Ti_2SC粉体的快速合成

Rapid Synthesis of Ti_2SC Powder

以TiS_2、Ti、石墨粉（C）为原料,在200~1 100℃,用微波混合加热法合成了Ti_2SC陶瓷粉体。探讨了反应温度对Ti_2SC制备的影响,并在1 000~1 400℃与无压烧结法进行了对比研究。采用XRD、SEM、DSC和热力学计算对样品的物相、形貌和反应机理进行分析。结果表明：利用无压烧结到1 400℃,保温15 min,样品中主相是C,只合成了少量目标相Ti_2SC;而用微波混合加热到400℃时,样品中主相为Ti_2SC,含有大量的C;升温到800℃,目标相衍射峰增强,C衍射峰减弱;在1 100℃,保温3 min,合成了单相Ti_2SC粉体材料,其颗粒粒径范围为2~5μm。在TiS_2-Ti-C体系中,400℃以下,TiS_2和Ti反应生成Ti-S化合物;400℃及以上,Ti、C和Ti-S化合物反应生成Ti_2SC。

Highly pure TizSC powder was synthesized by microwave hybrid heating using TiS2, Ti and graphite powder （ C ） as raw materials in the temperature range of 200 - 1 100 ℃. The effect of sintering temperature on the synthesis of Ti2SC was studied. For comparison, pressureless sintering （PLS） was used to synthesize Ti2SC powder from 1 000℃ to 1 400 ℃. The phase composition, morphology and reaction mechanism of the samples were characterized by XRD, SEM, DSC and thermodynamics. The results indicate that the main phase of the sample is graphite and there is a small amount of TizSC formed at 1 400 ℃ for 15 rain by pressureless sintering. However, by microwave hybrid heating,Ti2SC phase is a major phase and there is a large amount of graphite in the sample. The peak of Ti2SC phase became strong End that of graphite became weak at 800 ℃. At 1 100 ℃ ,single- phase Ti2 SC powder forms with an average size of 2 -5 μm. In TiS2-Ti-C system, TiS2reacts with Ti to form Ti-S compounds at temperature below 400 ℃, and Ti-S compounds reacts with Ti and graphite to produce Ti2 SC at temperature greater than or equal to 400 ℃.