<p>The synthesis of high-purity, fine-grained TiB<sub>2</sub> powders <i>via</i> carbothermal reduction is often limited by particle agglomeration and incomplete phase conversion. This work introduces an integrated microwave-assisted strategy combining precursor selection and additive engineering to overcome these issues. Thermodynamic and experimental analyses identify B<sub>4</sub>C as the optimal boron precursor, yielding TiB<sub>2</sub> with enhanced phase purity and fewer intermediates compared to H<sub>3</sub>BO<sub>3</sub>, HBO<sub>2</sub>, and B<sub>2</sub>O<sub>3</sub>. Microstructural control was further achieved <i>via</i> additives: glycerol (1.5 wt pct) served as a steric dispersant, refining particle size to 0.41 <i>μ</i>m, while nano-TiB<sub>2</sub> seeds (1.5 wt pct) reduced the nucleation barrier and promoted epitaxial growth. The seeded approach produced uniform TiB<sub>2</sub> powders (D50 = 0.25 <i>μ</i>m) with ultralow residual C (0.18 pct) and O (0.32 pct) contents. The synergistic use of B<sub>4</sub>C and nano-seeding provides a scalable, efficient route to high-quality TiB<sub>2</sub> powders, demonstrating strong potential for advanced ceramic applications.</p>

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Synergistic B4C and Nano-TiB2 Seed Strategy for Microwave Synthesis of High-Purity, Fine-Grained TiB2 Powders

  • Xin Li,
  • Zhaolei Zhang,
  • Pengfei Shi,
  • Zhenyang Liu,
  • Aichun Dou,
  • Yiran Wei,
  • Aixiong Ge

摘要

The synthesis of high-purity, fine-grained TiB2 powders via carbothermal reduction is often limited by particle agglomeration and incomplete phase conversion. This work introduces an integrated microwave-assisted strategy combining precursor selection and additive engineering to overcome these issues. Thermodynamic and experimental analyses identify B4C as the optimal boron precursor, yielding TiB2 with enhanced phase purity and fewer intermediates compared to H3BO3, HBO2, and B2O3. Microstructural control was further achieved via additives: glycerol (1.5 wt pct) served as a steric dispersant, refining particle size to 0.41 μm, while nano-TiB2 seeds (1.5 wt pct) reduced the nucleation barrier and promoted epitaxial growth. The seeded approach produced uniform TiB2 powders (D50 = 0.25 μm) with ultralow residual C (0.18 pct) and O (0.32 pct) contents. The synergistic use of B4C and nano-seeding provides a scalable, efficient route to high-quality TiB2 powders, demonstrating strong potential for advanced ceramic applications.