TiC nanocrystalline powders were synthesized by in-situ carbothermic reduction of Ti-O-C precursor under vacuum atmosphere. And the Ti-O-C precursor was formed by sol-gel method from titanium butyrate (TBOT) and sucrose. To obtain stable sol, TBOT was directly added into mixed solution which contains water, sucrose, acetic acid (AcOH) and acetylacetone (ACAC). This procedure is more convenient and economical because it avoids the use of alcohol which is used as solvent in most reports of alkoxide hydrolysis sol-gel method. TG-DSC, XRD, FTIR and SEM/TEM were employed to analyze and characterize the product during the entire process. The phase composition and crystalline structure parameters of powders with different C/Ti molar ratio were investigated by Rietveld refinement method, and elemental quantitative analysis of the samples were performed. Furthermore, the optimal parameters of carbothermal reduction were obtained and the grain growth mechanism was demonstrated. The results show that TiC nanocrystalline powders (C/Ti molar ratio is 3.5 in the precursor) were synthesized at 1300℃ for 2 h, which have near standard lattice parameter, well crystallinity and fine average grain size (~37.4 nm).

通过在真空气氛下原位碳热还原Ti-OC前驱体合成TiC纳米晶粉末。并通过溶胶-凝胶法由丁酸钛（TBOT）和蔗糖形成Ti-OC前驱体。为了获得稳定的溶胶，将TBOT直接添加到混合溶液中，该混合溶液中含有水，蔗糖，乙酸（AcOH）和乙酰丙酮（ACAC）。该方法更方便，更经济，因为它避免了在大多数醇盐水解溶胶-凝胶法的报道中使用醇作为溶剂。TG-DSC，XRD，FTIR和SEM / TEM在整个过程中用于分析和表征产品。采用Rietveld精制方法研究了不同C / Ti摩尔比的粉末的相组成和晶体结构参数，并对样品进行了元素定量分析。此外，获得了碳热还原的最佳参数，并证明了晶粒长大的机理。结果表明，TiC纳米晶体粉末（前体中C / Ti摩尔比为3.5）在1300℃下合成2 h，具有接近标准的晶格参数，良好的结晶度和精细的平均晶粒尺寸（〜37.4 nm）。