of the scale with a distinct morphology.

Jacobson, Nathan S.↗

NASA NTRS2004

SiC-Based Miniature High-Temperature Cantilever Anemometer

The figure depicts a miniature cantilever-type anemometer that has been developed as a prototype of compact, relatively nonintrusive anemometers that can function at temperatures up to 600 C and that can be expected to be commercially mass-producible at low cost. The design of this anemometer, and especially the packaging aspect of the design, is intended to enable measurement of turbulence in the high-temperature, high-vibration environment of a turbine engine or in any similar environment. The main structural components of the anemometer include a single-crystal SiC cantilever and two polycrystalline SiC clamping plates, all made from chemical-vapor-deposited silicon carbide. Fabrication of these components from the same basic material eliminates thermal-expansion mismatch, which has introduced spurious thermomechanical stresses in cantilever-type anemometers of prior design. The clamping plates are heavily oxidized to improve electrical insulation at high temperature. A cavity that serves as a receptacle for the clamped end of the cantilever is etched into one end of one clamping plate. Trenches that collectively constitute a socket for a multipin electrical plug (for connection to external electronic circuitry) are etched into the opposite end of this clamping plate. Metal strips for electrical contact are deposited on one face of the other clamping plate. Piezoresistive single-crystal SiC thin-film strain gauges are etched in the n-type SiC epilayer in a Wheatstone-bridge configuration. Metal contact pads on the cantilever that extend into the clamping-receptacle area, are obtained by deposition and patterning using standard semiconductor photolithography and etching methods. The cantilever and the two clamping plates are assembled into a sandwich structure that is then clamped in a stainless-steel housing. The Wheatstone- bridge carrying SiC cantilever with the metal contact pads on the piezoresistors is slid into the receptacle in the bottom clamping plate. The top clamping plate is brought into contact with the bottom plate so that the narrow section of the metal strips on the top clamp plate aligns with the metal contact pads on the cantilever. When the parts are clamped together, the metal strips provide electrical connections between the Wheatstone-bridge contact points and the sides the trenches that constitute the socket for the multipin electrical plug. Hence, to connect the Wheatstone bridge to external circuitry for processing of the anemometer readout, one need only insert the plug in the socket. In operation, the cantilever end of the stainless-steel housing is mounted flush with an engine wall and the unclamped portion of the cantilever is exposed into the flow. The cantilever is deflected in direct proportion to the force induced by component of flow parallel to the engine wall and perpendicular to the broad exposed face of the cantilever. The maximum strain on the cantilever occurs at the clamped edge and is measured by the piezoresistors, which are located there. The corresponding changes in resistance manifest themselves in the output of the Wheatstone bridge.

Okojie, Robert S.↗

NASA NTRS2014

Structural Characterization of Lateral-grown 6H-SiC am-plane Seed Crystals by Hot Wall CVD Epitaxy

The performance of commercially available silicon carbide (SiC) power devices is limited due to inherently high density of screw dislocations (SD), which are necessary for maintaining polytype during boule growth and commercially viable growth rates. The NASA Glenn Research Center (GRC) has recently proposed a new bulk growth process based on axial fiber growth (parallel to the c-axis) followed by lateral expansion (perpendicular to the c-axis) for producing multi-faceted m-plane SiC boules that can potentially produce wafers with as few as one SD per wafer. In order to implement this novel growth technique, the lateral homoepitaxial growth expansion of a SiC fiber without introducing a significant number of additional defects is critical. Lateral expansion is being investigated by hot wall chemical vapor deposition (HWCVD) growth of 6H-SiC am-plane seed crystals (0.8mm x 0.5mm x 15mm) designed to replicate axially grown SiC single crystal fibers. The post-growth crystals exhibit hexagonal morphology with approximately 1500 m (1.5 mm) of total lateral expansion. Preliminary analysis by synchrotron white beam x-ray topography (SWBXT) confirms that the growth was homoepitaxial, matching the polytype of the respective underlying region of the seed crystal. Axial and transverse sections from the as grown crystal samples were characterized in detail by a combination of SWBXT, transmission electron microscopy (TEM) and Raman spectroscopy to map defect types and distribution. X-ray diffraction analysis indicates the seed crystal contained stacking disorders and this appears to have been reproduced in the lateral growth sections. Analysis of the relative intensity for folded transverse acoustic (FTA) and optical (FTO) modes on the Raman spectra indicate the existence of stacking faults. Further, the density of stacking faults is higher in the seed than in the grown crystal. Bundles of dislocations are observed propagating from the seed in m-axis lateral directions. Contrast extinction analysis of these dislocation lines reveals they are edge type basal plane dislocations that track the growth direction. Polytype phase transition and stacking faults were observed by high-resolution TEM (HRTEM), in agreement with SWBXT and Raman scattering.

Single Crystal↗

NASA NTRS2010

Development of SiC Large Tapered Crystal Growth

Majority of very large potential benefits of wide band gap semiconductor power electronics have NOT been realized due in large part to high cost and high defect density of commercial wafers. Despite 20 years of development, present SiC wafer growth approach is yet to deliver majority of SiC's inherent performance and cost benefits to power systems. Commercial SiC power devices are significantly de-rated in order to function reliably due to the adverse effects of SiC crystal dislocation defects (thousands per sq cm) in the SiC wafer.

Neudeck, Phil↗