介孔氮化钛粉体还原氮化演变过程及电化学性能  

Reduction Nitride Evolution and Electrochemical Properties of Mesoporous Titanium Nitride Powder

作　　者：倪洁 陈越军 吕东风 张利芳 崔帅 崔燚 魏恒勇 卜景龙 Ni Jie;Chen Yuejun;Lv Dongfeng;Zhang Lifang;Cui Shuai;Cui Yi;Wei Hengyong;Bu Jinglong(College of Material Science and Engineering,North China University of Science and Technology,Tangshan 063210,China;Institute of Fuel Cell Power Sources,Tongji University,Shanghai 201800,China;School of Metallurgy,Northeastern University,Shenyang 110819,China)

机构地区：[1]华北理工大学材料科学与工程学院,河北唐山063210 [2]同济大学燃料电池复合电源研究所,上海201800 [3]东北大学冶金学院,辽宁沈阳110819

出　　处：《稀有金属材料与工程》2021年第12期4402-4409,共8页Rare Metal Materials and Engineering

基　　金：国家自然科学基金(51272066,51472072);河北省自然科学基金(E2013209183,E2019209474)。

摘　　要：以乙醇为氧供体,以TiCl_(4)为钛源,以P123为造孔剂,用非水解溶胶凝胶法结合氨气还原氮化法制备出介孔TiN粉体,将其作为电极材料制备扣式电容。利用XRD、SEM、EDS、BET和XPS等组分结构表征手段和CV、GDC和EIS等电化学测试手段研究了还原为氮化温度对粉体的物相、孔结构以及电化学性能的影响规律。结果发现,随着还原氮化温度的升高,粉体中TiO_(2)被逐步还原为TiO再被氮化为TiN,Ti-O键逐渐被Ti-N键合所部分取代,且其物相纯度增加,颗粒尺寸增大,粉体中介孔孔径则先增大后减小。当还原氮化温度为800℃时粉体比表面积为41 m^(2)/g,孔道结构发达,平均孔径为24 nm,有利于离子传输,电化学性能提高。此时,样品中内在阻抗较小,为0.9Ω,在电流密度为20 mA/g时,比电容为130 F/g,且在50 mA/g下经历1000次循环之后还能保持初始比电容的近90%。The mesoporous TiN powder was prepared by non-hydrolyzed sol-gel method combined with ammonia gas reduction nitrification method using ethanol as oxygen donor,titanium tetrachloride(TiCl_(4))as titanium source and P123 as pore-forming agent,and then was used an electrode material to prepare button capacitor.The effects of reduction nitride temperature on the phase,pore structure and electrochemical performance of mesoporous TiN powder were test by XRD,SEM,BET,XPS,CV,GDC and EIS.The results show that as the reduction nitrification temperature increases,TiO_(2)in the powder is reduced to TiO and then turns into TiN,and Ti-O bond is gradually replaced by Ti-N bond.In addition,the phase purity and particle size increase,and the pore diameter of the mesoporous first increases and then decreases.When the reduction nitrification temperature is 800℃,the specific surface area of the powder is 41 m^(2)/g,the pore structure is developed,and the average pore diameter is 24 nm,which is conducive to ion transfer and electrochemical performance improvement.At this point,the internal impedance is 0.9Ω.As the current density is 20 mA/g,the specific capacitance is130 F/g.It is worth mentioning that it also can keep nearly 90%of the initial specific capacitance after 1000 cycles under the current density of 50 mA/g.

关 键 词：氮化钛 介孔 还原氮化温度 电化学 超级电容器 

分 类 号：TF12[冶金工程—粉末冶金]