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<p>Titanium (Ti) is an indispensable structural and functional material owing to its high specific strength, outstanding corrosion resistance, and favorable biocompatibility. Ti sponge, which serves as the fundamental feedstock for downstream Ti processing, is industrially produced almost exclusively via the magnesium (Mg) thermal reduction route, commonly known as the Kroll process. Despite its long-standing industrial application, the intrinsic reduction mechanism of this process has not yet been fully elucidated, largely due to insufficient knowledge of the intermediate reaction stages. This limitation has impeded a clear interpretation of persistent production issues, including the formation of dense Ti regions and hard cores within the sponge, thereby restricting further improvements in product quality. In this study, the Mg thermal reduction of titanium tetrachloride (TiCl<sub>4</sub>) was systematically investigated with particular emphasis on the formation state and evolutionary behavior of reaction intermediates, as well as the role of reaction conditions in governing their transformation. The experimental results unambiguously identify titanium trichloride (TiCl<sub>3</sub>) and titanium dichloride (TiCl<sub>2</sub>) as the dominant intermediate species along the reduction pathway. Upon contact with molten Mg, TiCl<sub>4</sub> is preferentially reduced to TiCl<sub>3</sub> with the concurrent formation of MgCl<sub>2</sub>. As the resulting molten salt phase continues to interact with excess Mg, TiCl<sub>3</sub> undergoes further reduction to TiCl<sub>2</sub>, which subsequently serves as the direct precursor to metallic Ti under sustained reducing conditions. This study provides direct experimental evidence for the existence and sequential evolution of intermediate products during Ti sponge preparation by Mg thermal reduction. In addition, an isothermal kinetic analysis was conducted to establish the kinetic model governing TiCl<sub>2</sub> formation and to determine the associated activation energy. Collectively, these results offer a quantitative and mechanistic framework for understanding the reduction process, thereby supplying a theoretical basis for process optimization and the improvement of Ti sponge quality.</p>

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Study on the Formation and Evolution of Intermediate Products in the Preparation of Titanium Sponge via the Magnesium Thermal Reduction Process

  • 期刊论文

  • 发表日期：

    2026年3月25日

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  • Shiqing Tian,
  • Jun Li,
  • Kaihua Li,
  • Xin Tian,
  • Jiangqi Zhao,
  • Jinsong Liu,
  • Jiazhen Qiu,
  • Xin Yang,
  • Ying Liu

摘要

Titanium (Ti) is an indispensable structural and functional material owing to its high specific strength, outstanding corrosion resistance, and favorable biocompatibility. Ti sponge, which serves as the fundamental feedstock for downstream Ti processing, is industrially produced almost exclusively via the magnesium (Mg) thermal reduction route, commonly known as the Kroll process. Despite its long-standing industrial application, the intrinsic reduction mechanism of this process has not yet been fully elucidated, largely due to insufficient knowledge of the intermediate reaction stages. This limitation has impeded a clear interpretation of persistent production issues, including the formation of dense Ti regions and hard cores within the sponge, thereby restricting further improvements in product quality. In this study, the Mg thermal reduction of titanium tetrachloride (TiCl4) was systematically investigated with particular emphasis on the formation state and evolutionary behavior of reaction intermediates, as well as the role of reaction conditions in governing their transformation. The experimental results unambiguously identify titanium trichloride (TiCl3) and titanium dichloride (TiCl2) as the dominant intermediate species along the reduction pathway. Upon contact with molten Mg, TiCl4 is preferentially reduced to TiCl3 with the concurrent formation of MgCl2. As the resulting molten salt phase continues to interact with excess Mg, TiCl3 undergoes further reduction to TiCl2, which subsequently serves as the direct precursor to metallic Ti under sustained reducing conditions. This study provides direct experimental evidence for the existence and sequential evolution of intermediate products during Ti sponge preparation by Mg thermal reduction. In addition, an isothermal kinetic analysis was conducted to establish the kinetic model governing TiCl2 formation and to determine the associated activation energy. Collectively, these results offer a quantitative and mechanistic framework for understanding the reduction process, thereby supplying a theoretical basis for process optimization and the improvement of Ti sponge quality.