Sintered silicon nitride workpiece
A description is given of a sintering method for silicon nitride. A detailed explanation of the invention is presented. Four procedures for the sintering process are described.
Shinohara, N.↗
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Preparation of silicon carbide-silicon nitride fibers by the pyrolysis of polycarbosilazane precursors
The development of silicon carbide-silicon nitride fibers (SiC-Si3N4) by the pyrolysis of polycarbosilazane precursors is reviewed. Precursor resin, which was prepared by heating tris(N-methylamino)methylsilane or tris(N-methylamino)phenylsilane to about 520 C, was drawn into fibers from the melt and then made unmeltable by humidity conditioning at 100 C and 95 percent relative humidity. The humidity treated precursor fibers were pyrolyzed to ceramic fibers with good mechanical properties and electrical resistivity. For example, SiC-Si3N4 fibers derived from tris(N-methylamino)methylsilane had a tensile rupture modulus of 29 million psi and electrical resistivity of 6.9 x ten to the 8th power omega-cm, which is ten to the twelfth power times greater than that obtained for graphite fibers.
Penn, B. G.↗
Dynamic and static fatigue behavior of sintered silicon nitrides
The dynamic and static fatigue behavior of Kyocera SN220M sintered silicon nitride at 1000 C was studied. Fractographic analysis of the material failing in dynamic fatigue revealed the presence of slow crack growth (SCG) at stressing rates below 41 MPa/min. Under conditions of static fatigue this material also displayed SCG at stresses below 345 MPa. SCG appears to be controlled by microcracking of the grain boundaries. The crack velocity exponent (n) determined from both dynamic and static fatigue tests ranged from 11 to 16.
Chang, J.↗
Improved silicon nitride for advanced heat engines
The technology base required to fabricate silicon nitride components with the strength, reliability, and reproducibility necessary for actual heat engine applications is presented. Task 2 was set up to develop test bars with high Weibull slope and greater high temperature strength, and to conduct an initial net shape component fabrication evaluation. Screening experiments were performed in Task 7 on advanced materials and processing for input to Task 2. The technical efforts performed in the second year of a 5-yr program are covered. The first iteration of Task 2 was completed as planned. Two half-replicated, fractional factorial (2 sup 5), statistically designed matrix experiments were conducted. These experiments have identified Denka 9FW Si3N4 as an alternate raw material to GTE SN502 Si3N4 for subsequent process evaluation. A detailed statistical analysis was conducted to correlate processing conditions with as-processed test bar properties. One processing condition produced a material with a 97 ksi average room temperature MOR (100 percent of goal) with 13.2 Weibull slope (83 percent of goal); another condition produced 86 ksi (6 percent over baseline) room temperature strength with a Weibull slope of 20 (125 percent of goal).
Yeh, Hun C.↗
Radiation tolerant silicon nitride insulated gate field effect transistors
Metal-Insulated-Semiconductor Field Effect Transistor /MISFET/ device uses a silicon nitride passivation layer over a thin silicon oxide layer to enhance the radiation tolerance. It is useful in electronic systems exposed to space radiation environment or the effects of nuclear weapons.
Newman, P. A.↗
Silicon Nitride Plates for Turbine Blade Application: FEA and NDE Assessment
Engine manufacturers are continually attempting to improve the performance and the overall efficiency of internal combustion engines. The thermal efficiency is typically improved by raising the operating temperature of essential engine components in the combustion area. This reduces the heat loss to a cooling system and allows a greater portion of the heat to be used for propulsion. Further improvements can be achieved by diverting part of the air from the compressor, which would have been used in the combustor for combustion purposes, into the turbine components. Such a process is called active cooling. Increasing the operating temperature, decreasing the cooling air, or both can improve the efficiency of the engine. Furthermore, lightweight, strong, tough hightemperature materials are required to complement efficiency improvement for nextgeneration gas turbine engines that can operate with minimum cooling. Because of their low-density, high-temperature strength, and thermal conductivity, ceramics are being investigated as potential materials for replacing ordinary metals that are currently used for engine hot section components. Ceramic structures can withstand higher operating temperatures and other harsh environmental factors. In addition, their low densities relative to metals helps condense component mass (ref. 1). The objectives of this program at the NASA Glenn Research Center are to develop manufacturing technology, a thermal barrier coating/environmental barrier coating (TBC/EBC), and an analytical modeling capability to predict thermomechanical stresses, and to do minimal burner rig tests of silicon nitride (Si3N4) and SiC/SiC turbine nozzle vanes under simulated engine conditions. Furthermore, and in support of the latter objectives, an optimization exercise using finite element analysis and nondestructive evaluation (NDE) was carried out to characterize and evaluate silicon nitride plates with cooling channels.
