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NASA NTRS1989

Oxidation of chemically-vapor-deposited silicon nitride and single-crystal silicon

The present 1000 C and 1300 C oxidation tests on 111-oriented single-crystal Si and dense CVD Si3N4 notes the oxidation rates of the latter in wet O2, dry O2, wet inert gas, and steam atmosphere conditions to be several orders of magnitude lower than the rates for the former in identical atmospheric conditions. Although the parabolic rate constant for Si increased linearly as the water vapor pressure increased, the parabolic rate constant for Si3N4 exhibited a nonlinear dependency on water vapor pressure in the presence of O2. NO and NH3 formation at the reaction interface of Si3N4, and the counterpermeation of these reaction products, are noted to dominate reaction kinetics.

Choi, Doo J.↗

DOE OSTI2023

Photophysics of Intrinsic Single‐Photon Emitters in Silicon Nitride at Low Temperatures

A robust process for fabricating intrinsic single-photon emitters in silicon nitride is recently established. These emitters show promise for quantum applications due to room-temperature operation and monolithic integration with technologically mature silicon nitride photonics platforms. Here, the fundamental photophysical properties of these emitters are probed through measurements of optical transition wavelengths, linewidths, and photon antibunching as a function of temperature from 4.2 to 300 K. Important insight into the potential for lifetime-limited linewidths is provided through measurements of inhomogeneous and temperature-dependent broadening of the zero-phonon lines. At 4.2 K, spectral diffusion is found to be the main broadening mechanism, while spectroscopy time series reveal zero-phonon lines with instrument-limited linewidths.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1983

Deposition of silicon nitride from SiCl4 and NH3 in a low pressure RF plasma

Silicon nitride coatings were deposited in a low-pressure (1-10 Torr) RF plasma from SiCl4 and NH3 in the presence of argon onto stainless martensitic steel grounded and floating substrates at 300 C and 440 C respectively. The heating of the substrates depends mainly on the position and the induced RF power. The coatings were identified as silicon nitride by X-ray investigation and were found to contain chlorine by energy-dispersive analysis of X-rays. The growth rate, the microhardness and the chlorine concentration of the coatings were determined as a function of the total gas pressure, the RF power input and the NH3-to-SiCl4 ratio. It was observed that the coatings on the floating substrates have higher deposition rates and are of superior quality.

Ron, Y.↗

NASA NTRS1980

Effect of W and WC on the oxidation resistance of yttria-doped silicon nitride

The effect of tungsten and tungsten carbide contamination on the oxidation and cracking in air of yttria-doped silicon nitride ceramics is investigated. Silicon nitride powder containing 8 wt % Y2O3 was doped with 2 wt % W, 4 wt % W, 2 wt % WC or left undoped, and sintered in order to simulate contamination during milling, and specimens were exposed in air to 500, 750 and 1350 C for various lengths of time. Scanning electron and optical microscopy and X-ray diffraction of the specimens in the as-sintered state reveals that the addition of W or WC does not affect the phase relationships in the system, composed of alpha and beta Si3N4, melilite and an amorphous phase. Catastrophic oxidation is observed at 750 C in specimens containing 2 and 4 wt % W, accompanied by the disappearance of alpha Si3N4 and melilite from the structure. At 1350 C, the formation of a protective glassy oxide layer was observed on all specimens without catastrophic oxidation, and it is found that pre-oxidation at 1350 C also improved the oxidation resistance at 750 C of bars doped with 4 wt % W. It is suggested that tungsten contamination from WC grinding balls may be the major cause of the intermediate-temperature cracking and instability frequently observed in Si3N4-8Y2O3.

Schuon, S.↗

NASA NTRS1973

High gas velocity burner tests on silicon carbide and silicon nitride at 1200 C

Specimens of silicon carbide and silicon nitride were exposed to a Mach one gas velocity burner simulating a turbine engine environment. Cyclic tests up to 100 hour duration were conducted at specimen temperatures of 1200 C. A specimen geometry was used that develops thermal stresses during thermal cycling in a manner similar to blades and vanes of a gas turbine engine. Materials were compared on a basis of weight change, dimensional reductions, metallography, fluorescent penetrant inspection, X-ray diffraction analyses, failure mode, and general appearance. One hot pressed SiC, one reaction sintered SiC, and three hot pressed Si3N4 specimens survived the program goal of 100 one-hour cycle exposures. Of the materials that failed to meet the program goal, thermal fatigue was identified as the exclusive failure mode.

