Ceramic matrix composites (CMCs) have been designed and developed for extreme operating environments. The aim of the present study is to look for a rapid densification process providing a high level of material performance. The fibrous preform was made of Hi-Nicalon S fibers woven in a 3D interlock weave. The matrix was composed of Si2N2O prepared inside the CMCs by reacting a mixture of Si and SiO2 under high nitrogen pressure (1 to 3 MPa). Silica was either impregnated by slurry or obtained by oxidation of silicon grains inside the preform. The synthesis reaction was initiated by heating the impregnated preform by means of a carbon resistor submitted to Joule effect. Composition, homogeneity and porosity of the formed matrix were studied and interpreted as a function of the experimental parameters (nitrogen pressure, heating rate of the preform) as well as the recorded thermal history of the process. The present results show that the matrix formation is almost completed in less than one minute. Melting of silicon has a major influence on the process. Competition was observed between the formation of Si3N4 and Si2N2O, which could be mainly controlled by the heating rate of the preform and the nitrogen partial pressure.
Ceramic matrix composites (CMCs) have been prepared and optimized as already described in part I of this paper. The fibrous preform made of Hi-Nicalon S fibers was densified by a matrix composed of Si2N2O prepared inside the CMC by reacting a mixture of Si and SiO2 under high nitrogen pressure. This part describes the oxidation resistance and mechanical properties of the optimized CMC. The CMC submitted to oxidation in wet oxygen at 1400 °C for 170 h exhibited an oxidation gradient from the surface to almost the center of the sample. In the outer part of the sample, Si2N2O, Si3N4 and SiC were oxidized into silica in the cristobalite-crystallized form. The matrix microstructure looks similar to the original one at the center of the sample, while at the surface large pores are observed and the fiber/matrix interphase is consumed by oxidation. The elastic modulus and the hardness measured at room temperature by nano-indentation are, respectively, 100 and 8 GPa. The elastic modulus measured at room temperature by tensile tests ranges from 150 to 160 GPa and the ultimate yield strength from 320 to 390 MPa, which corresponds to a yield strain of about 0.6%. The yield strength identified by acoustic emission is about 40 MPa.
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