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Silicon nitride (Si3N4) ceramics with Y2O3-Al2O3 as sintering additives were prepared by pressureless sintering technology using two kinds of Si3N4 powders as raw materials. The particle size of Si3N4 powders ball-milled with various times were characterized and the effects of particle size on the densification behavior of Si3N4 ceramics were investigated. The relative density and microstructure of the sintered bodies at different sintering temperatures were determined. The experimental results show that the powders with longer milling time have finer particle size and the samples with fine particle display higher shrinkage-rate at lower sintering temperature than the one with coarse particle. By extending milling time, the density gap between the sintered ceramics using different Si3N4 powder become narrower. The main factor resulting in the difference of sintering densification behavior is the particle size of Si3N4 powders rather than metallic oxide impurity of raw powders.

Abstract

The wetting and spreading behaviors of pure nickel and nickel based alloys on sintered ZrB2-SiC ceramics and their interfacial microstructures were investigated in this presentation. The nickel-based alloys were mainly the commercial nickel-molybdenum-chromium products. The wetting and spreading properties were observed by a real-time thermal optical measurement system under flowing argon-5%hydrogen atmosphere. As temperature increased, the pure nickel cylinder sample on ZrB2-SiC substrate had few changes before 1228°C except for the thermal expansion in size. After that, liquid phase formed and spread gradually on the ceramic substrate. The contact angle was about 15o after holding 15min at 1600°C. Therefore, pure nickel could contact sintered ZrB2-SiC ceramics well. Meanwhile, the introduction of molybdenum and/or chromium in the pure nickel was beneficial for the wetting of nickel on sintered ZrB2-SiC ceramics. The contact angles of Ni-28Mo and Ni-16Mo-23Cr alloys on sintered ZrB2-SiC ceramics after 1600°C/15min were 13o and 2o, respectively. In addition, the temperatures of the liquid drop formed rose obviously in contrast to the pure nickel. The SEM images indicated that the interfacial microstructures of Ni-based alloys on sintered ZrB2-SiC ceramic substrates were uniform and the dissolved boundaries showed that they had a good bonding. However, some cracks were found in the Ni/ZrB2-SiC system for their high thermal mismatch. On the other hand, the Ni-Mo (-Cr)/ZrB2-SiC interface had few defections and evident elemental diffusion between the ceramic substrates and the alloys were found at the interface.

The effect of Al2O3 and SiC as the sintering additives for pressureless sintering boron carbide (B4C) was investigated. The aids were 10 wt% Al2O3 (10A), 10 wt% Al2O3 and 15 wt% SiC (10A15S), 10 wt% Al2O3 and 30 wt% SiC (10A30S), and 30 wt% SiC (30S) (all based on B4C). The sintering behavior, microstructure evolution and phase compositions of the samples were studied. 10A15S and 10A30S can effectively enhance the densification of B4C, comparing with 10A and 30S. The linear shrinkage rate of 14% for the 10A15S and 10A30S samples can be reached. The bending strength approaching 400MPa for the 10A30S sample sintered at 2170°C can be obtained.

Low fracture toughness of SiC ceramics limits their applications for the low reliability. Inclusion of second ceramic phase improves the toughness of SiC ceramics. In this presentation, SiC ceramics with 5wt% TiC was pressureless liquid phase sintered (LPS) with the additives of Al2O3 and Y2O3 to ~98% theoretical density at the temperature of 1920 °C for 1 hour. The TiC grains were well distributed and good for the uniform distribution of the liquid phase YAG in the SiC matrix, which resulted in the homogeneous microstructure with fine SiC grains. The existence of TiC benefited the formation of elongated α-SiC, which favored the bridging and deflection of cracks so that the fracture toughness was improved to some extent. Because the amount of TiC was so small that the inherent properties of SiC was not degraded. The flexural strength and Vickers hardness maintained similar with the LPS SiC without TiC. The phase compositions detected in the sample were SiC, YAG and TiC. And no solid-solution of SiC and TiC was revealed by the mapping of EDS.

Ultra-high temperature ceramic composites of ZrB2-SiC were densified by pressureless sintering. Ultra-fine ZrB2-SiC composite powders synthesized by sol-gel method were mixed with commercial ZrB2 and SiC powders. The sintered body of hybrid powders (combined commercial and synthesized composite powders) showed excellent properties not only in the relative density but also the flexure strength. Dry-pressed compacts using 4wt% Mo as a sintering aid were sintered to nearly full density at 2200C/2h. The average strength was ~560MPa and the maximum was ~632MPa. SEM and TEM showed that SiC particles were distributed homogenously in the ZrB2 matrix and the average particle size was ~5μm. From HRTEM observations, the grain boundaries were apparently free of glassy phases and no intermediate phases existed.

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Ultra-fine titanium diboride (TiB2) powders have been prepared by carbothermal reduction reactions in TiO2-B2O3-C system using tetrabutyl titanate, boric acid and phenolic resin as the solution-derived precursors. The reactions were substantially completed at relatively lower temperature (<1400°C) and the resulting products had a smaller average crystallite size (< 200 nm). However, below 1100°C, titanium carbide was the predominant phase and the relative content decreased with the rise of temperature. The thermodynamic change in TiO2-B2O3-C system was mainly studied by TG-DTA and the mechanism of synthesis of TiB2 was discussed. The crystallite size and morphology of the synthesized powders were characterized by SEM and TEM.

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3-D braided C fiber preform was used to reinforce SiC matrix by polymer infiltration and pyrolysis (PIP). The effect of PCS pyrolysis process on the uncoated carbon fiber was studied. During the pyrolysis, amorphous SiCxOy and some free silicon yielded. The Si element diffused into the C fiber from the matrix because of the concentration gradient at high temperature and destroyed the intrinsic structure of the uncoated C fiber. At the same time, the free Si reacted with the uncoated C fiber. Thus, strong bonding between the fiber and matrix was formed. As a result, bending strength of the composite was decreased.

A method of waved-thermal field chemical vapor infiltration was introduced. And interphases of silicon carbide layer and carbon layer were processed via the route. The preforms with the interfacial coatings were densified by method of forced-flow thermal-gradient chemical vapor infiltration (FCVI) employing hexamethyldisilazane (HMDS) as precursor material of the matrix. The matrix of the composites annealed at 1400°C consists of nano-polycrystalline silicon carbide. The configuration of fracture surface was observed by scanning electronic microscopy (SEM). The interphases behaved successfully as mechanical fuse for the reinforcing fibers.

Stable ZrB2-based ultra-high temperature ceramic slurries were prepared and characterized with a solid content 40 vol% by aqueous gelcasting which was suitable to form high quality and complexshaped ceramic parts. In the present work, Ammonium Citrate Tribasic (ACT) was used as the dispersant. The properties of ZrB2 slurry, and the influencing factors were investigated by conventional techniques such as sedimentation tests, particle size distribution measurements, electrokinetic measurements and rheological analysis. High solids loading and low viscosity slurry was obtained by controlling the optimal conditions for the ZrB2-based ceramic powders.