Sanders, W. A.↗

NASA NTRS1985

Reliability of two sintered silicon nitride materials

Two types of sintered silicon nitride were evaluated in terms of reliability: an experimental high pressure nitrogen sintered material and a commercial material. The results show wide variations in strength for both materials. The Weibull moduli were 5.5, 8.9, and 11 for the experimental material at room temperature, 1200, and 1370 C, respectively. The commercial material showed Weibull moduli of 9.0, 8.6, and 8.9 at these respective temperatures. No correlation between strength and flaw size was noted for the experimental material. The applicability of the Weibull and Griffith theories to processing defects on the order of 100 microns or less in size are discussed.

Mieskowski, D. M.↗

NASA NTRS2008

Evaluation of Silicon Nitride for Brayton Turbine Wheel Application

Silicon nitride (Si3N4) is being evaluated as a risk-reduction alternative for a Jupiter Icy Moons Orbiter Brayton turbine wheel in the event that the Prometheus program design requirements exceed the creep strength of the baseline metallic superalloys. Five Si3N4 ceramics, each processed by a different method, were screened based on the Weibull distribution of bend strength at 1700 F (927 C). Three of the Si3N4 ceramics, Honeywell AS800, Kyocera SN282, and Saint-Gobain NT154, had bend strengths in excess of 87 ksi (600 MPa) at 1700 F (927 C). These were chosen for further assessment and consideration for future subcomponent and component fabrication and testing.

Freedman, Marc R.↗

NASA NTRS1993

Quantitative Mapping of Pore Fraction Variations in Silicon Nitride Using an Ultrasonic Contact Scan Technique

An ultrasonic scan procedure using the pulse-echo contact configuration was employed to obtain maps of pore fraction variations in sintered silicon nitride samples in terms of ultrasonic material properties. Ultrasonic velocity, attenuation coefficient, and reflection coefficient images were obtained simultaneously over a broad band of frequencies (e.g., 30 to 110 MHz) by using spectroscopic analysis. Liquid and membrane (dry) coupling techniques and longitudinal and shear-wave energies were used. The major results include the following: Ultrasonic velocity (longitudinal and shear wave) images revealed and correlated with the extent of average through-thickness pore fraction variations in the silicon nitride disks. Attenuation coefficient images revealed pore fraction nonuniformity due to the scattering that occurred at boundaries between regions of high and low pore fraction. Velocity and attenuation coefficient images were each nearly identical for machined and polished disks, making the method readily applicable to machined materials. Velocity images were similar for wet and membrane coupling. Maps of apparent Poisson's ratio constructed from longitudinal and shear-wave velocities quantified Poisson's ratio variations across a silicon nitride disk. Thermal wave images of a disk indicated transient thermal behavior variations that correlated with observed variations in pore fraction and velocity and attenuation coefficients.

Roth, Don J.↗

NASA NTRS1982

Fabrication of turbine components and properties of sintered silicon nitride

This paper presents a status report on the injection molding of sinterable silicon nitride at GTE Laboratories. The effort involves fabrication of single axial turbine blades and monolithic radial turbine rotors. The injection molding process is reviewed and the fabrication of the turbine components discussed. Oxidation resistance and strength results of current injection molded sintered silicon nitride as well as dimensional checks on sintered turbine blades demonstrate that this material is a viable candidate for high temperature structural applications.

Neil, J. T.↗

NASA NTRS1987

Devitrification and delayed crazing of SiO2 on single-crystal silicon and chemically vapor-deposited silicon nitride

The linear growth rate of cristobalite was measured in thin SiO2 films on silicon and chemically vapor-deposited silicon nitride. The presence of trace impurities from alumina furnace tubes greatly increased the crystal growth rate. Under clean conditions, the growth rate was still 1 order-of-magnitude greater than that for internally nucleated crystals in bulk silica. Crystallized films cracked and lifted from the surface after exposure to atmospheric water vapor. The crystallization and subsequent crazing and lifting of protective SiO2 films on silicon nitride should be considered in long-term applications.

Choi, Doo Jin↗

NASA NTRS1996

"Inert" Strengths of Silicon Nitride Ceramics at Elevated Temperatures

An attempt to determine high temperature "inert" strengths of several silicon nitride ceramics was made by using dynamic fatigue testing at the very high stressing rate of 2 x 106 MPa/min. The fatigue strengths of all the silicon nitride materials exhibited a well-defined convergence to the corresponding room-temperature inert strengths as stressing rate was increased. The result showed that the high temperature Inert" strength of a ceramic material can be obtained by using sufficiently high stressing rates (greater or = 2 x 10(exp 6) MPa/min) at which fatigue strength converges to a specific value. The specific value can be close to the room-temperature strength of the material.

