氨气还原氮化法制备有序介孔TiN粉体及其电化学性能

以四氯化钛为原料,嵌段共聚物P123(PEO_(20)-PPO_(70)-PEO_(20))为模板剂,氰胺为稳定剂,采用非水解溶胶-凝胶法制备有序介孔TiO_2粉体,再经氨气还原氮化处理得到有序介孔TiN粉体.利用广角/小角X射线衍射、电子显微镜和N_2气吸-脱附等对TiN粉体的结构进行了表征,并通过循环伏安和充放电测试表征了电化学性能.结果显示,该粉体为高纯立方TiN相,呈球形颗粒状,具有有序介孔结构,比表面积高达97 m~2/g.在不同扫描速率下循环伏安曲线均呈类矩形,根据电流密度为50 m A/g时的恒流充放电(GCD)曲线计算比电容为233 F/g,且经2000次充放电循环后比容量仍保持90%以上,在功率密度为0.1 k W/kg时能量密度高达65 W·h·kg~(-1).

Synthesis of Ordered Mesoporous TiN Powder via Ammonia Reduction Nitridation Reaction and Its Electrochemical Performance

The ordered mesoporous TiN powder was synthesized by reduction-nitridation method based on the nonhydrolytic sol-gel process using titanium tetrachloride as the raw material,P123 as the structure-directing agent and cyanamide as the stabilizer.The structural information of the composite powder was characterized by wide-angle/small-angle X-ray diffraction,scanning electronic microscopy,N2 adsorption-desorption analysis,and the electrochemical properties were characterized by cyclic voltammetry (CV) and galvanostatic chargedischarge(GCD) measurements.The results show that the synthesized TiN powder was highly pure cubic TiN phase and had ordered mesoporous structure,its specific surface area was 97 m2/g.The CV curves at different scan rates look like the rectangle.The specific capacitance was 233 F/g at current density of 50 mA/g,and remained 90％ even after 2000 cycles.When the power density was 0.1 kW/kg,the energy density was as high as 65 W · h/kg.