液相法によるリチウムイオン伝導性酸化物の低温合成

采用低温溶胶-凝胶法制备了锂石榴石型氧化物Li7-xLa3Zr2-xNbxO12 （LLZNbO, x=0-1）。然后，用玻璃添加剂LiO2-B2O3-SiO2玻璃和BaO-B2O3-SiO2玻璃刺激陶瓷电解质的烧结，在低温下保持立方相稳定。立方石榴石相热处理形成的溶胶-凝胶法导出前驱粉末在600 - 700度c . presursor粉和玻璃添加剂,53 lio2･31 b2o3･12二氧化硅(摩尔%)(LiO2-B2O3-SiO2玻璃)或35包･10曹･5氧化铝･15 b2o3･10二氧化硅(摩尔%)(BaO-B2O3-SiO2玻璃)压制成球团和烧结在900度城建relatative密度为86%,通过烧结玻璃添加剂在900度c复合材料烧结BaO-B2O3-SiO2玻璃,当浓度高于4 wt%时，可检测到La2Zr2O7的存在，而用LiO2-B2O3-SiO2玻璃烧结的复合材料得到了单立方相。在30℃下，使用重量为4wt .%的LiO2-B2O3-SiO2玻璃，得到的复合材料的离子电导率为8x10^- 5s /cm。电导率比固相反应工艺报道的材料低20%，但使用的热处理比常规固相反应工艺所需的热处理温度低300℃左右。这为LLZNbO固体电解质在全固态电池中的进一步应用做出了重要贡献。

Lithium garnet-type oxides Li7-xLa3Zr2-xNbxO12 (LLZNbO, x=0-1) were prepared by a sol-gel process at low temperatures. Then, glass additives, LiO2-B2O3-SiO2 glass and BaO-B2O3-SiO2 glass, were used to stimulate the sintering of the ceramic electrolyte retaining the cubic phase stable at low temperatures.The cubic garnet phase was formed by a heat-treatment of sol-gel derived precursor powders at 600 - 700 degree C. The presursor powders and glass additives, 53LiO2･31B2O3･12SiO2 (mol%) (LiO2-B2O3-SiO2 glass) or 35BaO･10CaO･5Al2O3･15B2O3･10SiO2 (mol%) (BaO-B2O3-SiO2 glass) were pressed into pellets and sintered at 900 degree C.The relatative density of 86% was achieved by the sintering with glass additives at 900 degree C. In the composites sintered with the BaO-B2O3-SiO2 glass, the presence of La2Zr2O7 was detected at concentration higher of 4 wt%, while the single cubic phase was obtained for the composites sintered with the LiO2-B2O3-SiO2 glass.The ionic conductivity of the obtained composite was 8x10^-5 S/cm at 30 degree C using 4 wt.% of LiO2-B2O3-SiO2 glass. The conductivity is 20% lower than the material reported by the solid state reaction process, but the heat treatment used is about 300 degree C lower than that required by the conventional solid state reaction process. This represents an important contribution to further application of the LLZNbO solid electlolyte to all-solid-state battery.