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在CaO-CaCl2-NaCl熔盐中,以高钛渣和石墨粉混合物料为阴极,石墨棒为阳极,电解制备出了TiC/SiC纳米级复合粉体。研究了电解时间、槽电压等参数对阴极电解产物的影响。实验结果表明,高钛渣中的钛氧化物在直接电解还原过程中生成了CaTiO3、Ti2O3、TiO等中间产物,CaTiO3的后续电解还原是该过程的控速环节。探讨了CaO在CaCl2-NaCl熔盐中的含量对高钛渣电脱氧过程的影响。结果表明,当熔盐中CaO含量小于1mol%时,添加少量的CaO,可促进CaTiO3的还原;当CaO含量大于2mol%时,过多的CaO则不利于CaTiO3的进一步电解还原,说明CaO的加入对CaTiO3的电脱氧影响显著。分析了高钛渣中Ca、Mg、Al等氧化物的去向。实验结果表明,在高槽压下Ca、Mg、Al氧化物均能被电解还原成相应金属,经过HCl浸出后,上述金属杂质可以除去。研究表明,采用CaCl2-NaCl熔盐中CaO加入量为1mol%、电解温度为900℃、槽电压3.2V,电解时间为6h的高钛渣被完全还原,经HCl浸出后所得产物TiC/SiC复合粉体为纳米级材料,粉体粒径分布均匀,平均值约为50nm。
In CaO-CaCl2-NaCl molten salt, TiC / SiC nano-sized composite powders were electrolytically prepared by using a mixture of high titanium slag and graphite powder as a cathode and a graphite rod as an anode. The effects of electrolysis time, cell voltage and other parameters on cathodic electrolysis products were studied. The experimental results show that the titanium oxide in high titanic slag generates intermediate products of CaTiO3, Ti2O3 and TiO during the process of direct electrolytic reduction. The subsequent electrolytic reduction of CaTiO3 is the speed control step of the process. The effect of CaO content in CaCl2-NaCl molten salt on the electrical deoxygenation of high-titanium slag was discussed. The results show that when the CaO content in the molten salt is less than 1mol%, adding a small amount of CaO can promote the reduction of CaTiO3. When CaO content is more than 2mol%, excess CaO is not conducive to the further electrolytic reduction of CaTiO3, indicating CaO addition The electrical deoxidation of CaTiO3 significantly. The orientation of Ca, Mg, Al and other oxides in high titanium slag was analyzed. The experimental results show that Ca, Mg and Al oxides can be electrolytically reduced to the corresponding metals under high cell pressure. The metal impurities can be removed after HCl leaching. The results show that the TiC / SiC composite obtained after the CaCl2-NaCl molten salt is added with 1 mol% CaO, the electrolysis temperature is 900 ℃, the cell voltage is 3.2V and the electrolysis time is 6h. The powder is a nano-sized material, and the particle size distribution of the powder is even, with an average value of about 50 nm.