A novel technology was proposed to fabricate non-stoichiometric titanium dioxide (TiO_2−x) compacts in one-step thermal process by in-situ reduction of rutile TiO₂ with carbon powder via spark plasma sintering (SPS). The rutile TiO₂ powder was reduced with three different carbon powders for comparison, and the effect of the sintering conditions on the fabricated compacts was investigated. It is found that the in-situ reduction of rutile TiO₂ with charcoal powder was easily achieved at a low pressure and high temperature (above 1473 K). Besides, the design of dynamic sintering pressure during SPS was proposed, and the results suggest that the dynamic sintering pressure contributes to the reduction of TiO₂ and the fabrication of the compacts with high-density. In addition, density methods, X-ray diffraction, scanning electronic microscopy and laser micro-Raman spectrometer were performed to analyze the sintering sates, microstructures, crystal structures and phase distributions. The results show that a stable sintering environment without an increase in the pressure caused by reaction gas is a crucial role for the reduction of TiO₂ and the TiO_2−x fabrication, even the formation of Magnéli phases Ti_nO_2n−1. Finer charcoal powder is more conducive to fabricating the compact with a single Magnéli phase Ti₆O₁₁. It is expected to achieve a new breakthrough in fabrication method of the non-stoichiometric TiO₂ by a safe and economically viable method.

提出了一种新技术，通过放电等离子体烧结 (SPS) 用碳粉原位还原金红石 TiO _{2 ，}以一步热工艺制造非化学计量二氧化钛 (TiO _2-x ) 压块。用三种不同的碳粉还原金红石 TiO ₂粉末以进行比较，并研究了烧结条件对制造的压块的影响。发现木炭粉原位还原金红石TiO ₂很容易在低压和高温（1473 K以上）下实现。此外，提出了SPS过程中动态烧结压力的设计，结果表明动态烧结压力有助于TiO ₂的还原。以及高密度压块的制造。此外，通过密度法、X射线衍射、扫描电子显微镜和激光显微拉曼光谱仪对烧结态、微观结构、晶体结构和相分布进行了分析。结果表明，稳定的烧结环境没有由反应气体引起的压力增加，对于还原 TiO ₂和制备TiO _2-x，甚至形成 Magnéli 相 Ti _n O _{2n-1 都}至关重要。更细的木炭粉更有利于制造具有单一 Magnéli 相 Ti ₆ O _{11 的}压块. 有望通过一种安全、经济可行的方法在非化学计量TiO ₂的制备方法上取得新的突破。