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2023 Vol.32, Issue 2 Preview Page

Research Paper

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

수소분위기 내 사염화타이타늄의 마그네슘 열환원을 이용한 수소화타이타늄 분말 합성

Sung-Hun Park12†
,
So-Yeong Lee1†
,
Ho-Seong Lee1
,
Jungshin Kang3
,
Ho-Sang Sohn1*
박 성훈12†
,
이 소영1†
,
이 호성1
,
강 정신3
,
손 호상1*
1School of Materials Science and Engineering, Kyungpook National University, 80 Daehak-ro, Buk-gu, Daegu 41566, Republic of Korea
2Korea Institute of Geoscience and Mineral Resources, 124 Gwahak-ro, Yuseong-gu, Daejeon 34132, Republic of Korea
3School of Materials Science and Engineering, Pusan National University, 2, Busandaehak-ro 63beon-gil, Geumjeong-gu, Busan 46241, Republic of Korea
1경북대학교 신소재공학부
2한국지질자원연구원 자원활용연구본부
3부산대학교 재료공학부
*Corresponding Author
†Both authors contributed equally to this work.
30 April 2023. pp. 19-32
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Abstract

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.

Keywords
titanium hydride
titanium powder
titanium tetrachloride
magnesiothermic reduction
hydrogen

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, 1073 K 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.

키워드
수소화타이타늄
타이타늄 분말
사염화타이타늄
마그네슘 열환원
수소
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Information
  • Publisher :The Korean Institute of Resources Recycling
  • Publisher(Ko) :한국자원리싸이클링학회
  • Journal Title :Resources Recycling
  • Journal Title(Ko) :자원리싸이클링
  • Volume : 32
  • No :2
  • Pages :19-32
  • Received Date : 2023-02-22
  • Revised Date : 2023-03-26; 2023-04-05
  • Accepted Date : 2023-04-06
  • DOI :https://doi.org/10.7844/kirr.2023.32.2.19
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