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At least 19 records

Oxynitride glass fibers

Research at the Army Materials Technology Laboratory (AMTL) and elsewhere has shown that many glass properties including elastic modulus, hardness, and corrosion resistance are improved markedly by the substitution of nitrogen for oxygen in the glass structure. Oxynitride glasses, therefore, offer exciting opportunities for making high modulus, high strength fibers. Processes for making oxynitride glasses and fibers of glass compositions similar to commercial oxide glasses, but with considerable enhanced properties, are discussed. We have made glasses with elastic moduli as high as 140 GPa and fibers with moduli of 120 GPa and tensile strengths up to 2900 MPa. AMTL holds a U.S. patent on oxynitride glass fibers, and this presentation discusses a unique process for drawing small diameter oxynitride glass fibers at high drawing rates. Fibers are drawn through a nozzle from molten glass in a molybdenum crucible at 1550 C. The crucible is situated in a furnace chamber in flowing nitrogen, and the fiber is wound in air outside of the chamber, making the process straightforward and commercially feasible. Strengths were considerably improved by improving glass quality to minimize internal defects. Though the fiber strengths were comparable with oxide fibers, work is currently in progress to further improve the elastic modulus and strength of fibers. The high elastic modulus of oxynitride glasses indicate their potential for making fibers with tensile strengths surpassing any oxide glass fibers, and we hope to realize that potential in the near future.

Patel, Parimal J.↗

Temperature dependence of the biaxial modulus, intrinsic stress and composition of plasma deposited silicon oxynitride films

Silicon oxynitride films were deposited by plasma-enhanced chemical-vapor deposition. The elemental composition was varied between silicon nitride and silicon dioxide: SiO(0.3)N(1.0), SiO(0.7)N(1.6), SiO(0.7)N(1.1), and SiO(1.7)N(0.%). These films were annealed in air, at temperatures of 40-240 C above the deposition temperature (260 C), to determine the stability and behavior or each composition. the biaxial modulus, biaxial intrinsic stress, and elemental composition were measured at discrete intervals within the annealing cycle. Films deposited from primarily ammonia possessed considerable hydrogen (up to 38 at.%) and lost nitrogen and hydrogen at anneal temperatures (260-300 C) only marginally higher than the deposition temperature. As the initial oxygen content increased a different mechanism controlled the behavior or the film: The temperature threshold for change rose to approximately equal to 350 C and the loss of nitrogen was compensated by an equivalent rise in the oxygen content. The transformation from silicon oxynitride to silica was completed after 50 h at 400 C. The initial biaxial modulus of all compositions was 21-3- GPa and the intrinsic stress was -30 to 85 MPa. Increasing the oxygen content raised the temperature threshold where cracking first occurred; the two film compositions with the highest initial oxygen content did not crack, even at the highest temperature (450 C) investigated. At 450 C the biaxial modulus increased to approximately equal to 100 GPa and the intrinsic stress was approximately equal to 200 MPa. These increases could be correlated with the observed change in the film's composition. When nitrogen was replaced by oxygen, the induced stress remained lower than the biaxial strength of the material, but, when nitrogen and hydrogen were lost, stress-relieving microcracking occurred.

Harding, David R.↗

Crack Growth Testing of an Aluminum Oxynitride (AlON) for International Space Station Kick Panes

The mechanical properties of an aluminum oxynitride supplied as ground beams and disks were measured using ASTM International (formerly American Society for Testing and Materials) standard test methods. The slow crack growth tests were complicated by a "short" finish that increased strength scatter. Refining of the finish by more material removal in the second stage of grinding or the use of uniaxial grinding as specified in ASTM C1499 might have avoided the issue. The structural design parameters are an elastic modulus of E = 319 GPa, Poisson's ratio of v = 0.26, a fracture toughness of KIvb(A) = 2.18 MPa/m, slow crack growth (SCG) parameter n = 36, and SCG parameter A = 1.96 x 10-11 m/s.(MPa/m)n. For a ground finish, the Weibull parameters are a mean modulus of m = 14.0 and characteristic strength of sigma theta = 250.2 MPa. The 2015 vintage material exhibits similar mechanical properties to a 2010 vintage billet. Indentation flaws were not sensitive to the inherent crack growth mechanisms of this material and produced misleading results.

strength↗

Effect of Si3N4 powder reactivity on the preparation of the Si2N2O-Al2O3 silicon aluminum oxynitride solid solution

Dense high-purity silicon aluminum oxynitride was prepared by reactive hot-pressing of an Si3N4-Al2O3-SiO2 mixture. The formation of a single-phase material was found to be critically dependent on the Si3N4 powder in the starting mixture. It is suggested that evolution of a chlorine- and nitrogen-containing species may enhance the reactivity of Si3N4 in this reaction. Densities of O prime sialons are very similar to that of Si2N2O, the widely quoted value in the ceramics literature of 3.1 g/cu cm for the density of Si2N2O being incorrect.

