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NASA NTRS2001

Microstructure and Tensile Properties of BN/SiC Coated Hi-Nicalon, and Sylramic SiC Fiber Preforms

Batch to batch and within batch variations, and the influence of fiber architecture on room temperature physical and tensile properties of BN/SiC coated Hi-Nicalon and Sylramic SiC fiber preform specimens were determined. The three fiber architectures studied were plain weave (PW), 5-harness satin (5HS) and 8-harness satin (8HS) Results indicate that the physical properties vary up to 10 percent within a batch, and up to 20 percent between batches of preforms. Load-reload (Hysteresis) and acoustic emission methods were used to analyze damage accumulation occurring during tensile loading. Early acoustic emission activity, before observable hysteretic behavior, indicates that the damage starts with the formation of nonbridged tunnel cracks. These cracks then propagate and intersect the load bearing "0" fibers giving rise to hysteretic behavior, For the Hi-Nicalon preform specimens, the onset of "0" bundle cracking stress and strain appeared to be independent of the fiber architecture. Also, the "0" fiber bundle cracking strain remained nearly the same for the preform specimens of both fiber types. Transmission Electron Microscope (TEM) analysis indicates that the Chemical Vapor Infiltration (CVI) Boron Nitride (BN) interface coating is mostly amorphous and contains carbon and oxygen impurities, and the CVI SiC coating is crystalline. No reaction exists between the CVI BN and SiC coating.

Bhatt, Ramakrishna T.↗

NASA NTRS1995

Effect of Stacking Faults on the X-Ray Diffraction Profiles of Beta-SiC Powders

X-ray diffraction patterns or beta-SiC (3C or the cubic polytype or sic) powders often exhibit an additional peak at d = 0.266 nm, high background intensity around the (111) peak, and relative intensities for peaks which differ from those predicted from the crystal structure. Computer simulations were used to show that all these features are due to stacking faults in the powders and not due to the presence of other polytypes in the powders. Such simulations allow diffraction patterns to be generated for different types, frequencies, and spatial distribution or faults. Comparison of the simulation results to the XRD data indicates that the B-SiC particles consist either of heavily faulted clusters distributed irregularly between regions that have only occasional faults or twins, or the powders consist of two types of particles with different populations of faults: those with a high density of faults and those with only twins or occasional faults. Additional information is necessary to determine which description is correct. However, the simulation results can be used to rule out certain fault configurations.

Pujar, Vijay V.↗

NASA NTRS2002

Microstructure and Tensile Properties of BN/SiC Coated Hi-Nicalon, and Sylramic SiC Fiber Preforms

Batch to batch and within batch variations, and the influence of fiber architecture on room temperature physical and tensile properties of BN/SiC coated Hi-Nicalon and Sylramic SiC fiber preform specimens were determined. The three fiber architectures studied were plain weave (PW), 5-harness satin (5HS), and 8-harness satin (8HS). Results indicate that the physical properties vary up to 10 percent within a batch, and up to 20 percent between batches of preforms. Load-reload (Hysteresis) and acoustic emission methods were used to analyze damage accumulation occurring during tensile loading. Early acoustic emission activity, before observable hysteretic behavior, indicates that the damage starts with the formation of nonbridged tunnel cracks. These cracks then propagate and intersect the load bearing "0 deg" fibers giving rise to hysteretic behavior. For the Hi-Nicalon preform specimens, the onset of "0 deg" bundle cracking stress and strain appeared to be independent of the fiber architecture. Also, the "0 deg" fiber bundle cracking strain remained nearly the same for the preform specimens of both fiber types. TEM analysis indicates that the CVI BN interface coating is mostly amorphous and contains carbon and oxygen impurities, and the CVI SiC coating is crystalline. No reaction exists between the CVI BN and SiC coating.

Bhatt, Ramakrishna T.↗

NASA NTRS2003

Application of Powder Diffraction Methods to the Analysis of Short- and Long-Range Atomic Order in Nanocrystalline Diamond and SiC: The Concept of the Apparent Lattice Parameter (alp)

Two methods of the analysis of powder diffraction patterns of diamond and SiC nanocrystals are presented: (a) examination of changes of the lattice parameters with diffraction vector Q ('apparent lattice parameter', alp) which refers to Bragg scattering, and (b), examination of changes of inter-atomic distances based on the analysis of the atomic Pair Distribution Function, PDF. Application of these methods was studied based on the theoretical diffraction patterns computed for models of nanocrystals having (i) a perfect crystal lattice, and (ii), a core-shell structure, i.e. constituting a two-phase system. The models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the shell. X-ray and neutron experimental diffraction data of nanocrystalline SiC and diamond powders of the grain diameter from 4 nm up to micrometers were used. The effects of the internal pressure and strain at the grain surface on the structure are discussed based on the experimentally determined dependence of the alp values on the Q-vector, and changes of the interatomic distances with the grain size determined experimentally by the atomic Pair Distribution Function (PDF) analysis. The experimental results lend a strong support to the concept of a two-phase, core and the surface shell structure of nanocrystalline diamond and SiC.

