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以工业硼酸、碳黑及TiO_2为原料,经碳热还原法于1650~1800℃合成了纯B_4C及TiB_2含量分别为10~20vol％的B_4C/TiB_2复合粉末,同时确定了原料B/C摩尔比,进行了热力学分析并探讨了球磨工艺、TiB_2的生成对粉末合成的影响.结果表明:原料及产物的B/C摩尔比分别为4.4和3.98~4.03,产物纯度均大于99wt％;湿法球磨可迅速消除粉末的团聚现象,降低原始粉末的粒度,TiB_2颗粒较均匀分散于B_4C中,呈近圆片状,TiB_2的生成有助于降低B_4C/TiB_2的合成温度,由1800℃降至1650℃,并改善了B_4C的颗粒形状,由无定形态变为近球形及条状.“,”B4C and B4C/TiB2 composite powder comprising 10-20vol%TiB2 are synthesized with the temperature of 1650℃ to 1800℃ by carbothermal reduction processing using industrial Boron acid , carbon black and TiO2powder as starting materials, and B/C mole ratio of starting materials is ascertained, thermodynamics temperature of reaction is calculated and the effect of ball milling techniques on the synthesis of powder are discussed. The experimental results indicate that B/C mole ratio of starting materials and synthesized powder are 4.4 and 3.98~4.03 respectively and the pure degree of powder is more than 99wt%; The reuniting and granularity of primordial powder can be eliminated by ball milling techniques. TiB2 grain in the shape of round flake dispersing in the B4C equably can reduce the synthetical temperature of B4C/TiB2, from 1800℃ to 1650℃ and meliorate the shape of B4C grain, from amorphism to similar roundness and strip.