TEM characterization of some crude or air heat-treated SiC Nicalon fibres

Abstract

Commercial Nicalon fibres were prepared by thin transverse sectioning and studied by transmission electron microscopy. A progressive tilting of the incident beam allows us to explore the selected-area diffraction (SAD) pattern along two orthogonal directions, increasing the tilting angle (dark-field (DF) imaging). The lattice fringes technique was also used. The samples were Nicalon 001, 101 and 201 fibres, the latter also being studied after heat treatment in air at 1300° C for 48 h. The SAD pattern of the 001 fibre only shows the SiC, 1 1 intense halo whereas the other samples show all the SiC (1 1 1, 2 2 0 and 31 1) strongly scattered beams, indicating a microcrystalline state. Correspondingly, DF imaging does not indicate any localized measurable scattering domain for 001. Only bright dots can be seen, less than 1 nm in size. The other fibres show SiC microcrystals respectively 2 nm (1 01 ), 3 nm (201 ) and up to 7 nm (heat-treated 201) in extent. Free aromatic carbon, shaped in small units less than 1 nm in size fills up the interstices between SiC. These units tend to lie flat on SiC. In heat-treated fibres, they form incomplete layers around the edges. In addition, the heat-treated 2 01 fibre show a 1μm thick layer of cristobalite at the fibre surface. These crystals are polytypes.