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Abstract: SiBON fiber precursor was successfully synthesized through sol–gel method when distilled water was used as solvent, boric acid (H3BO3), melamine (C3H6N6) and tetraethoxysilane (TEOS) were used as raw materials. The precursor was nitrogenized in N2 at 1400–1800°C to prepare SiBON fiber. The chemical bonds structure, the micrograph and the elemental distribution of SiBON fiber have been investigated by X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive spectrometer (EDS) and infrared spectroscopy (FTIR). The results showed: (1) the best nitrogenization temperature of SiBON fiber precursor was 1800°C; (2) SiBON fiber was amorphous materials of nitrides containing a small quantity of SiO2 and BN crystals; (3) bonds of BN, BOSi, BNSi and SiOSi existed in the SiBON fiber. [Copyright &y& Elsevier]