铝热还原TiO2制备Magnéli相低价钛氧化物工艺及过程机制研究  

Process Parameters and Mechanism of Magnéli Phase Titanium Suboxide Prepared by Aluminothermy Reduction of Titanium Dioxide

作　　者：李军[1,2] 鲁雄刚 杨绍利[2] 吴恩辉 侯静 李重河 Li Jun;Lu Xionggang;Yang Shaoli;Wu Enhui;Hou Jing;Li Chonghe(National Key Laboratory of High-Quality Special Steel Metallurgy and Preparation by the Province and the Min- istry, Shanghai University, Shanghai 200072, China;Panxi Scientific and Technological Innovation Center, Panzhihua University, Panzhihua 617000, China)

机构地区：[1]上海大学省部共建高品质特殊钢冶金与制备国家重点实验室,上海200072 [2]攀枝花学院攀西科技创新中心,四川攀枝花617000

出　　处：《稀有金属》2018年第6期627-633,共7页Chinese Journal of Rare Metals

基　　金：国家重点基础研发展计划项目(2014CB643403);四川省科技支撑计划资助项目(2017JY0117);国家级大学生创新创业计划项目(201511360040)资助

摘　　要：Magnéli相（TinO2n-1）（4〈n〈10）低价钛氧化物材料具有导电性好、可见光响应强、耐磨、优异的耐腐蚀性能等,被广泛应用于制备电池、惰性电极及光催化降解材料。在空气气氛下利用铝还原锐钛矿相TiO2制备Magnéli相低价钛氧化物材料,研究了不同焙烧温度、焙烧时间和配铝量等工艺参数对制备黑色Magnéli相低价钛氧化物复合材料相变过程的影响,并采用X射线衍射（XRD）、拉曼光谱（Raman）、X射线光电子能谱（XPS）、扫描电子显微镜（SEM）等分析手段对制备出的Magnéli相低价氧化物复合材料的物相组成变化及微观组织形貌进行表征,结果表明：不同焙烧温度和焙烧时间下制备的样品主要物相为Ti9O17,Ti8O15,Ti7O13,Ti4O7,随着焙烧温度的升高和焙烧时间的延长,还原程度不断加深,TinO2n-1中的n值不断降低。制备的Magnéli相低价氧化物材料呈颗粒状,粒径200～400 nm左右。通过稀盐酸浸出,可以将Magnéli相材料中过剩的铝除去得到较为纯净的Magnéli相TinO2n-1材料。Magnéli phase（TinO2n-1）（4 〈 n 〈 10） titanium suboxide was widely adopted in battery,inertelectrode and photocatalytic degradation material because of their many excellent properties such as high electronic conductivity,strong visible light absorption,wear-resisting property,superior corrosion resistance. Calcination temperature,calcination time and the amount of aluminum of preparation of black magnéli phase titanium suboxide in air were researched. Characterization methods of X-ray diffraction（XRD）,Raman spectroscopy,X-ray photoelectron spectroscopy（XPS）,scanning microscopy electron microscope（SEM） were used to determine the major phase compositions change and microstructure of sample. The results showed that main phase of the as-prepared samples under different calcination temperature and calcination time were Ti9O17,Ti8O15,Ti7O13,Ti4O7,the degree of reduction was deepening and the value of n in TinO2n-1 decreased with the increase of calcination temperature and the prolongation of calcination time. Particle size of sample was about 200 ～ 400 nm. Pure magnéli-phase titanium suboxides could be obtained when dissolved in hydrochloric acid and filtered.

关 键 词：铝热还原 TinO2n-1 Magnéli相 

分 类 号：TK91[动力工程及工程热物理]