A study on the growth mechanism of rutile single crystal by skull melting method and conditions of RF generator

스컬용융법에 의한 루틸 단결정 성장메커니즘과 RE generator 조건에 관한 연구

  • Seok jeong-Won (Department of Gemological Engineering, Dongshin University, Ceramic Processing Research Center(CPRC)) ;
  • Choi Jong-Koen (Department of Gemological Engineering, Dongshin University, Ceramic Processing Research Center(CPRC))
  • 석정원 (동신대학교 보석공학과, 세라믹공정연구센터) ;
  • 최종건 (동신대학교 보석공학과, 세라믹공정연구센터)
  • Published : 2005.10.01

Abstract

Ingots of rutile single crystals were grown by the skull melting method, and their characteristics were compared in terms of melt-dwelling time for each melt. The method is based on direct inductive heating of an electrically conducted melt by an alternating RF field, and the heating is performed by absorption of RF energy. $TiO_2$ is an insulator at room temperature but its electric conductivity increases elevated temperature. Therefore, titanium metal ring(outside diameter : 6cm, inside diameter : 4cm, thickness 0.2cm) was embedded into $TiO_2$, powder (anatase phase, CERAC, 3N) for initial RF induction heating. Important factors of the skull melting method are electric resistivity of materials at their melting point, working frequency of RF generator and cold crucible size. In this study, electric resitivity of $TiO_2$, $(10^{-2}\~10^{-1}\;{\Omega}{\cdot}m)$ at its melting point was estimated by compairing the electric resitivities of alumina and zirconia. Inner diameter and height of the cold crucible was 11 and 14cm, respectively, which were determined by considering of the Penetration depth $(0.36\~1.13cm)$ and the frequency of RF generator.

스컬용융법에 의해 루틸 단결정들을 성장시켰으며, 서로 다른 융액의 유지시간에 따른 ingot의 특성을 비교하였다. 스컬용융법은 교류전자기장(RF)에 의해 전기가 흐르는 융액의 직접유도가열에 근거하며, 가열은 RF 에너지의 흡수로 실행된다. $TiO_2$는 상온에서는 부도체이지만 온도가 올라갈수록 전기 전도성이 증가한다. 따라서, 초기 RF 유도가열을 위해 티타늄 금속 링(외경 : 6cm, 내경 : 4cm, 두께 : 0.2cm)을 $TiO_2$ 분말(아나타제상, CERAC, 3N)내부에 묻었다. 스컬용융법에 의한 산화물 용융에서 매우 중요한 것은 융점에서의 전기 저항 값, RF generator의 주파수 그리고 냉각도가니 크기이다. 본 연구에서는, $TiO_2$의 융점에서의 전기저항$(10^{-2}\~10^{-1}\;{\Omega}{\cdot}m)$은 알루미나$(10^{-1}\;{\Omega}{\cdot}m)$의 지르코니아$(10^{-3}\;{\Omega}{\cdot}m)$의 전기저항 데이터를 바탕으로 추정하였다. 냉각도가니의 내부직경은 11cm, 높이는 14cm였으며, 이것은 침투깊이$(0.36\~1.13cm)$와 RF generator 주파수를 고려하여 결정하였다

Keywords

References

  1. J.K. Park, K.B. Shim, K.H. Auh and I. Tanaka, 'Growth of $TiO_2$ (rutile) single crystal by FZ method under high oxygen pressure', J. the Korean Crystal Growth and Crystal Technology 11(3) (2001) 85
  2. H. Machida and T. Fukuda, 'Difficulties encountered during the Czochralski growth of $TiO_2$ single crystals', J. of Crystal Growth 112 (1991) 835 https://doi.org/10.1016/0022-0248(91)90142-R
  3. H. Machida, K. Hoshikawa and T. Fukuda, 'Unstable forming of rutile crystal grown by EFG method', Pro. the 12th KACG tech. meeting and the 4th Korea-Japan EMGS (1997) 159
  4. M. Higuchi, K. Hatta, J. Takahashi, K. Kodaira, H. Kaneda and J. Saito, 'Floating-zone growth of rutile single crystal inclined at $48^{\circ}$ to the c-axis', J. Crystal Growth 208 (2000) 501
  5. J.K. Park, K.H. Kim, I. Tanaka and K.B. Shim, 'Characteristics of rutile single crystals grown under two different oxygen partial pressures', J. Crystal Growth 268 (2004) 103 https://doi.org/10.1016/j.jcrysgro.2004.04.105
  6. M. Higuchi, T. Togi and K. Kodaira, 'Growth of rutile single crystals by the pulling-down method', J. Crystal Growth 230 (1999) 450
  7. J.W. Seok and J.K. Choi, 'A study on the growth of rutile single crystal by skull melting method', J. the Korean Crystal Growth and Crystal Technology 14(6) (2004) 262
  8. C. Gross, W. Assmus, A. Muiznieks, A. MUhlbauer, C. Stenzel and O. Schulz, 'Possible use of Skull melting under rnicrogravity', J. Crystal Growth 198/199 (1999) 190
  9. C. Gross, W. Assmus, A. Muiznieks, G. Raming, A. M?hlbauer and C. Stenzel, 'Power consumption of skull melting, Part I : Analytical Aspects and Experiments', Cryst. Res. Technol. 34 (1999) 324
  10. R.F. Sekerka, R.A. Hartzell and B.J. Farr, 'Instability phenomena during the RF heating and melting of ceramics', J. Crystal Growth 50 (1980) 787
  11. V.I. Aleksandrov, V.V. Osiko, A.M. Prokhorov and V.M. Tatarintsev, 'Synthesis and crystal growth of refractory materials by RF melting in a cold container', Current Topics in Meterials Science 1(1978) 431