Preparation of vanadium nitride using a thermally processed precursor with coating structure

Abstract

A new effective method is proposed to prepare vanadium nitride (VN) via carbothermal reduction–nitridation (CRN) of the precursor, obtained by adding carbon black (C) to the stripping solution during the vanadium recovery from black shale. VN was successfully prepared at a low temperature of 1150 °C for only 1 h with a C/V2O5 mass ratio of 0.30 in N2 atmosphere, but a temperature of 1300–1500 °C is required for several hours in the traditional CRN method. The low synthesis temperature and short period for the preparation of VN was due to the vanadium-coated carbon structure of the precursor, which enlarged the contact area between reactants significantly and provided more homogeneous chemical composition. In addition, the simultaneous direct reduction and indirect reduction of the interphase caused by the coating structure obviously accelerated the reaction. The phase evolution of the precursor was as follows: (NH4)2V6O16·1.5H2O→V2O5→V6O13→VO2 !V4O7 →V2O3→VC→VN. The precursor converted to V6O13 and VO2 completely after being calcined at 550 °C, indicating that the pre-reduction of V2O5 in the traditional CRN method can be omitted. This method combined the synthesis of VN with the vanadium extraction creatively, having the advantages of simple reaction conditions, low cost and short processing time.