<p>High-quality Ti(C<sub><i>x</i></sub>, N<sub>1-<i>x</i></sub>) powders with low oxygen content were synthesized via high-temperature carbothermal reduction–nitridation (CRN) of TiO<sub>2</sub> combined with a subsequent Ca treatment. The effects of CRN temperature, N<sub>2</sub> partial pressure, and C/TiO<sub>2</sub> molar ratio on C/N ratio, residual oxygen content, microstructure, and grain size were investigated using X-ray diffraction (XRD), C-S and O-N-H analyses, and field-emission scanning electron microscopy (FE-SEM). The obtained powders presented high purity, homogeneous morphology, excellent crystallinity, and superior dispersibility. With increasing CRN temperature and C/TiO<sub>2</sub> ratio, as well as decreasing N<sub>2</sub> partial pressure, there is an increase in C/N ratio. Meanwhile, the residual oxygen content decreased with increasing CRN temperature and C/TiO<sub>2</sub> ratio, with powders synthesized at 1600°C and 1650°C exhibiting oxygen contents below 0.5 wt.%. The mean grain size increased with elevated CRN temperature and reduced N<sub>2</sub> partial pressure, from 0.80 ± 0.32&#xa0;<i>μ</i>m to 1.12 ± 0.31&#xa0;<i>μ</i>m and from 0.93 ± 0.32 to 1.07 ± 0.34&#xa0;<i>μ</i>m, respectively, while decreased from 0.93 ± 0.32 to 0.76 ± 0.40&#xa0;<i>μ</i>m with higher C/TiO<sub>2</sub> ratios. At a C/TiO<sub>2</sub> ratio of 3.5, the powder displayed a bimodal grain size distribution with peaks at approximately 0.39&#xa0;<i>μ</i>m and 0.97&#xa0;<i>μ</i>m.</p>

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Controlled Preparation of High-Quality Ti(Cx, N1-x) Powders with Low Oxygen Content

  • Xiao-Dong Kang,
  • Guo-Hua Zhang

摘要

High-quality Ti(Cx, N1-x) powders with low oxygen content were synthesized via high-temperature carbothermal reduction–nitridation (CRN) of TiO2 combined with a subsequent Ca treatment. The effects of CRN temperature, N2 partial pressure, and C/TiO2 molar ratio on C/N ratio, residual oxygen content, microstructure, and grain size were investigated using X-ray diffraction (XRD), C-S and O-N-H analyses, and field-emission scanning electron microscopy (FE-SEM). The obtained powders presented high purity, homogeneous morphology, excellent crystallinity, and superior dispersibility. With increasing CRN temperature and C/TiO2 ratio, as well as decreasing N2 partial pressure, there is an increase in C/N ratio. Meanwhile, the residual oxygen content decreased with increasing CRN temperature and C/TiO2 ratio, with powders synthesized at 1600°C and 1650°C exhibiting oxygen contents below 0.5 wt.%. The mean grain size increased with elevated CRN temperature and reduced N2 partial pressure, from 0.80 ± 0.32 μm to 1.12 ± 0.31 μm and from 0.93 ± 0.32 to 1.07 ± 0.34 μm, respectively, while decreased from 0.93 ± 0.32 to 0.76 ± 0.40 μm with higher C/TiO2 ratios. At a C/TiO2 ratio of 3.5, the powder displayed a bimodal grain size distribution with peaks at approximately 0.39 μm and 0.97 μm.