用于焰熔法金红石单晶体生长的微米级TiO_2粉体制备与表征
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摘要
以提纯后的TiCl_4为原料,氨水作为形核剂,PEG400为分散剂,制备出高纯TiO_2粉体。采用ICP、XRD、SEM等手段对所得样品进行分析。结果表明,TiCl_4溶液经60℃水浴2h后加入含15mL PEG400的氨水溶液,在900℃下煅烧3h,可以制备出晶型为单一金红石相,平均粒度为70μm,形貌为近球形,流动性良好的高纯TiO2粉体。
The high purity TiO_2 powders were prepared using purified TiCl_4 as raw materials,PEG400 as dispersant and ammonia as nucleation agent.The obtained samples were analyzed by ICP,XRD and SEM.The results indicated that after 60℃ water bath 2 h,the ammonia solution containing 15 mL PEG400 was joined into TiCl_4 solution,and then,calcined under 900 ℃,the high purity TiO_2 powders with rutile crystalline phase were obtained.The average particle size of the powders was 70μm,the morphology was nearly spherical,and the liquidity was good.
The high purity TiO_2 powders were prepared using purified TiCl_4 as raw materials,PEG400 as dispersant and ammonia as nucleation agent.The obtained samples were analyzed by ICP,XRD and SEM.The results indicated that after 60℃ water bath 2 h,the ammonia solution containing 15 mL PEG400 was joined into TiCl_4 solution,and then,calcined under 900 ℃,the high purity TiO_2 powders with rutile crystalline phase were obtained.The average particle size of the powders was 70μm,the morphology was nearly spherical,and the liquidity was good.
引文
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[11]Wu Nan,Ma Weimin,Bi Xiaoguo,et al.Preparation of high-purity TiO2ultra-fine powders[J].Journal of Synthetic Crystals,2012,41(2):485-490(in Chinese).吴南,马伟民,毕孝国,等.高纯TiO2超微粉体的制备[J].人工晶体学报,2012,41(2):485-490.
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[13]Bi Xiaoguo,Liu Xudong,Li Qiang,et al.Preparation of titanium dioxide powder by phase transfer method[J].Journal of Shenyang Institute of Engineering(Natural Science),2012,8(4):362-365(in Chinese).毕孝国,刘旭东,李强,等.相转移法制备二氧化钛粉体的工艺研究[J].沈阳工程学院学报(自然科学版),2012,8(4):362-365.
[2]Bi Xiaoguo,Xiu Zhimeng,Ma Weimin.Study on growth of rutile(TiO2)single crystals[J].Journal of Northeastern University(Natural Science),2004,25(10):977-979(in Chinese).毕孝国,修稚萌,马伟民,等.金红石(TiO2)单晶体的生长研究[J].东北大学学报(自然科学版),2004,25(10):977-979.
[3]Machide H,Fukuda T.Difficulties encountered during the czochralski growth of TiO2 single crystals[J].J Crystal Growth,1991,112(4):835-837.
[4]Tang Jian,Bi Xiaoguo,Liu Xudong,et al.Current situation of development of preparation method of rutile single crystal[J].Journal of Shenyang Normal University(Natural Science Edition)2017,35(1):43-46(in Chinese).唐坚,毕孝国,刘旭东,等.金红石单晶体制备方法发展现状[J].沈阳师范大学学报(自然科学版),2017,35(1):43-46.
[5]Satoshi Watauchi,Md Abdur Razzaque Sarker,Masanori Nagao,et al.Crystal growth of rutile by tilting-mirrortype floating zone method[J].Journal of Crystal Growth,2012,360(7):105-110.
[6]Koohpayeh S M,Fort D,Abell J S.Some observations on the growth of rutile single crystals using the optical floating zone method[J].Journal of Crystal Growth,2005,282(1):190-198.
[7]Higuchi M,Hosokawa T,Kimura S.Growth of rutile single crystals by floating zone method[J].Journal of Crystal Growth,1991,112(4):354-358.
[8]Watauchi S,Tanaka I,Havashi K,et al.Crystal growth of Ca12Al14O33by the floating zone method[J].J Crystal Growth,2002,237-239(01):801-805.
[9]Liu Xudong,Bi Xiaoguo,Sun Xudong.Numerical simulation of temperature distribution in growth chamber for preparation of strontium titanate crystal with flame fusion method[J].Materials Review,2017,31(16):138-143(in Chinese).刘旭东,毕孝国,孙旭东.焰熔法生长钛酸锶单晶体生长室内温度分布的数值模拟[J].材料导报,2017,31(16):138-143.
[10]Jong Kwan Park,Kyoung Hun Kim,Isao Tanaka,Kwang Bo Shim.Characteristics of rutile single crystals grown under two different oxygen partial pressures[J].Journal of Crystal Growth,2004,268(1):103-107.
[11]Wu Nan,Ma Weimin,Bi Xiaoguo,et al.Preparation of high-purity TiO2ultra-fine powders[J].Journal of Synthetic Crystals,2012,41(2):485-490(in Chinese).吴南,马伟民,毕孝国,等.高纯TiO2超微粉体的制备[J].人工晶体学报,2012,41(2):485-490.
[12]Yurii V K,Alexander A.Synthesis of nanocrystalline TiO2powders from aqueous TiOSO4solutions under hydrothermal conditions[J].Materials Letters,2003,57(5):1124-1129.
[13]Bi Xiaoguo,Liu Xudong,Li Qiang,et al.Preparation of titanium dioxide powder by phase transfer method[J].Journal of Shenyang Institute of Engineering(Natural Science),2012,8(4):362-365(in Chinese).毕孝国,刘旭东,李强,等.相转移法制备二氧化钛粉体的工艺研究[J].沈阳工程学院学报(自然科学版),2012,8(4):362-365.