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수소분위기 내 사염화타이타늄의 마그네슘 열환원을 이용한 수소화타이타늄 분말 합성

Synthesis of Titanium Hydride Powder Via Magnesiothermic Reduction of TiCl4 in H2 gas Atmosphere

  • 박성훈 (경북대학교 신소재공학부) ;
  • 이소영 (경북대학교 신소재공학부) ;
  • 이호성 (경북대학교 신소재공학부) ;
  • 강정신 (부산대학교 재료공학부) ;
  • 손호상 (경북대학교 신소재공학부)
  • Sung-Hun Park (School of Materials Science and Engineering, Kyungpook National University) ;
  • So-Yeong Lee (School of Materials Science and Engineering, Kyungpook National University) ;
  • Ho-Seong Lee (School of Materials Science and Engineering, Kyungpook National University) ;
  • Jungshin Kang (School of Materials Science and Engineering, Pusan National University) ;
  • Ho-Sang Sohn (School of Materials Science and Engineering, Kyungpook National University)
  • 투고 : 2023.02.22
  • 심사 : 2023.04.06
  • 발행 : 2023.04.30

초록

본 연구에서는 수소분위기 내 사염화타이타늄의 마그네슘 열환원을 이용한 수소화타이타늄 분말 합성 과정 중 온도 및 소결 조건에 따른 분말 특성 변화를 조사하였다. 수소화타이타늄 생성에 미치는 온도의 영향을 검토하기 위해 1023~1123 K의 1 atm 수소분위기에서 약 30 분간 사염화타이타늄과 마그네슘을 반응시켰다. 환원반응 후 생성된 수소화타이타늄 분말의 소결이 진행되도록 0~120 분간 환원반응 온도를 유지시켰으며, 반응 종료 후 회수된 생성물의 산소농도를 분석하였다. 실험결과, 1023 K에서는 TiH1.924 이 생성되었으나, 1073K 및 1123 K에서는 TiH1.924와 TiH1.5의 혼합물이 생성되었다. 또한, 반응온도가 높을수록 생성된 수소화타이타늄 분말의 수소농도는 감소하였다. 반응온도 및 소결시간이 증가할수록 분말의 산소농도는 감소하였으며, 이는 분말의 비표면적 감소에 기인하였다. 반응온도 1073 K 및 소결시간 120 분 실험조건에서 최저 산소농도 0.246 mass%인 TiH1.924와 TiH1.5의 혼합물이 제조되었다.

A novel method for the synthesis of titanium hydride powder from titanium tetrachloride via the magnesiothermic reduction in an hydrogen gas atmosphere was investigated. To examine the influence of temperature on the formation of titanium hydride, the reduction was conducted at 1023~1123 K under 1 atm of hydrogen gas atmosphere for approximately 30 min. Subsequently, the titanium hydride powder was sintered by maintaining the temperature for 0~120 min, and the decrease in the oxygen concentration of the powder was investigated. The experimental results showed that TiH1.924 was produced at 1023 K, whereas mixtures of TiH1.924 and TiH1.5 were produced at 1073 K and 1123 K. In addition, the hydrogen concentration in the powder decreased with increasing temperature. The concentration of oxygen in the powder decreased with increasing temperature and sintering time owing to the decrease in the specific surface area of the powder. The minimum concentration of oxygen was 0.246 mass% when the mixture of TiH1.924 and TiH1.5 was obtained at 1073 K and a sintering time of 120 min.

키워드

과제정보

The authors are grateful to all members of the scientific instruments center of Kyungpook National University for their technical assistance. The authors are also grateful to all members of the industrial-academic cooperation group of Kyungpook National University for their operational support.

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