Optimization of precursor structure by dispersants to promote nitrogen reduction process to prepare high-quality VN

Abstract

In this study, three dispersants of polyvinyl pyrrolidone (PVP), polyethylene glycol (PEG) and citric acid (CA) are used to optimize the structure of the precursor in order to prepare high quality VN. Under optimum condition, the VN with nitrogen content of 17.94 % is prepared by adding 5 % PVP. The sequence of phase evolution from the precursor to VN is: APV → V2O5 → V6O13 → V7O13 → VO2 → V3O5 → V2O3 → (VC) → VN. The precursors of adding 5 % PVP have lower Ea of 0.17 kJ mol−1, 20.51 kJ mol−1 and 62.70 kJ mol−1 during reduction and nitration process, which is easier to be reduced and nitridated. PVP not only promotes the uniform dispersion of the carbon powders in the vanadium rich solution but also enhance the hydrogen bonding of APV ions to promote their nucleation and growth. The precursor with uniform and concentrated particle size distribution, complete and stable encapsulation of shell of APV and core of carbon powder, and uniform and moderate thickness of APV shell is successfully prepared by adding PVP. The precursor has a larger phase reaction interface and more reactive sites during the nitriding reduction process, which results in a faster reduction and nitriding rate. In comparison with the current process, the nitriding reaction temperature has been reduced from 1400 ∼ 1500 °C to 1150 ∼ 1200 °C, the reaction time has been shortened by 75 %, and the N2 consumption has been reduced by 40 %.