Abdul-Aziz, Ali↗
Thermogravimetric analysis of silicon carbide-silicon nitride fibers at ambient to 1000 C in air
Thermogravimetric analysis of silicon carbide-silicon nitride fibers was carried out at ambient to 1000 C in air. The weight loss over this temperature range was negligible. In addition, the oxidative stability at high temperature for a short period of time was determined. Fibers heated at 1000 C in air for fifteen minutes showed negligible weight loss (i.e., less than 1 percent).
Daniels, J. G.↗
Development of a continuous spinning process for producing silicon carbide - silicon nitride precursor fibers
An apparatus was designed for the continuous production of silicon carbide - silicon nitride precursor fibers. The precursor polymer can be fiberized, crosslined and pyrolyzed. The product is a metallic black fiber with the composition of the type C sub x Si sub y n sub z. Little, other than the tensile strength and modulus of elasticity, is known of the physical properties.
Source record↗
Estimation of crack closure stresses for in situ toughened silicon nitride with 8 wt pct scandia
An 8-wt pct-scandia silicon nitride with an elongated grain structure was fabricated. The material exhibited high fracture toughness and a rising R-curve as measured by the indentation strength technique. The 'toughening' exponent m was found to be m about 0.1. The high fracture toughness and R-curve behavior was attributed mainly to bridging of the crack faces by the elongated grains. The crack closure (bridging) stress distribution in the wake region of the crack tip was estimated as a function of crack size from the R-curve data, with an arbitrarily assumed distribution function.
Choi, Sung R.↗
Reaction bonded silicon nitride prepared from wet attrition-milled silicon
Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 vol% hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high-strength specimens and both subsurface and surface flaws in low-strength specimens.
Herbell, T. P.↗
Reaction bonded silicon nitride prepared from wet attrition-milled silicon
Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 volume percent hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high strength specimens and both subsurface and surface flaws in low strength specimens.
Herball, T. P.↗
Role of the interfacial thermal barrier in the effective thermal diffusivity/conductivity of SiC-fiber-reinforced reaction-bonded silicon nitride
Experimental thermal diffusivity data transverse to the fiber direction for composites composed of a reaction bonded silicon nitride matrix reinforced with uniaxially aligned carbon-coated silicon carbide fibers indicate the existence of a significant thermal barrier at the matrix-fiber interface. Calculations of the interfacial thermal conductances indicate that at 300 C and 1-atm N2, more than 90 percent of the heat conduction across the interface occurs by gaseous conduction. Good agreement is obtained between thermal conductance values for the oxidized composite at 1 atm calculated from the thermal conductivity of the N2 gas and those inferred from the data for the effective composite thermal conductivity.
Bhatt, Hemanshu↗
Unraveling fundamental mechanisms of silicon nitride crystallization in microelectronics manufacturing
This research project investigates the fundamental mechanisms of silicon nitride (SiN) crystallization, aiming to enhance the understanding of this critical material in microelectronics manufacturing. Through a collaborative effort between Sandia National Laboratories, the University of Tennessee, and the University of Florida, we developed a comprehensive framework that integrates experimental techniques, atomistic modeling, meso-scale simulations, and an integrated multi-scale model to capture this physical phenomenon on multiple time and length scales . The project developed a new machine learning based atomistic potential and utilized advanced phase field modeling to capture the complexities of polycrystalline growth and the influence of mechanical stresses on crystallization dynamics. By employing a grain tracker algorithm, the meso-scale model effectively identified and tracked individual crystal grains, enabling the simulation of anisotropic growth behaviors reflective of SiN’s physical properties. The integration of atomistic simulations with meso-scale modeling created a powerful multi-scale framework that validated atomistic inputs and enhanced predictive accuracy for crystallization dynamics at larger scales, validated experimentally. This adaptable modeling capability not only accelerates development times by informing manufacturing processes but also serves as a valuable starting point for understanding crystallization physics in similar materials. The insights gained from this research unlock new opportunities for the development of advanced materials tailored for future microelectronics and photonics applications. Overall, this project represents a significant advancement in understanding of fundamental physics of SiN and establishes a foundation for future research in material science, bridging the gap between atomic-level phenomena and macroscopic material behaviors for practical applications.
