采用凝胶燃烧-等离子氮杂方法制备了磷灰石型硅酸镧(La9.33Si6O26-1.5xNx)固体电解质,并对氮杂样品进行了XRD、FT-IR和Raman表征,测试了样品的热稳定性及电导率。结果表明:La9.33Si6O26-1.5xNx的六边磷灰石型物相结构不变。氮杂导致硅酸镧晶体结构中[SiO4]的环境发生改变,并影响其振动模式。TG-DSC分析表明氮杂硅酸镧的烧结温度应为1 200℃。在微波功率为300W,作用时间为15min条件下制备的氮杂硅酸镧的烧结体的电导率达1.28×10-2 S.cm-1(800℃)。初步分析认为氮杂导致通道氧空位浓度增加、氧离子迁移速率加快、电导率变大,形成空间电导增强效应。
Apatiteztype nitrogen doping lanthanum silicate ( La9.33 Si6O26-1.5xNx ) solid electrolytes Were prepared by gel combustion-plasma. The samples were characterized by XRD, FT-IR and Raman, moreover, their thermostability and conductivity were tested. The results show that the six-edge apatie-type structure of La9.33 Si6O26-1.5x Nx does not change. The surroundings of ESiO4-] tetrahedral in lanthanum silicate crystal structure change due to the nitrogen doping and then the vibrational modes were affected. The TG-DSC analyses show that the sintering temperature of nitrogen-doped lanthanum silicate should be 1 200℃. The conductivity of the lanthanum silicate sintered body, which was prepared under the conditions as microwave power of 300 W and action time of 15 min, can be up to 1.28×10-2 S · cm-1 (800 ℃). Preliminary analysis indicates that nitrogen doping leads to the increase of channel oxygen vacancy concentration, then the oxygen ion migration rate becomes faster and the conductivity is improved, finally, the space conductivity enhancement effect is created.