固化剂对喷雾干燥-焙烧法制备快离子导体Li_1.3Al_0.3Ti_1.7(PO₄)₃的影响

杨 波，李新海，郭华军，王志兴，吴飞翔

(中南大学 冶金科学与工程学院，长沙 410083)

摘 要：采用喷雾干燥法合成Li_1.3Al_0.3Ti_1.7(PO₄)₃的前驱体，将所得前驱体在不同温度下焙烧得到锂离子固态电解质Li_1.3Al_0.3Ti_1.7(PO₄)₃，研究固化剂PEG-6000对合成过程的影响。通过X射线衍射(XRD)、扫描电镜(SEM)、热重分析(TG-DTA)和傅里叶变换红外光谱(FTIR)对合成样品进行表征。结果表明：喷雾干燥法得到的前驱体均为球型颗粒，粒度为2~5 μm，添加固化剂的前驱体颗粒更细；固化剂降低前驱体合成纯相Li_1.3Al_0.3Ti_1.7(PO₄)₃的焙烧温度；无固化剂的前驱体在800 ℃下焙烧得到纯相Li_1.3Al_0.3Ti_1.7(PO₄)₃；添加固化剂的前驱体在700 ℃下得到纯相Li_1.3Al_0.3Ti_1.7(PO₄)₃。

关键词：Li_1.3Al_0.3Ti_1.7(PO₄)₃；快离子导体；喷雾干燥法

Effect of solidifying agent on preparation of Li_1.3Al_0.3Ti_1.7(PO₄)₃ by spray-drying and post-calcining method

YANG Bo, LI Xin-hai, GUO Hua-jun, WANG Zhi-xing, WU fei-xiang

(School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China)

Abstract:The solid state electrolyte Li_1.3Al_0.3Ti_1.7(PO₄)₃ was prepared by post-calcining the precursors obtained through spray-drying method. The effect of PEG-6000 addition on the microstructure and calcination temperature of Li_1.3Al_0.3Ti_1.7(PO₄)₃ was studied. The prepared samples were characterized by X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and differential thermal analysis and Fourier transform infrared spectroscopy. The results show that the precursors obtained by spray-drying are spherical particles with the average size of 2-5 μm. With the addition of PEG-6000, the decomposition and crystallinity temperature decrease, the particle sizes of the powders become smaller. The precursors without PEG-6000 calcined at 800 ℃ are well crystallized while the precursors with PEG-6000 are also well crystallized at only 700 ℃.

Key words:Li_1.3Al_0.3Ti_1.7(PO₄)₃; fast ionic conductor; spray-drying