A mixture of cubic silicon powder, hexagonal boron nitride powder and graphite powder was mechanically alloyed for 30 hrs in argon. The as-milled 2Si-B-3C-N composite powder was heated up to 1900 °C in nitrogen, with a heating rate of 25 °C/min and under a pressure of 80 MPa. XRD and HRTEM results show that the as-milled 2Si-B-3C-N composite powder has a well amorphous structure. Under the current hot-pressing circumstances, the amorphous ceramic starts to crystallize at a temperature between 1800 °C and 1900 °C. Once the temperature is higher than crystallization temperature, crystallites appear in the amorphous matrix with a great nucleation rate, but a small growth rate. Hot pressed at 1900 °C for 0 mins or 10 mins, the prepared 2Si-B-3C-N bulk ceramic has an average grain size of 8.7 nanometers and 22.3 nanometers, respectively. After an intensive literature search, we believe the present work is the first one to make clear that it is possible to use the mechanical alloying route to prepare amorphous Si-B-C-N ceramic with such a high crystallization temperature.