Application of the chemical vapor infiltration and reaction (CVI-R) technique for the preparation of highly porous biomorphic SiC ceramics derived from paper

Chemical vapor infiltration and reaction (CVI-R) is used to produce biomorphic high porous SiC ceramics based on biological structures such as paper. The paper fibers are first converted into a biocarbon (Cb) template by a carbonization step. In a second step methyltrichlorosilane (MTS) in excess of hydrogen is infiltrated into the Cb-template by CVI technique, depositing a Si/SiC layer around each fiber. The reaction (R) between biocarbon and excess silicon to form additional silicon carbide occurs during a subsequent thermal treatment as a third step of the ceramization process. Due to the mild infiltration conditions (850–900 °C) the initial micro- and macrostructure of the carbon preform is retained in the final ceramics. The applied characterization methods after every step of the ceramization process are X-ray Photoelectron Spectroscopy (XPS), Raman spectroscopy, Thermal Gravimetric Analysis (TGA), and Scanning Electron Microscopy (SEM). The bending strength of the resulting porous ceramics is measured by the double ring bending test. It is found that a slight excess of free Si in relation to the amount of carbon from the Cb-template must be deposited in the Si/SiC layer to achieve a nearly complete conversion of the Cb-templates into SiC ceramic. The weight gain after infiltration has to be at least 400 wt.%. Varying the infiltration conditions such as temperature, MTS concentration and infiltration time, ceramics in a wide range of porosity (55–80%) and mechanical properties (5–40 MPa) can be produced. A thermal treatment temperature of 1400 °C is found to be optimal for the reaction between the deposited Si and the biocarbon.