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无表面活性剂水热法大规模合成铝酸锂纳米棒:参数优化及生长机理研究

Large-scale, surfactant-free, hydrothermal synthesis of lithium aluminate nanorods: optimization of parameters and investigation of growth mechanism.

作者信息

Joshi Upendra A, Lee Jae Sung

机构信息

Eco-friendly Catalysis and Energy Laboratory NRL, Pohang University of Science and Technology, Pohang, Korea.

出版信息

Inorg Chem. 2007 Apr 16;46(8):3176-84. doi: 10.1021/ic062227m. Epub 2007 Mar 20.

Abstract

Lithium aluminate nanorods were successfully synthesized from Al2O3 nanoparticles and lithium hydroxide by a simple, large-scale hydrothermal process without any surfactant or template. The various reaction parameters were optimized to achieve the maximum yield. The as-obtained nanorods had orthorhombic beta-lithium aluminate structure with edges in the range of 40-200 nm and lengths of 1-2 mum confirmed by SEM, TEM, XRD, and NMR. Upon calcination at 1273 K for 12 h it transformed to gamma-lithium aluminate, yet maintained the initial morphology, demonstrating the thermal stability. The ratio of lithium hydroxide to aluminum oxide showed a significant effect on the morphology as Li/Al = 1 gives "microroses", whereas Li/Al = 3 and Li/Al = 15 gave "microbricks" and "nanorods", respectively. Investigation of the mechanism showed that the nanorods were formed via a "rolling-up" mechanism. As we used all-inorganic raw materials and a simple synthetic procedure under mild conditions, the scale-up of this process for large-scale production should be very easy.

摘要

通过简单的大规模水热法,以氧化铝纳米颗粒和氢氧化锂为原料,在无任何表面活性剂或模板的情况下成功合成了铝酸锂纳米棒。对各种反应参数进行了优化以实现最大产率。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)和核磁共振(NMR)证实,所制备的纳米棒具有正交晶系的β-铝酸锂结构,其边缘尺寸在40 - 200纳米范围内,长度为1 - 2微米。在1273 K下煅烧12小时后,它转变为γ-铝酸锂,但仍保持初始形态,表明其具有热稳定性。氢氧化锂与氧化铝的比例对形态有显著影响,当Li/Al = 1时生成“微玫瑰”,而Li/Al = 3和Li/Al = 15时分别生成“微砖”和“纳米棒”。机理研究表明,纳米棒是通过“卷曲”机制形成的。由于我们使用的是全无机原料且合成过程简单、条件温和,该工艺放大用于大规模生产应该非常容易。

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