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NASA NTRS2009

Joining and Integration of Silicon Nitride Ceramics for Aerospace and Energy Systems

Light-weight, creep-resistant silicon nitride ceramics possess excellent high-temperature strength and are projected to significantly raise engine efficiency and performance when used as turbine components in the next-generation turbo-shaft engines without the extensive cooling that is needed for metallic parts. One key aspect of Si3N4 utilization in such applications is its joining response to diverse materials. In an ongoing research program, the joining and integration of Si3N4 ceramics with metallic, ceramic, and composite materials using braze interlayers with the liquidus temperature in the range 750-1240C is being explored. In this paper, the self-joining behavior of Kyocera Si3N4 and St. Gobain Si3N4 using a ductile Cu-based active braze (Cu-ABA) containing Ti will be presented. Joint microstructure, composition, hardness, and strength as revealed by optical microscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Knoop microhardness test, and offset compression shear test will be presented. Additionally, microstructure, composition, and joint strength of Si3N4/Inconel 625 joints made using Cu-ABA, will be presented. The results will be discussed with reference to the role of chemical reactions, wetting behavior, and residual stresses in joints.

Singh, M.↗

DOE OSTI2023

Ultra‐Low‐Loss Silicon Nitride Photonics Based on Deposited Films Compatible with Foundries

Abstract The fabrication processes of silicon nitride (Si 3 N 4 ) photonic devices used in foundries require low temperature deposition, which typically leads to high propagation losses. Here, it is shown that propagation loss as low as 0.42 dB cm −1 can be achieved using foundry compatible processes by solely reducing waveguide surface roughness. By postprocessing the fabricated devices using rapid thermal anneal (RTA) and furnace anneal, propagation losses down to 0.28 dB cm −1 and 0.06 dB cm −1 , respectively, are achieved. These low losses are comparable to the conventional devices using high temperature, high‐stress LPCVD films. The dispersion of the devices is also tuned, and it is proved that these devices can be used for linear and nonlinear applications. Low threshold parametric oscillation, broadband frequency combs, and narrow‐linewidth laser are demonstrated. This work demonstrates the feasibility of scalable photonic systems based on foundries.

Ji, Xingchen↗

NASA NTRS1989

Oxidation effects on the mechanical properties of SiC fiber-reinforced reaction-bonded silicon nitride matrix composites

The room temperature mechanical properties of SiC fiber reinforced reaction bonded silicon nitride composites were measured after 100 hrs exposure at temperatures to 1400 C in nitrogen and oxygen environments. The composites consisted of approx. 30 vol percent uniaxially aligned 142 micron diameter SiC fibers in a reaction bonded Si3N4 matrix. The results indicate that composites heat treated in a nitrogen environment at temperatures to 1400 C showed deformation and fracture behavior equivalent to that of the as-fabricated composites. Also, the composites heat treated in an oxidizing environment beyond 400 C yielded significantly lower tensile strength values. Specifically in the temperature range from 600 to 1000 C, composites retained approx. 40 percent of their as-fabricated strength, and those heat treated in the temperatures from 1200 to 1400 C retained 70 percent. Nonetheless, for all oxygen heat treatment conditions, composite specimens displayed strain capability beyond the matrix fracture stress; a typical behavior of a tough composite.

Bhatt, Ramakrishna T.↗

NASA NTRS1994

Crack-Growth Resistance of in Situ-Toughened Silicon Nitride

The fracture toughness of a commercial, hot-pressed, in situ-toughened silicon nitride with an elongated grain structure is determined by four different testing methods. The fracture toughness is found to be 5.76 +/- 0.27, 8.48 +/- 0.50, 10.16 +/- 0.66, and 10.68 +/- 0.39 MPa x m(exp 1/2), respectively, by indentation crack size measurement, indentation strength, single-edge-precracked-beam, and chevron-notched-beam methods. The discrepancy in fracture toughness between the testing methods is related to R-curve behavior, as measured using the indentation strength technique. These results indicate that there is no unique fracture toughness value and that a fracture toughness testing method with appropriate qualifiers is needed for rising R-curve materials. Therefore, care should be taken in interpreting and utilizing fracture toughness values evaluated from different testing methods if a material exhibits a rising R-curve. Complete characterization of the R-curve may be a prerequisite.