Choi, Sung R.↗

NASA NTRS1989

Plasma deposited silicon nitride for indium phosphide encapsulation

The composition and the annealing characteristics of plasma-deposited silicon-nitride encapsulating films on the ion-implanted InP substrates were investigated, using two different substrate-cleaning procedures (organic solvents and HF or HIO3 solutions) prior to encapsulation. The effect of plasma deposition of silicon nitride on the InP substrates was assessed through the current-voltage characteristics of Schottky diodes. Results of XPS analyses showed that the cleaning procedure that employed HF solution left less oxygen on the InP surface than the procedure involving HIO3. No chemical interaction between the film and the substrate was observed before or after annealing.

Valco, G. J.↗

NASA NTRS2005

Effect of Silicon Nitride Balls and Rollers on Rolling Bearing Life

Three decades have passed since the introduction of silicon nitride rollers and balls into conventional rolling-element bearings. For a given applied load, the contact (Hertz) stress in a hybrid bearing will be higher than an all-steel rolling-element bearing. The silicon nitride rolling-element life as well as the lives of the steel races were used to determine the resultant bearing life of both hybrid and all-steel bearings. Life factors were determined and reported for hybrid bearings. Under nominal operating speeds, the resultant calculated lives of the deep-groove, angular-contact, and cylindrical roller hybrid bearings with races made of post-1960 bearing steel increased by factors of 3.7, 3.2, and 5.5, respectively, from those calculated using the Lundberg-Palmgren equations. An all-steel bearing under the same load will have a longer life than the equivalent hybrid bearing under the same conditions. Under these conditions, hybrid bearings are predicted to have a lower fatigue life than all-steel bearings by 58 percent for deep-groove bearings, 41 percent for angular-contact bearings, and 28 percent for cylindrical roller bearings.

Zaretsky, Erwin V.↗

NASA NTRS1984

Crystallization of the glassy phase of grain boundaries in silicon nitride

Three types of hot-pressed silicon nitride specimens (containing 5wt% Y2O3 and 2wt% Al2O3 additives) which were subjected to different temperature heat treatments were studied by X-ray diffraction, X-ray microanalysis and high resolution electron microscopy. The results indicated that there were phase changes in the grain boundaries after heat treatment and the glassy phase at the grain boundaries was crystallized by heat treatment.

Jefferson, D. A.↗

NASA NTRS1987

Strength characterization of yttria/alumina-doped sintered silicon nitride

The flexural strength of yttria/alumina-doped sintered silicon nitride (Ford Material-RM 20) was measured as a function of temperature (20 to 1400 deg C), applied stress and time. Flexural stress rupture testing at 800 and 1000 deg C indicated that the material can sustain 344 MPa and 276 MPa, respectively, without failure, for a limited time (less than or equal to 100 h). The RM 20 material was susceptible to both oxidation and early stages of creep deformation at temperatures above 1000 deg C and displayed extensive creep deformation and degradation in strength above 1300 deg C.

Govila, R. K.↗

NASA NTRS1990

High-temperature tensile properties of fiber reinforced reaction bonded silicon nitride

Measurements of tensile properties of unidirectional silicon carbide fiber-reinforced reaction-bonded silicon nitride (SiC/RBSN) composite specimens were carried out in air at 25, 1300, and 1500 C, using a new testing technique and a specially designed gripping system that minimizes bending moment and assures that failure always occurred in the gage section. The material was found to display metallike stress-strain behavior at all temperatures tested, and a noncatastrophic failure beyond the matrix fracture. The tensile properties were found to be temperature dependent, with the values of the ultimate tensile strength decreasing with temperature, from 543 MPa at 25 C to 169 at 1500 C.

Jablonski, David A.↗

NASA NTRS2002

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

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

Fox, Dennis S.↗

DOE OSTI2022

Determination of the nonlinear thermo-optic coefficient of silicon nitride and oxide using an effective index method

There is little literature characterizing the temperature-dependent thermo-optic coefficient (TOC) for low pressure chemical vapor deposition (LPCVD) silicon nitride or plasma enhanced chemical vapor deposition (PECVD) silicon dioxide at temperatures above 300 K. In this study, we characterize these material TOC’s from approximately 300-460 K, yielding values of (2.51 ± 0.08) · 10 −5 K −1 for silicon nitride and (5.67 ± 0.53) · 10 −6 K −1 for silicon oxide at room temperature (300 K). We use a simplified experimental setup and apply an analytical technique to account for thermal expansion during the extraction process. We also show that the waveguide geometry and method used to determine the resonant wavelength have a substantial impact on the precision of our results, a fact which can be used to improve the precision of numerous ring resonator index sensing experiments.

36 MATERIALS SCIENCE↗