1. Synthesis and formation mechanism of HfB2 ultrafine powders with low oxygen via flocculating settling assisted process and carbo/borothermal reduction.
- Author
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Wang, Zhen, Cheng, Yuan, Li, Kewei, Wang, Tianxu, Hu, Mengen, Zheng, Chunxue, Li, Xinyang, Huang, Zhulin, Hu, Xiaoye, Li, Yue, and Zhang, Xinghong
- Subjects
POWDERS ,ECONOMIC lot size ,CHLORINE ,SODIUM borohydride ,COMPLEXATION reactions ,SPECIFIC gravity ,MASS production ,TRANSITION metals - Abstract
• A liquid-phase flocculating settling assisted carbothermal reduction method to prepare ultrafine powders of single-phase HfB 2 with low oxygen and carbon content. • Manuscript proposes a new reaction path that the HfC is not an intermediate product of HfB 2 powder at lower temperature, but by-products at high temperature in the carbothermal reduction process. • The flocculating settling method can be extended to the synthesis of other high-purity and ultrafine group IV and v transition metal (Ti, Zr, Ta, Nb) diboride powders. • The work has proved to be applicable to the mass production of kilogram grade ultrafine HfB 2 powder with high purity. In this study, ultrafine HfB 2 powders with low oxygen were synthesized by a flocculating settling process which yielded ceramic precursors and subsequent carbo/borothermal reduction of the precursors. The liquid phase precursor method can achieve uniform mixing of components at the molecular level through multiple complexation reactions, and then realize the carbo/borothermal reduction reaction at a lower temperature to obtain ultrapure HfB 2 powders. The as-resulted quasi-spherical HfB 2 powders under the optimum conditions (atomic molar ratio M:B:C = 1:2.8:10) calcined at 1500 °C for 1 h have an average particle size of 205 nm and an oxygen content of 0.097 wt.%. Detailed analysis of the phase evolution of precursors shows that the formation of HfB 2 particles is a mass diffusion mode from the external to internal HfO 2 cores. We reveal that below 1300 °C, HfC is not an intermediate product of HfB 2 powder during the transition of precursors. Instead, HfC was formed as a by-product at high temperatures in the carbo/borothermal reduction process. The proposed formation mechanism of HfB 2 is completely different from the traditional two-step transformation method. After the sintering of the ultrafine powders, the HfB 2 ceramics show a relative density of 96.1% and superior mechanical properties compared to other works. Furthermore, by simply replacing the initial metal source, chlorinated group IV and V transitional metals (Ti, Zr, Ta, Nb) can also convert into high-purity and ultrafine diborides. This work shows that flocculating settling assisted carbo/borothermal reduction has potential in lot size production of various high-purity and ultrafine boride powders. [Display omitted] [ABSTRACT FROM AUTHOR]
- Published
- 2023
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