Salem, Jonathan A.↗

NASA NTRS1985

Fracture of yttria-doped, sintered reaction-bonded silicon nitride

Flexural strength of an yttria-doped, slip-cast, sintered reaction-bonded silicon nitride was evaluated as a function of temperature (20 to 1400 C in air), applied stress, and time. Static oxidation at 700 to 1400 C was investigated in detail; in tests at 1000 C in air, the material showed anomalous weight gain. Flexural stress-rupture testing at 800 to 1200 C in air indicated that the material is susceptible to stress-enhanced oxidation and early failure. Fractographic evidence for time-dependent and -independent failures is presented.

Govila, R. K.↗

NASA NTRS1987

Fracture of flash oxidized, yttria-doped sintered reaction-bonded silicon nitride

The oxidation behavior of a slip cast, yttria-doped, sintered reaction-bonded silicon nitride after 'flash oxidation' was investigated. It was found that both the static oxidation resistance and flexural stress rupture life (creep deformation) were improved at 1000 C in air compared to those of the same material without flash oxidation. Stress rupture data at high temperatures (1000 to 1200 C) are presented to indicate applied stress levels for oxidation-dependent and independent failures.

Govila, R. K.↗

NASA NTRS1988

Laminate behavior for SiC fiber-reinforced reaction-bonded silicon nitride matrix composites

The room temperature mechanical properties of SiC fiber reinforced reaction-bonded silicon nitride matrix composite laminates (SiC/RBSN) have been measured. The laminates contained approx 30 volume fraction of aligned 142-micron diameter SiC fiber in a porous RBSN matrix. Three types of laminate studied were unidirectional: (1) (0) sub 8, (2) (10) sub 8, and (3) (45) sub 8, and (90) sub 8; cross plied laminates (0 sub 2/90 sub 2); and angle plied laminates: (+45 sub 2/-45 sub 2). Each laminate contained eight fiber plies. Results of the unidirectionally reinforced composites tested at various angles to the reinforcement direction indicate large anisotropy in in-plane properties. In addition, strength properties of these composites along the fiber direction were independent of specimen gage length and were unaffected by notches normal to the fiber direction. Splitting parallel to the fiber at the notch tip appears to be the dominant crack blunting mechanism responsible for notch insensitive behavior of these composites. In-plane properties of the composites can be improved by 2-D laminate construction. Mechanical property results for (0 sub 2/90 sub 2)sub s and (+45/-45 sub 2) sub s laminates showed that their matrix failure strains were similar to that for (0) sub 8 laminates, but their primary elastic moduli, matrix cracking strengths, and ultimate composite strengths were lower. The elastic properties of unidirectional, cross-ply, and angle-ply composites can be predicted from modified constitutive equations and laminate theory. Further improvements in laminate properties may be achieved by reducing the matrix porosity and by optimizing the bond strength between the SiC fiber and RBSN matrix.

Rhatt, R. T.↗

NASA NTRS1990

Laminate behavior for SiC fiber-reinforced reaction-bonded silicon nitride matrix composites

The room temperature mechanical properties of SiC fiber reinforced reaction-bonded silicon nitride matrix composite laminates (SiC/RBSN) have been measured. The laminates contained approx 30 volume fraction of aligned 142-micron diameter SiC fiber in a porous RBSN matrix. Three types of laminate studied were unidirectional: (1) (0) sub 8, (2) (10) sub 8, and (3) (45) sub 8, and (90) sub 8; cross plied laminates (0 sub 2/90 sub 2); and angle plied laminates: (+45 sub 2/-45 sub 2). Each laminate contained eight fiber plies. Results of the unidirectionally reinforced composites tested at various angles to the reinforcement direction indicate large anisotropy in in-plane properties. In addition, strength properties of these composites along the fiber direction were independent of specimen gage length and were unaffected by notches normal to the fiber direction. Splitting parallel to the fiber at the notch tip appears to be the dominant crack blunting mechanism responsible for notch insensitive behavior of these composites. In-plane properties of the composites can be improved by 2-D laminate construction. Mechanical property results for (0 sub 2/90 sub 2) sub s and (+45/-45 sub 2) sub s laminates showed that their matrix failure strains were similar to that for (0) sub 8 laminates, but their primary elastic moduli, matrix cracking strengths, and ultimate composite strengths were lower. The elastic properties of unidirectional, cross-ply, and angle-ply composites can be predicted from modified constitutive equations and laminate theory. Further improvements in laminate properties may be achieved by reducing the matrix porosity and by optimizing the bond strength between the SiC fiber and RBSN matrix.