Palosz, B.↗

NASA NTRS2004

Measurement of N-Type 6H SiC Minority-Carrier Diffusion Lengths by Electron Bombardment of Schottky Barriers

Minority-Carrier diffusion lengths of n-type 6H-SiC were measured using the electron-beam induced current (EBIC) technique. Experimental values of primary beam current, EBIC, and beam voltage were obtained for a variety of SIC samples. This data was used to calculate experimental diode efficiency vs. beam voltage curves. These curves were fit to theoretically calculated efficiency curves, and the diffusion length and metal layer thickness were extracted. The hole diffusion length in n-6H SiC ranged from 0.93 +/- 0.15 microns.

Hubbard, S. M.↗

NASA NTRS1998

Interfacial Thickness Guidelines for SiC(Fiber)/SiC(Matrix) Composites

Researchers at the NASA Lewis Research Center have developed a guideline for the interface thickness necessary for SiC(Fiber)/SiC(Matrix) composites to demonstrate good composite properties. These composite materials have potential commercial applications for high-temperature structural components such as engine hot sections. Several samples of each were composed from three different small-diameter (less than 20 mm), polymer-derived SiC fibers that were woven into two-dimensional cloths and laid up as preforms. The preforms were treated with a chemical-vapor-infiltrated boron nitride layer as an interfacial coating on the fiber surfaces to provide the necessary debonding characteristics for successful composite behavior. Then, the preforms were filled with additional SiC as a matrix phase.

Hurst, Janet B.↗

NASA NTRS2002

Methods for growth of relatively large step-free SiC crystal surfaces

A method for growing arrays of large-area device-size films of step-free (i.e., atomically flat) SiC surfaces for semiconductor electronic device applications is disclosed. This method utilizes a lateral growth process that better overcomes the effect of extended defects in the seed crystal substrate that limited the obtainable step-free area achievable by prior art processes. The step-free SiC surface is particularly suited for the heteroepitaxial growth of 3C (cubic) SiC, AlN, and GaN films used for the fabrication of both surface-sensitive devices (i.e., surface channel field effect transistors such as HEMT's and MOSFET's) as well as high-electric field devices (pn diodes and other solid-state power switching devices) that are sensitive to extended crystal defects.

Neudeck, Philip G.↗

NASA NTRS2008

Tensile Creep and Fatigue of Sylramic-iBN Melt-Infiltrated SiC Matrix Composites: Retained Properties, Damage Development, and Failure Mechanisms

An understanding of the elevated temperature tensile creep, fatigue, rupture, and retained properties of ceramic matrix composites (CMC) envisioned for use in gas turbine engine applications are essential for component design and life-prediction. In order to quantify the effect of stress, time, temperature, and oxidation for a state-of-the-art composite system, a wide variety of tensile creep, dwell fatigue, and cyclic fatigue experiments were performed in air at 1204 C for the SiC/SiC CMC system consisting of Sylramic-iBN SiC fibers, BN fiber interphase coating, and slurry-cast melt-infiltrated (MI) SiC-based matrix. Tests were either taken to failure or interrupted. Interrupted tests were then mechanically tested at room temperature to determine the residual properties. The retained properties of most of the composites subjected to tensile creep or fatigue were usually within 20% of the as-produced strength and 10% of the as-produced elastic modulus. It was observed that during creep, residual stresses in the composite are altered to some extent which results in an increased compressive stress in the matrix upon cooling and a subsequent increased stress required to form matrix cracks. Microscopy of polished sections and the fracture surfaces of specimens which failed during stressed-oxidation or after the room-temperature retained property test was performed on some of the specimens in order to quantify the nature and extent of damage accumulation that occurred during the test. It was discovered that the distribution of stress-dependent matrix cracking at 1204 C was similar to the as-produced composites at room temperature; however, matrix crack growth occurred over time and typically did not appear to propagate through thickness except at final failure crack. Failure of the composites was due to either oxidation-induced unbridged crack growth, which dominated the higher stress regime (> 179 MPa) or controlled by degradation of the fibers, probably caused by intrinsic creep-induced flaw growth of the fibers or internal attack of the fibers via Si diffusion through the CVI SiC and/or microcracks at the lower stress regime (< 165 MPa).

