数控焰熔法生长金红石单晶体的气体参数优化试验研究
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摘要
使用数控焰熔法晶体生长炉和三管燃烧器进行了金红石单晶体的生长工艺实验研究。研究表明,在3个气体参数中,内氧是基础。当内氧流量小于特征值O_(in)(min)=6.6 L/min或大于特征值O_(in)(max)=7.1 L/min时,晶体生长或易于发生熔体流淌,或不易扩肩,生长过程被迫中止,晶体很难生长成为大尺寸晶体;当内氧流量大于6.6 L/min而小于7.1 L/min时,生长过程稳定,能够生长成为大尺寸晶体。当内氧流量为7 L/min时生长出了直径30 mm、长度45 mm的金红石单晶体。通过能谱仪、X射线衍射仪(XRD)和拉曼光谱仪对晶体的组成、结构和键的结构进行表征,表明该晶体为典型的金红石单晶体,生长方向是[110]。
The growth process of rutile single crystal was studied by numerical control flame melting crystal growing furnace and three-tube burner. It is shown that internal oxygen was the basis of the three gas parameters. When the internal oxygen flow was less than the characteristic value O_(in)(min) of 6.6 L/min or greater than the characteristic value(O_(in)(max) of 7.1 L/min, the crystal growth was prone to melt flow or not easy to expand, and the growth process was forced to stop, so the crystal was difficult to grow into large-size crystals. When the internal oxygen flow was larger than 6.6 L/min and smaller than 7.1 L/min, the growth process was stable and could grow into large-size crystals. When the internal oxygen flow was 7 L/min, rutile single crystal with a diameter of 30 mm and a length of 45 mm was grown. The composition, structure and bond structure of the crystal were characterized by energy spectrometer, X-ray diffraction(XRD) and Raman spectrometer, indicating that the crystal was a typical single crystal of rutile, and the growth direction was [110].
The growth process of rutile single crystal was studied by numerical control flame melting crystal growing furnace and three-tube burner. It is shown that internal oxygen was the basis of the three gas parameters. When the internal oxygen flow was less than the characteristic value O_(in)(min) of 6.6 L/min or greater than the characteristic value(O_(in)(max) of 7.1 L/min, the crystal growth was prone to melt flow or not easy to expand, and the growth process was forced to stop, so the crystal was difficult to grow into large-size crystals. When the internal oxygen flow was larger than 6.6 L/min and smaller than 7.1 L/min, the growth process was stable and could grow into large-size crystals. When the internal oxygen flow was 7 L/min, rutile single crystal with a diameter of 30 mm and a length of 45 mm was grown. The composition, structure and bond structure of the crystal were characterized by energy spectrometer, X-ray diffraction(XRD) and Raman spectrometer, indicating that the crystal was a typical single crystal of rutile, and the growth direction was [110].
引文
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[15] Xiao Ping,You Jinglin,Jiang Guochang,et al.Structure of titanium oxide and its Raman spectrum characterization[J].Spectroscopy and Spectral Analysis,2007,27(5):936-939(in Chinese).肖萍,尤静林,蒋国昌,等.钛氧化物结构及其拉曼光谱表征[J].光谱学与光谱分析,2007,27(5):936-939.
[2] Koohpayeh S M,Fort D,Abell J S.Some observations on the growth of rutile single crystals using the optical floating zone method[J].J Cryst Growth,2005,282(1-2):190-198.
[3] Park J K,Shim K B,Auh K H,et al.The growth of TiO2 (rutile) single crystals using the FZ method under high oxygen pressure[J].J Cryst Growth,2002,237(1):730-734.
[4] Cheng Gang.Study on the growth and radiation properties of rutile by flame melting [D].Chengdu:Sichuan University,2003(in Chinese).承刚.金红石的焰熔法生长及其辐射物性研究[D].成都:四川大学,2003.
[5] Bi Xiaoguo,Liu Xudong,Niu Wei.Flame-fusion growth of rutile single crystal [J].Advanced Materials Research,2012,535-537(9):2571-2576.
[6] Scheel H J.Crystal growth technology CGT for energy:saving energy and renewable energy [J].J Cryst Growth,2005,275(1-2):331-337.
[7] Liu Xudong,Bi Xiaoguo,Tang Jian,et al.Study on temperature distribution in combustion chamber of single crystal grown by flame melting[J].Journal of Shenyang Institute of Engineering(Natural Science),2014,10(4):378-381(in Chinese).刘旭东,毕孝国,唐坚,等.焰熔法生长单晶体燃烧室内温度分布研究[J].沈阳工程学院学报(自然科学版),2014,10(4):378-381.
[8] Scheel H J.Historical aspects of crystal growth technology[J].J Cryst Growth,2000,211(1):1-12.
[9] Bi Xiaoguo.Preparation of single crystal of rutile (TiO2),strontium titanate (SrTiO3) and strontium niobate (Nb∶SrTiO3) [D].Shenyang:Northeast University,2003(in Chinese).毕孝国.金红石(TiO2)、钛酸锶(SrTiO3)与加铌钛酸锶(Nb∶SrTiO3)单晶体制备研究[D].沈阳:东北大学,2003.
[10] Gu O,Ar G.The effects of O deficiency on the electronic structure of rutile TiO2[J].J Phys Chem Solids,2006,68(3):324-330.
[11] Park J K,Kim K H,Tanaka I ,et al.Characteristics of rutile single crystals under two different oxygen partial pressures[J].J Cryst Growth,2004,268(1-2):103-107.
[12] Bi Xiaoguo,Xiu Zhimeng,Ma Weimin,et al.Effects of growth atmosphere and growth rate on the growth of single crystal of rutile (TiO2)[J].Journal of Synthetic Crystals,2004,33(4):657-661(in Chinese).毕孝国,修稚萌,马伟民,等.生长气氛和速度在金红石(TiO2)单晶体生长中的作用研究[J].人工晶体学报,2004,33(4):657-661.
[13] Donnet J B,Oulanti H,Schmitt M,et al.Sythesis of large single crystal diamond using combustion-flame method[J].Carbon,2006,44(2):374-380.
[14] Liu Xudong,Cai Yunping,Sun Xudong.Numerical simulation of indoor temperature distribution of flame-fused single crystal growth of rutile[J].Journal of Synthetic Crystals,2016,45(1):138-145(in Chinese).刘旭东,蔡云平,孙旭东.焰熔法生长金红石单晶体生长室内温度分布的数值模拟[J].人工晶体学报,2016,45(1):138-145.
[15] Xiao Ping,You Jinglin,Jiang Guochang,et al.Structure of titanium oxide and its Raman spectrum characterization[J].Spectroscopy and Spectral Analysis,2007,27(5):936-939(in Chinese).肖萍,尤静林,蒋国昌,等.钛氧化物结构及其拉曼光谱表征[J].光谱学与光谱分析,2007,27(5):936-939.