Sekercioglu, I.↗

The interaction of molten silicon with silicon aluminum oxynitrides

Silicon aluminum oxynitride solid solutions (sialons) based on beta-Si3N4 and Si2N2O behave differently in contact with molten silicon. The Si2N2O-based sialons convert to almost pure Si3N4, apparently through a two-step decomposition and solution-precipitation reaction, whereas the beta-Si3N4 sialons are preferentially attacked at the grain boundaries. The composition of the grain-boundary phase appears to control the rate of reaction.

Wills, R. R.↗

Evidence from transmission electron microscopy for an oxynitride layer in oxidized Si3N4

Microstructural and energy dispersive spectrometry evidence is produced, from transmission electron microscopy, to show that a silicon oxynitride inner layer is produced by the oxidation of silicon nitride in dry oxygen at 1350 C as proposed by Tressler et al. (1989). However, details of the microstructures at the oxide/nitride interface do not agree entirely with the rest of the Tressler model for the oxidation of Si3N4.

Ogbuji, Linus U. J. T.↗

Thermal shock resistance of silicon oxynitride

The thermal shock resistance of Si2N2O refractory material was studied. The thermal expansion coeff. is 3.55x10 to the -6th power at 20 to 800 C and 2.86x10 to the -6th power m/m/deg at 20 to 200 C. The breaking loads are high at high stress. Young's modulus E and the shear modulus G decrease linearly with increasing porosity. For dense material E sub o approx. = 216,500 N/mm2 and G approx = 90,600 N/mm2. The Vickers hardness of the dense material is comparable to that of sapphire. The results on thermal shock show that R, the breaking load, stays constant for T T sub c, the first cracks appear and R decreases sharply for T=T sub c. As the severity of the thermal shock is increased at T T sub c, a small no. of new, large-size cracks appears. The shock's cumulative effect is negligible, and repeated shocks do not change the cracks. The low values of the thermal expansion coefficient and Young's modulus and the high tension breaking load are considered. Sintered Si2N2O with 5% MgO shows excellent cracking resistance under thermal shock.

Glandus, J. C.↗

Optical and electrical characterizations of laser-chemical-vapor-deposited aluminum oxynitride films

Composition-dependent optical and electrical properties of L-CVD (Al2O3)1-c-(AlN)c composite films are examined. The optical properties exhibit a continuous change from Al2O3 to AlN with increasing value of the composition parameter c from zero to one. There is a critical concentration value of about 0.3 below and above which Al2O3- and AlN-like optical properties are observed. The impurity absorption regions are 5.1-6.7 eV for Al2O32 and 4.6-6.0 for AlN, while the energy gap is about 6.7 eV for Al2O3 and 6.0 eV for AlN. The electrical properties of Al-insulator n-Si MIS structures display externally programmable states when bulk-controlled electron emission occurs from the traps. In the high-field region a persistent polarization field is established within the insulator. C-V characteristics of the samples are more sensitive to the concentration factor c than the I-V characteristics. A large clockwise hysteresis is observed for AlN, but a smaller counterclockwise one is observed for Al2O3.

Demiryont, H.↗

Calculated Coupling Efficiency Between an Elliptical-Core Optical Fiber and a Silicon Oxynitride Rib Waveguide [Corrected Copy]

The effective-index method and Marcatili's technique were utilized independently to calculate the electric field profile of a rib channel waveguide. Using the electric field profile calculated from each method, the theoretical coupling efficiency between a single-mode optical fiber and a rib waveguide was calculated using the overlap integral. Perfect alignment was assumed and the coupling efficiency calculated. The coupling efficiency calculation was then repeated for a range of transverse offsets.

Tuma, Margaret L.↗

Mechanism of incipient oxidation of bulk chemical vapor deposited Si3N4

X-ray photoelectron spectroscopy was employed, in conjunction with ion bombardment, to analyze the chemical composition profile across thin (less than 50 nm) oxide films on chemically vapor deposited Si3N4. The thermal oxides were grown in dry oxygen at 1100 C on samples with or without native oxide film (formed in room air). The results show that the thermal oxidation product was silicon oxynitride of graded N:O ratio, and that the presence of a native oxide film promotes the formation of a SiO2 crust over the oxynitride. It is proposed that the fundamental mechanism of Si3N4 oxidation is progressive O-for-N substitution in the silicon oxynitride unit tetrahedron, which is best designated SiN(2-x)O(2+x), where x is also an index of depth. The corresponding equation for nonstoichiometric oxidation of Si3N4 describes a bulk (rather than an interface) reaction process, with significant implications for O2 and N2 fluxes and diffusivities.

