氨解法制备立方相氮化铌纳米粉体

Synthesis of Nanosized NbN Powder with Cubic Structure by Ammonolysis Method

以沉淀法制备的高比表面积无定形Nb2O5为原料,采用氨解法在600～800℃、氮化3～8h制备了氮化铌纳米粉体.对不同氨解温度、氨解时间合成的NbN粉体用X射线衍射(XRD)、透射电镜(TEM)、氮吸附比表面积(BET)、热分析(TG/DTA)、氮分析等方法进行了表征,研究了氨解温度、氨解时间对NbN粉体性能的影响.结果表明: 该方法所需设备简单,氮化温度低,反应时间短,产品纯度高.在650～800℃氮化3～8h可得到粒径为15～40nm的X射线衍射纯立方相NbN纳米粉体.

The nanosized niobium oxide powder was synthesized by precipitation method. Then it was nitrided by NH 3 at 600～800℃ for 3～8 h and obtained nanosized niobium nitride powder. X-ray powder diffraction(XRD), transmission electron microscopy (TEM), BET surface area techniques,thermal analysis(TGDTA), and nitrogen content analysis were adopted for the characterization of the powders obtained under different ammonolysis conditions. The influences of the ammonolysis temperature and the holding time on the powder properties were investigated. It is concluded that this process need shorter time, lower temperature, and simple equipments. The 15～40 nm nanosized XRD pure cubic NbN powder can be prepared by nitrided at 650～800℃ for 3～8 h.