Bhatt, Ramakrishna T.↗

NASA NTRS1994

Thermal Shock Behavior of Silicon Nitride Flexure Beam Specimens with Indentation Cracks

The experimental results of thermal shock testing of silicon nitride flexure beam specimens containing indentation cracks are presented. The thermal stress induced by water quenching is much greater in the transverse direction than in the longitudinal direction, resulting in an insensitivity of residual bend strength to temperature differences up to 580 C. This result indicates that a flexure beam configuration is not an appropriate geometry for thermal shock testing when thermal shock behavior is to be evaluated from residual bend strength data.

Choi, Sung R.↗

NASA NTRS1990

Mechanical behavior and failure phenomenon of an in situ-toughened silicon nitride

The Weibull modulus, fracture toughness and crack growth resistance of an in-situ toughened, silicon nitride material used to manufacture a turbine combustor were determined from room temperature to 1371 C. The material exhibited an elongated grain structure that resulted in improved fracture toughness, nonlinear crack growth resistance, and good elevated temperature strength. However, low temperature strength was limited by grains of excessive length (30 to 100 microns). These excessively long grains were surrounded by regions rich in sintering additives.

Salem, Jonathan A.↗

NASA NTRS1992

Mechanical behaviour and failure phenomenon of an in situ toughened silicon nitride

Salem, J. A.↗

NASA NTRS2000

Silicon Nitride Creep Under Various Specimen-Loading Configurations

Extensive creep testing of a hot-pressed silicon nitride (NC 132) was performed at 1300 C in air using five different specimen-loading configurations: (1) pure tension, (2) pure compression, (3) four-point uniaxial flexure, (4) ball-on-ring biaxial flexure, and (5) ring-on-ring biaxial flexure. This paper reports experimental results as well as test techniques developed in this work. 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 compression loading, nominal creep strain generally decreased with time, resulting in a less-defined steady-state condition. Of the four creep formulations-power-law, hyperbolic sine, step, and redistribution--the conventional power-law formulation still provides the most convenient and reasonable estimation of the creep parameters of the NC 132 material. The data base to be obtained will be used to validate the NASA Glenn-developed design code CARES/Creep (ceramics analysis and reliability evaluation of structures and creep).

Choi, Sung R.↗

NASA NTRS2009

Thermal Residual Stress in Environmental Barrier Coated Silicon Nitride - Modeled

When exposed to combustion environments containing moisture both un-reinforced and fiber reinforced silicon based ceramic materials tend to undergo surface recession. To avoid surface recession environmental barrier coating systems are required. However, due to differences in the elastic and thermal properties of the substrate and the environmental barrier coating, thermal residual stresses can be generated in the coated substrate. Depending on their magnitude and nature thermal residual stresses can have significant influence on the strength and fracture behavior of coated substrates. To determine the maximum residual stresses developed during deposition of the coatings, a finite element model (FEM) was developed. Using this model, the thermal residual stresses were predicted in silicon nitride substrates coated with three environmental coating systems namely barium strontium aluminum silicate (BSAS), rare earth mono silicate (REMS) and earth mono di-silicate (REDS). A parametric study was also conducted to determine the influence of coating layer thickness and material parameters on thermal residual stress. Results indicate that z-direction stresses in all three systems are small and negligible, but maximum in-plane stresses can be significant depending on the composition of the constituent layer and the distance from the substrate. The BSAS and REDS systems show much lower thermal residual stresses than REMS system. Parametric analysis indicates that in each system, the thermal residual stresses can be decreased with decreasing the modulus and thickness of the coating.