Morscher, Greg↗

NASA NTRS2005

Demonstration of the First 4H-SiC EUV Detector with Large Detection Area

Ultraviolet (UV) and Extreme Ultraviolet (EUV) detectors are very attractive in astronomy, photolithography and biochemical applications. For EUV applications, most of the semiconductor detectors based on PN or PIN structures suffer from the very short penetration depth. Most of the carries are absorbed at the surface and recombined there due to the high surface recombination before reach the depletion region, resulting very low quantum efficiency. On the other hand, for Schottky structures, the active region starts from the surface and carriers generated from the surface can be efficiently collected. 4H-Sic has a bandgap of 3.26eV and is immune to visible light background noise. Also, 4H-Sic detectors usually have very good radiation hardness and very low noise, which is very important for space applications where the signal is very weak. The E W photodiodes presented in this paper are based on Schottky structures. Platinum (Pt) and Nickel (Ni) are selected as the Schottky contact metals, which have the highest electron work functions (5.65eV and 5.15eV, respectively) among all the known metals on 4H-Sic.

Xin, Xiaobin↗

NASA NTRS2012

A New Method to Grow SiC: Solvent-Laser Heated Floating Zone

The solvent-laser heated floating zone (solvent-LHFZ) growth method is being developed to grow long single crystal SiC fibers. The technique combines the single crystal fiber growth ability of laser heated floating zone with solvent based growth techniques (e.g. traveling solvent method) ability to grow SiC from the liquid phase. Initial investigations reported in this paper show that the solvent-LHFZ method readily grows single crystal SiC (retains polytype and orientation), but has a significant amount of inhomogeneous strain and solvent rich inclusions.

Woodworth, Andrew A.↗

NASA NTRS2011

Assessment of Durable SiC JFET Technology for +600 C to -125 C Integrated Circuit Operation

Electrical characteristics and circuit design considerations for prototype 6H-SiC JFET integrated circuits (ICs) operating over the broad temperature range of -125 C to +600 C are described. Strategic implementation of circuits with transistors and resistors in the same 6H-SiC n-channel layer enabled ICs with nearly temperature-independent functionality to be achieved. The frequency performance of the circuits declined at temperatures increasingly below or above room temperature, roughly corresponding to the change in 6H-SiC n-channel resistance arising from incomplete carrier ionization at low temperature and decreased electron mobility at high temperature. In addition to very broad temperature functionality, these simple digital and analog demonstration integrated circuits successfully operated with little change in functional characteristics over the course of thousands of hours at 500 C before experiencing interconnect-related failures. With appropriate further development, these initial results establish a new technology foundation for realizing durable 500 C ICs for combustion engine sensing and control, deep-well drilling, and other harsh-environment applications.

Neudeck, P. G.↗

NASA NTRS2012

A New Method to Grow SiC: Solvent-Laser Heated Floating Zone

Woodworth, A. A.↗

NASA NTRS2014

5.8kV SiC PiN Diode for Switching of High-Efficiency Inductive Pulsed Plasma Thruster Circuits

Inductive Pulsed Plasma Thruster (IPPT) pulse circuits, such as those needed to operate the Pulsed Inductive Thruster (PIT), are required to quickly switch capacitor banks operating at a period of μs while conducting current at levels on the order of at least 10 kA. [1,2] For all iterations of the PIT to date, spark gaps have been used to discharge the capacitor bank through an inductive coil. Recent availability of fast, high‐power solid state switching devices makes it possible to consider the use of semiconductor switches in modern IPPTs. In addition, novel pre‐ionization schemes have led to a reduction in discharge energy per pulse for electric thrusters of this type, relaxing the switching requirements for these thrusters. [3,4] Solid state switches offer the advantage of greater controllability and reliability, as well as decreased drive circuit dimensions and mass relative to spark gap switches. The use of solid state devices such as Integrated Gate Bipolar Transistors (IGBTs), Gate Turn‐off Thyristors (GTOs) and Silicon‐Controlled Rectifiers (SCRs) often involves the use of power diodes. These semiconductor devices may be connected antiparallel to the switch for protection from reverse current, or used to reduce power loss in a circuit by clamping off current ringing. In each case, higher circuit efficiency may be achieved by using a diode that is able to transition, or 'switch,' from the forward conducting state ('on' state) to the reverse blocking state ('off' state) in the shortest amount of time, thereby minimizing current ringing and switching losses. Silicon Carbide (SiC) PiN diodes offer significant advantages to conventional fast‐switching Silicon (Si) diodes for high power and fast switching applications. A wider band gap results in a breakdown voltage 10 times that of Si, so that a SiC device may have a thinner drift region for a given blocking voltage. [5] This leads to smaller, lighter devices for high voltage applications, as well as reduced forward conduction losses, faster reverse recovery time (faster turn‐off), and lower‐magnitude reverse recovery current. In addition, SiC devices have lower leakage current as compared to their Si counterparts, and a high thermal conductivity, potentially allowing the former to operate at higher temperatures with a smaller, lighter heatsink (or no heatsink at all).

