以常规无机试剂和含硅有机试剂为原料,采用溶胶-凝胶过程与压制成型烧结相结合的方法制备了NASICON纳米晶固体材料,利用TG-DTA对前驱凝胶原粉进行了分析测试,结果表明,NASICON相结构的形成温度范围为750～890℃.实验中重点对800～1000℃烧结所得纳米晶材料进行了表征.目的产物的XRD、FT-IR、FE-SEM、IS结果以及阿基米德法致密度测量结果显示,采用合适的烧结温度和周期可以成功制备出具有纳米级颗粒尺寸、良好结晶特性和较高致密度的固体电解质NASICON材料.材料电学特性测试结果表明,所制备的纳米晶固体电解质材料具有良好的离子导电特性和合理的离子传导激活能,其复合电导与温度倒数的Arrhenius图具有很好的线性关系,并且具有较高结晶特性的材料显示出更高的离子电导率.
Nanocrystalline solid material of NASICON (sodium super ionic conductor) was synthesized by the sol-gel and
high-temperature sintering process, in which normal inorganic reagents and silicon organic reagent were used as the raw materials. The temperature range
of 750～890℃ for the formation of NASICON phase was recognized through the analysis of TG-DTA result conducted for NASICON xerogel. Thus,
the sintering process was carried out in the temperature range of 800～1000℃. As shown from the results of some analytical
methods such as XRD, FT-IR, FE-SEM, impedance spectrum and the measurement of Archemede density, the solid-electrolyte NASICON with grain size of
nanometer, good crystallinity and high relative density was synthesized successfully by adopting appropriate sintering temperature and period. A
linear Arrhenius plot for the resulted NASICON material was achieved and a reasonable active energy was got based on the complex impedance measurement
conducted at different temperatures. The solid material possessed an ideal ionic conductivity. Moreover, highly crystallized NASICON
showed higher ionic conductivity.
参考文献
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