Ali, Abdul-Aziz↗

NASA NTRS2018

Fabrication and Sub-Assembly of Electrostatically Actuated Silicon Nitride Microshutter Arrays

We have developed a new microshutter array (MSA) subassembly. The MSA and a silicon substrate are flip-bonded together. The MSA has a new back side fabrication process to actuate the microshutters electrostatically, and the new silicon substrate has light shields. The microshutters with a pixel size of 100 x 200 sq micrometers are fabricated on silicon with thin silicon nitride membranes. The microshutters rotate 90 deg on torsion bars. The selected microshutters are actuated, held, and addressed electrostatically by applying voltages on the electrodes the front and back sides of the microshutters. The substrate has the light shield to block lights around the microshutters. Also, electrical connections are made from the MSA to a controller board via the substrate.

microshutter array (MSA) sub-assembly↗

NASA NTRS1984

Silicon Nitride Antireflection Coatings for Photovoltaic Cells

Chemical-vapor deposition adapted to yield graded index of refraction. Silicon nitride deposited in layers, refractive index of which decreases with distance away from cell/coating interface. Changing index of refraction allows adjustment of spectral transmittance for wavelengths which cell is most effective at converting light to electric current. Average conversion efficiency of solar cells increased from 8.84 percent to 12.63 percent.

Johnson, C.↗

NASA NTRS1990

Matrix density effects on the mechanical properties of SiC fiber-reinforced silicon nitride matrix properties

The room temperature mechanical properties were measured for SiC fiber reinforced reaction-bonded silicon nitride composites (SiC/RBSN) of different densities. The composites consisted of approx. 30 vol percent uniaxially aligned 142 micron diameter SiC fibers (Textron SCS-6) in a reaction-bonded Si3N4 matrix. The composite density was varied by changing the consolidation pressure during RBSN processing and by hot isostatically pressing the SiC/RBSN composites. Results indicate that as the consolidation pressure was increased from 27 to 138 MPa, the average pore size of the nitrided composites decreased from 0.04 to 0.02 microns and the composite density increased from 2.07 to 2.45 gm/cc. Nonetheless, these improvements resulted in only small increases in the first matrix cracking stress, primary elastic modulus, and ultimate tensile strength values of the composites. In contrast, HIP consolidation of SiC/RBSN resulted in a fully dense material whose first matrix cracking stress and elastic modulus were approx. 15 and 50 percent higher, respectively, and ultimate tensile strength values were approx. 40 percent lower than those for unHIPed SiC/RBSN composites. The modulus behavior for all specimens can be explained by simple rule-of-mixture theory. Also, the loss in ultimate strength for the HIPed composites appears to be related to a degradation in fiber strength at the HIP temperature. However, the density effect on matrix fracture strength was much less than would be expected based on typical monolithic Si3N4 behavior, suggesting that composite theory is indeed operating. Possible practical implications of these observations are discussed.

Bhatt, Ramakrishna T.↗

NASA NTRS1982

Study of phenomena related to the sintering process of silicon nitride at atmospheric pressure

A procedure was perfected for the production of components used in engineering applications of silicon nitride. Particles of complex geometry that combine remarkable mechanical properties with a high density are obtained. The process developed, in contrast to the "hot pressing" method, does not use external pressures, and in contrast to the reaction bonding method, final densities close to the theoretical value are obtained.

Bertani, A.↗

NASA NTRS1984

Effect of hot isostatic pressing on reaction-bonded silicon nitride

Specimens of nearly theoretical density have been obtained through the isostatic hot pressing of reaction-bonded silicon nitride under 138 MPa of pressure for two hours at 1850, 1950, and 2050 C. An amorphous phase that is introduced by the hot isostatic pressing partly accounts for the fact that while room temperature flexural strength more than doubles, the 1200 C flexural strength increases significantly only after pressing at 2050 C.

Watson, G. K.↗