微波加热制备氮化钒工艺

Preparation Technology of Vanadium Nitride by Microwave Heating

摘要:

以五氧化二钒或偏钒酸铵为原料，炭黑为还原剂，采用微波法研究氮化钒的制备工艺。探讨在还原时间为60 min，还原最高温度为933 K时，混合物配碳比、氮化温度、氮化时间、氮气的流量、混合物成形压力等因素对产物氮含量的影响。由一步法结果表明：在混合物成形压力为20 MPa，配碳比为35%，氮化时间为120 min，氮化温度为1723 K，氮流量为2 L/min，产物氮化钒的氮含量为12.6%，钒含量79.2%，碳含量4.6%，密度为4.5 g/cm3。经 XRD检测产物为纯氮化钒。同时与传统的电阻炉加热方式相比，微波加热缩短了反应和冷却时间，节省能耗，简化工艺，降低成本。

Abstract:

Vanadium nitride was synthesized by the microwave heating process with V2O5 (or ammonium metavanadate) as starting materials and carbon black as reductant in N2 atmosphere. The effects of the ratio of the carbon black to V2O5, nitridation temperature, nitridation time, N2 flux and the mixture pressure on the nitrogen content of the product were investigated when the reduction time was 60 min and the highest reduction temperature 933 K. Results show that the product of vanadium nitride has 12.6% nitrogen, 79.2% vanadium and 4.6% carbon and its density is 4.5 g/cm3, when the mixture pressure is 20 MPa, the ratio of carbon to V2O5 35%, nitridation time 120 min, nitridation temperature 1723 K and N2 flux 2 L/min. XRD patterns detect the product is pure vanadium nitride. Compared with the conventional resistance furnace heating method, the microwave heating process can shorten the time of reaction and cooling, save the energy, simplify the process and reduce the cost.