采用熔盐电脱氧法,以石墨固定的氧化物粉末为阴极,石墨棒为阳极,NaCl-CaCl2混合熔盐为电解质,石墨坩埚为电解槽在8OO℃低温熔盐中制备金属Ti.进行不同电解时间的电脱氧实验,研究了阴极产物.分别以石墨和钼为工作电极、对电极和参比电极,对TiO 2电脱氧还原的过程进行了动力学研究,测定了循环伏安曲线。结果表明:未烧结TiO2粉末经过4Oh的恒压电解后,TiO2还原成Ti;石墨电极虽然有较宽的电化学窗口,但是电极活性高、表面积大,不能在高温条件下作为CV曲线电极材料使用;钼的电化学性质稳定,是比较理想的电极材料;二氧化钛的电化学还原分四步进行:TiO2/Ti3O5,Ti3Os/Ti2O3,CaTi2O4/TiO,TiO/T,前两步都伴随CaTiOz与CaTi2O4的自发形成。
The method of electro-deoxidation in molten salts was adopted to to prepare Ti with unsintered Ti02 powder loaded in the graphite capsule, and the graphite crucible was used as electrolytic cell at 800 IC. In this paper, different electro-deoxidation time were taken as to analyse the cathode products. During the CV experiment, the graphite and molybdenum was individually used as the work electrode material, counter electrode material and reference electrode material for the Studies on Kinetics of Ti02 reduction and the CV curves were recorded by AutoLab PGSTAT 320 N potentiostat. Result showed that metal Ti was gotted with unsintered Ti02 powder as raw material after 40 h constant voltage electrolysis, and graphite electrode was not a good choice to used as electrode material in the CV experiment at high temperature for its high electrode activity and large surface area, although there were a wide electrochemical window potential, while the molybdenum was quite an ideal choice for its stable electrochemical properties. The Ti02 electrochemical reduction steps contain four steps: TiO2/Ti3Os, Ti3Os/Ti203, CaTi2Oa/TiO, TiO/T during; the former two steps CaTi03 and ~aTi20a spontaneously formed.