Ogbuji, L. U. T.↗

Development and evaluation of die and container materials

X = 0.75 Beta prime Sialon (a silicon aluminum oxynitride) and Sibeon (silicon beryllium oxynitride) are promising die materials. In sessile drop tests in contact with molten silicon, beryllium contamination was less than ppm and aluminum contamination 50 ppm. A shaping die of the Sialon material was successfully fabricated. Dry milling studies for the preparation of Si3N4-Al2O3-ALN mixtures were performed with butanol, acetic anhydride, oleic acid, and triethanolamine milling aids. Optimum mixing was achieved with 0.15 percent triethanolamine using a milling time of 8 hours. Preliminary evaluation of Sibeon materials indicates that they are more resistent to molten silicon attack than Sialon. Silicon contamination from the beryllium was less than aluminum contamination even though the aluminum impurity level in the Sibeon was only 450 to 1300 ppm. Work designed to produce an aluminum-free Sibeon is described.

Wills, R. R.↗

Development and evaluation of die and container materials. Low cost silicon solar array project

Specific compositions of high purity silicon aluminum oxynitride (Sialon) and silicon beryllium oxynitride (Sibeon) solid solutions were shown to be promising refractory materials for handling and manipulating solar grade silicon into silicon ribbon. Evaulation of the interaction of these materials in contact with molten silicon indicated that solid solutions based upon beta-Si3N4 were more stable than those based on Si2N2O. Sibeon was more resistant to molten silicon attack than Sialon. Both materials should preferably be used in an inert atmosphere rather than under vacuum conditions because removal of oxygen from the silicon melt occurs as SiO enhances the dissolution of aluminum and beryllium. The wetting angles of these materials were low enough for these materials to be considered as both die and container materials.

Wills, R. R.↗

A kinetic model for the thermal nitridation of SiO2/Si

To explain the observed nitrogen distributions in thermally nitridated SiO2 films, a kinetic model is proposed in which the nitridation process is simulated, using the first-order chemical kinetics and Arrhenius dependence of the diffusion and reaction rates on temperature. The calculations show that initially, as the substrate reacts with diffusing nitrogen, a nitrogen-rich oxynitride forms at the SiO2-Si interface, while at nitridation temperatures above 1000 C, an oxygen-rich oxynitride subsequently forms at the interface, due to reaction of the substrate with an increasingly concentrated oxygen displaced by the slower nitridation of the SiO2. This sequence of events results in a nitrogen distribution in which the peak of the interfacial nitrogen concentration occurs away from the interface. The results are compared with the observed nitrogen distribution. The calculated results have correctly predicted the positions of the interfacial nitrogen peaks at the temperatures of 800, 1000, and 1150 C. To account for the observed width of the interfacial nitrogen distribution, it was found necessary to include in the simulations the effect of interfacial strain.

Vasquez, R. P.↗

Chemical profiling of silicon nitride structures

X ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), and scanning electron microscopy (SEM) were used to study structural and chemical inhomogeneities in several electronic materials and device structures of relevance to radiation hard electronics. The systems studied include metal nitride oxide semiconductor (MNOS) structures, silicon oxynitride (SiO(x)N(y)) formed by the thermal nitridation of SiO2, and semiconductor on insulator (SOI) structures. Studies of MNOS structures suggest that the effect of H2 annealing is to make the Si3N4/SiO2 interface less abrupt by causing interdiffusion of silanol and silamine groups with subsequent oxynitride formation. Another effect of the annealing appears to be to relieve the strain at the SiO2/Si interface.

Vasquez, R. P.↗

The mineralogy of meteorites.

Of particular interest among minerals recently discovered in meteorites are five phosphate minerals, three of them unknown in terrestrial rocks; a chromium nitride and a silicon oxynitride; lonsdaleite and chaoite, new polymorphs of carbon; ringwoodite and majorite, the spinel and garnet analogs of olivine and pyroxene, respectively; a number of calcium- and aluminum-rich silicates in the Allende meteorite, a type III carbonaceous chondrite which fell in 1969; and several alkali-rich silicates found as inclusions in iron meteorites. Knowledge of the compositional range of the common minerals olivine, pyroxene, and plagioclase has also been greatly increased by recent researches.

Mason, B.↗

Development and Evaluation of Die Materials for Use in the Growth of Silicon Ribbons by the Inverted Ribbon Growth Process. Task 2: LSSA Project

Several ribbon growth experiments were performed from V-shaped dies coated with CVD Si3N4. The most significant result was the ability to perform five consecutive growth runs from the same die without mechanical degradation of the die through temperature cycling. The die was made from vitreous carbon coated with CVD Si3N4. Silicon oxynitride, Si2N2O, was examined with respect to thermal stability in contact with molten silicon. The results of X-ray analysis indicate that this material is converted to both alpha - and beta-Si3N4 in the presence of molten silicon. Experiments on the stability of CVD SiOxNy shoe that this material can be maintained in contact with molten silicon (sessile drop test) for greater than 30 h at 1450 C without total decompositon. These layers are converted mainly to beta-Si3N4.

Duffy, M. T.↗

Ceramic for Silicon-Shaping Dies

Silicon beryllium oxynitride (SiBON) is a promising candidate material for manufacture of shaping dies used in fabricating ribbons or sheets of silicon. It is extremely stable, resists thermal shock, and has excellent resistance to molten silicon. SiBON is a solid solution of beryllium silicate in beta-silicon nitride.

Sekercioglu, I.↗