Conduction properties of pyrolytic silicon nitride films.
Conduction properties of silicon nitride thin films noting temperature dependence and thermal emission
Taylor, H. L.↗
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Improved silicon nitride for advanced heat engines
Silicon nitride is a high temperature material currently under consideration for heat engine and other applications. The objective is to improve the net shape fabrication technology of Si3N4 by injection molding. This is to be accomplished by optimizing the process through a series of statistically designed matrix experiments. To provide input to the matrix experiments, a wide range of alternate materials and processing parameters was investigated throughout the whole program. The improvement in the processing is to be demonstrated by a 20 percent increase in strength and a 100 percent increase in the Weibull modulus over that of the baseline material. A full characterization of the baseline process was completed. Material properties were found to be highly dependent on each step of the process. Several important parameters identified thus far are the starting raw materials, sinter/hot isostatic pressing cycle, powder bed, mixing methods, and sintering aid levels.
Yeh, H. C.↗
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.↗
Foreign Object Damage of Two Gas-Turbine Grade Silicon Nitrides in a Thin Disk Configuration
Foreign object damage (FOD) behavior of two commercial gas-turbine grade silicon nitrides, AS800 and SN282, was determined at ambient temperature through post-impact strength testing for thin disks impacted by steel-ball projectiles with a diameter of 1.59 mm in a velocity range from 115 to 440 m/s. AS800 silicon nitride exhibited a greater FOD resistance than SN282, primarily due to its greater value of fracture toughness (K(sub IC)). The critical impact velocity in which the corresponding post-impact strength yielded the lowest value was V(sub c) approx. 440 and 300 m/s for AS800 and SN282, respectively. A unique lower-strength regime was typified for both silicon nitrides depending on impact velocity, attributed to significant radial cracking. The damages generated by projectile impact were typically in the forms of ring, radial, and cone cracks with their severity and combination being dependent on impact velocity. Unlike thick (3 mm) flexure bar specimens used in the previous studies, thin (2 mm) disk target specimens exhibited a unique backside radial cracking occurring on the reverse side just beneath the impact sites at and above impact velocity of 160 and 220 m/s for SN282 and AS800, respectively.
Choi, Sung R.↗
Development of silicon nitride of improved toughness
The application of reaction sintered Si2N4 energy absorbing surface layers to hot-pressed Si3N4 was investigated. The surface layer was formed by in-place nitridation of silicon powder. It was found that reaction sintered Si3N4 layers of 1 mm thickness, fabricated from either -100, +200, -200, or -325 mesh Si powder and nitrided in 96% N2/4% H2 so that approximately 20-25 vol % unnitrided Si remained in the layer, resulted in a sevenfold increase in ballistic impact resistance of a 0.64 cm thick hot-pressed SI3N4 substrate from RT 1370 C. Both NC-132 SI3N4, with MgO additive, and NCX-34 Si3N4, with Y2O3 additive, were evaluated as substrate material. The finer grain size -200 and -325 mesh nitrided Si layers were for their smoothness and relatively high density. It was found that nitriding in N2/H2 mixtures, rather than pure N2, resulted in a microstructure that did not substantially degrade the strength of the hot-pressed Si3N4 substrate. Thermal cycling tests on the RSSN/HPSN combinations from 200 C to 1370 C for 75 cycles in air did not degrade the impact resistance nor the interfacial bonding, although a large amount of internal silica formation occurred within the RSSN layer. Mach 0.8, 5 hr, hot gas erosion tests showed no surface recession of RSSN layers at 1200 C and slight surface recession at 1370 C.
Brennan, J. J.↗
Foreign Object Damage in Disks of Two Gas-turbine-grade Silicon Nitrides by Steel Ball Projectiles at Ambient Temperature
Foreign object damage (FOD) behavior of two commercial gas-turbine-grade silicon nitrides, AS800 and SN282, was determined at ambient temperature through postimpact strength testing of disks impacted by steel ball projectiles with a diameter of 1.59 mm in a velocity range from 115 to 440 m/s. AS800 silicon nitride exhibited a greater FOD resistance than SN282, primarily due to its greater value of fracture toughness (k(sub Ic)). The critical impact velocity V(sub c) for which the corresponding postimpact strength was the lowest was V(sub c) approximately equal to 440 and 300 m/s AS800 and SN282, respectively. A unique lower strength regime was typified for both silicon nitrides depending on impact velocity and was attributed to significant radial cracking. The damage generated by projectile impact was typically in the form of ring, radial, and cone cracks with their severity and combination being dependent on impact velocity. Unlike the thick (4 millimeters) flexure bar specimens used in our previous studies, the thin (2 millimeter) disk target specimen exhibited a unique back-side radial cracking on the reverse side just beneath the impact sites at and above impact velocities of 160 meters per second for SN282 and 220 meters per second AS800.
Choi, Sung R.↗
Process for the production of metal nitride sintered bodies and resultant silicon nitride and aluminum nitride sintered bodies
A process for the manufacture of metal nitride sintered bodies, in particular, a process in which a mixture of metal nitrite powders is shaped and heated together with a binding agent is described. Of the metal nitrides Si3N4 and AIN were used especially frequently because of their excellent properties at high temperatures. The goal is to produce a process for metal nitride sintered bodies with high strength, high corrosion resistance, thermal shock resistance, thermal shock resistance, and avoidance of previously known faults.
Yajima, S.↗
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.↗
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.↗
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.↗
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.↗
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.↗
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.↗
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.↗
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.↗
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↗
"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.↗
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.↗