Effect of nitrogen gas pressure during heat treatment on the morphology of silicon nitride fibers synthesized by carbothermal nitridation

The effects of N2 gas pressure on the diameter and morphology of Si3N4 fibers obtained via carbothermal nitridation were investigated. Sol–gel-derived precursors containing a silica and carbon mixture were placed in an Al2O3 crucible and heat-treated under various N2 pressures from 0.1 to 0.5 MPa at 1500ºC. The heat-treated samples were characterized by X-ray diffraction (XRD), a scanning electron microscope (SEM) coupled with an energy dispersion X-ray (EDX) spectrometer, and transmission electron microscopy (TEM). Various nitride fibers with α- and β-phase Si3N4 were formed. The fiber diameter decreased with increases in N2 pressure, and nanometer-scale fibers of around 200 nm in diameter were obtained at a N2 pressure of 0.5 MPa. It was found that silicon oxynitride Si2N2O or its Al-doped form, O′-SiAlON, was produced due to high N2 pressure and doping with Al originating from the Al2O3 crucible. This oxynitride was considered to act as a template for Si3N4 fiber growth by the direct phase transformation mechanism. It was shown that the diameter of the Si3N4 fibers decreased for two reasons: decreased partial pressure of SiO gas due to high N2 pressure and increased formation of the silicon oxynitride templates.