Toftul, Alexandra↗

NASA NTRS2014

Demonstration of SiC Pressure Sensors at 750 C

We report the first demonstration of MEMS-based 4H-SiC piezoresistive pressure sensors tested at 750 C and in the process confirmed the existence of strain sensitivity recovery with increasing temperature above 400 C, eventually achieving near or up to 100% of the room temperature values at 750 C. This strain sensitivity recovery phenomenon in 4H-SiC is uncharacteristic of the well-known monotonic decrease in strain sensitivity with increasing temperature in silicon piezoresistors. For the three sensors tested, the room temperature full-scale output (FSO) at 200 psig ranged between 29 and 36 mV. Although the FSO at 400 C dropped by about 60%, full recovery was achieved at 750 C. This result will allow the operation of SiC pressure sensors at higher temperatures, thereby permitting deeper insertion into the engine combustion chamber to improve the accurate quantification of combustor dynamics.

Semiconductor↗

NASA NTRS2004

Atomic Force Microscope Observation of Growth and Defects on As-Grown (111) 3C-SiC Mesa Surfaces

This paper presents experimental atomic force microscope (AFM) observations of the surface morphology of as-grown (111) silicon-face 3C-SiC mesa heterofilms. Wide variations in 3C surface step structure are observed as a function of film growth conditions and film defect content. The vast majority of as-grown 3C-SiC surfaces consisted of trains of single bilayer height (0.25 nm) steps. Macrostep formation (i.e., step-bunching) was rarely observed, and then only on mesa heterofilms with extended crystal defects. As supersaturation is lowered by decreasing precursor concentration, terrace nucleation on the top (111) surface becomes suppressed, sometimes enabling the formation of thin 3C-SiC film surfaces completely free of steps. For thicker films, propagation of steps inward from mesa edges is sometimes observed, suggesting that enlarging 3C mesa sidewall facets begin to play an increasingly important role in film growth. The AFM observation of stacking faults (SF's) and 0.25 nm Burgers vector screw component growth spirals on the as-grown surface of defective 3C films is reported.

Neudeck, Philip G.↗

NASA NTRS2016

Stellar Origins of C-13 and N-15-Enriched Presolar SiC Grains

Extreme excesses of 13 C ( C (12 C/ 13 C<10) and 15 N ( N (14 N/ 15 N< 20) in rare presolar SiC 20) in rare presolar SiClar SiC grains have been considered diagnostic of an origin in classical novae [1], though an origin in core-collapse supernovae (CCSNe) has also been proposed [2]. We report multi-element isotopic data for 19 13 C- and 15 N-enriched presolar SiC grains(12 C/13 C<16 and 14 N/ 15 N<~150) from an acid resistant residue of the Murchison meteorite. These grains are enriched in 13 C and15 N, but with quite diverse Si isotopic signatures. Four grains with isotopic signatures. Four grains with isotopic signatures. Four grains with isotopic signatures. Four grains with isotopic signatures.

Liu, Nan↗

NASA NTRS2017

High Temperature Characteristics of Pt/TaSi2/Pt/W and Pt/Ti/W Diffusion Barrier Systems for Ohmic Contacts to 4H-SiC

The degradation of ohmic contacts to 4H-SiC pressure sensors over time at high temperature is primarily due to two failure mechanisms: migrating bond pad Au and atmospheric O toward the ohmic contact SiC interface and the inter-metallic mixing between diffusion barrier systems (DBS) and the underlying ohmic contact metallization. We investigated the effectiveness of Pt/TaSi2/Pt/W (DBS-A) and Pt/Ti/W (DBS-B) in preventing Au and O diffusion through the underlying binary Ti/W or alloyed W50:Ni50 ohmic contacts to 4H-SiC and the DBS ohmic contact intermixing at temperature up to 700 C.

Platinum↗

NASA NTRS2018

Importance of Measuring SiC Fiber Diameter Prior to Conducting Fiber Stress Rupture / Creep Tests?

A very significant amount of SiC fiber creep / stress rupture data has been generated and reported in the past by various researchers. Due to the difficulty of measuring fiber diameter and the amount of time required to make accurate measurements, researchers have quite often used an accepted average diameter value (which is fiber type-dependent) when determining the load that will be applied to a fiber to generate a specific stress during testing. Of course, this approach has less of an effect on data scatter when the individual fibers in a tow have very similar diameters (minimal fiber-to-fiber variation in diameter). NASA GRC has begun using a laser fiber diameter measurement system, and we are considering eventually characterizing each SiC fiber prior to testing in creep/stressed oxidation. The laser system will be described in this presentation, as well as examples of fiber diameter data obtained in the past at AFRL. We are currently discussing the merits of using an average diameter in testing/data analysis vs. using a measured or "known" diameter. Information about our current intermediate temperature SiC fiber stress rupture testing will also be provided.

ceramic matrix composites↗