36 MATERIALS SCIENCE↗
Preparation of silicon carbide-silicon nitride fibers by the pyrolysis of polycarbosilazane precursors - A review
The development of silicon carbide-silicon nitride fibers (SiC-Si3N4) by the pyrolysis of polycarbosilazane precursors is reviewed. Precursor resin, which was prepared by heating tris(N-methylamino)methylsilane or tris(N-methylamino)phenylsilane to about 520 C, was drawn into fibers from the melt and then made unmeltable by humidity conditioning at 100 C and 95 percent relative humidity. The humidity treated precursor fibers were pyrolyzed to ceramic fibers with good mechanical properties and electrical resistivity. For example, SiC-Si3N4 fibers derived from tris(N-methylamino)methylsilane had a tensile rupture modulus of 29 million psi and electrical resistivity of 6.9 x ten to the 8th power omega-cm, which is ten to the twelfth power times greater than that obtained for graphite fibers.
Penn, B. G.↗
Dynamic fatigue property of silicon carbide whisker-reinforced silicon nitride
The dynamic fatigue behavior of 30 vol pct SiC whisker-reinforced silicon nitride was determined in flexure as a function of temperature from 1100 to 1300 C in an air environment. The fatigue susceptibility parameter n decreased from 88.1 to 20.1 with increasing temperature from 1100 to 1300 C. A transition in the dynamic fatigue curve occurred at a lowest stressing rate of 2 MPa/min at a temperature of 1300 C, resulting in a considerably lower value of n = 5.8. This transition was primarily due to creep that was enhanced by a combination of high temperature and very slow deformation rate. The fatigue resistance of natural flaws at 1100 C was found to be greater than that of artificial flaws produced by indentation.
Choi, Sung R.↗
Role of interfacial carbon layer in the thermal diffusivity/conductivity of silicon carbide fiber-reinforced reaction-bonded silicon nitride matrix composites
Experiments were carried out on samples of reaction-bonded silicon nitride uniaxially reinforced by SiC monofilaments with and without a 3-micron-thick carbon-rich coating. It is found that a combination of a carbon coatings on the fibers and an interfacial gap due to the thermal expansion mismatch in the composite can significantly (by a factor of 2) lower the effective thermal diffusivity in the direction transverse to the fiber. At atmospheric pressure, gaseous conduction across the interfacial gap makes a significant contribution to the heat transfer across the interface, indicated by significantly lower values of the effective thermal diffusivity under vacuum than in nitrogen or helium at atmospheric pressure.
Bhatt, Hemanshu↗
Oxidation Protection of Porous Reaction-Bonded Silicon Nitride
Oxidation kinetics of both as-fabricated and coated reaction-bonded silicon nitride (RBSN) were studied at 900 and 1000 C with thermogravimetry. Uncoated RBSN exhibited internal oxidation and parabolic kinetics. An amorphous Si-C-O coating provided the greatest degree of protection to oxygen, with a small linear weight loss observed. Linear weight gains were measured on samples with an amorphous Si-N-C coating. Chemically vapor deposited (CVD) Si3N4 coated RBSN exhibited parabolic kinetics, and the coating cracked severely. A continuous-SiC-fiber-reinforced RBSN composite was also coated with the Si-C-O material, but no substantial oxidation protection was observed.
Fox, D. S.↗
Creep of a Silicon Nitride Under Various Specimen/Loading Configurations
Extensive creep testing of a hot-pressed silicon nitride (NC132) was performed at 1300 C in air using five different specimen/loading configurations, including pure tension, pure compression, four-point uniaxial flexure, ball-on-ring biaxial flexure, and ring-on-ring biaxial flexure. Nominal creep strain and its rate for a given nominal applied stress were greatest in tension, least in compression, and intermediate in uniaxial and biaxial flexure. Except for the case of compressive loading, nominal creep strain generally decreased with time, resulting in less-defined steady-state condition. Of the four different creep formulations - power-law, hyperbolic sine, step, redistribution models - the conventional power-law model still provides the most convenient and reasonable means to estimate simple, quantitative creep parameters of the material. Predictions of creep deformation for the case of multiaxial stress state (biaxial flexure) were made based on pure tension and compression creep data by using the design code CARES/Creep.
Choi, Sung R.↗