以钛酸四丁酯和二乙烯基苯(DVB)为原料,制备了TiC先驱体,并采用红外(IR)、热重-差热(TGA-DSC)、X射线衍射(XRD)等方法对先驱体和裂解产物进行了表征.结果表明:在283~296℃温度段,由于有机物分解出小分子导致TGA-DSC曲线上大的失重;在445~461 ℃之间,先驱体分解生成TiO_2.更高温度下,TiO_2与DVB裂解生成的碳发生碳热还原反应,生成TiC,且随着裂解温度的提高,TiC的结晶度也随之提高.XRD分析表明随着DVB用量的增加,同一温度下制备的产物结晶度提高.1200 ℃裂解的陶瓷产率均在30%左右.
Titanium carbide precursor was prepared by the reaction of titanium butoxide with divinylbenzene (DVB). The synthesized products and the pyrolysis products were characterized by infrared (IR), thermogravimetric-differential scanning calorimeter (TGA-DSC) and X-ray diffraction (XRD). The results show that the volatilization of small molecules caused the considerable mass loss in the interval of 283~296.76℃. The titanium-containing precursors decomposed between 445℃ and 461℃ and TiO_2 was obtained. At higher temperature, carbothermal reduction process was carried out between TiO_2 and pyrolytic carbon and TiC was got. The crystal degree of TiC is improved with the temperature increasing. The results of XRD indicate that the crystal degree is improved while more DVB was added. The ceramic yields of different reagent ratios are all about 30%.
参考文献
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