吉林大学学报(工学版) ›› 2023, Vol. 53 ›› Issue (8): 2272-2276.doi: 10.13229/j.cnki.jdxbgxb.20211048

• 材料科学与工程 • 上一篇    

快速热压烧结制备立方相Li7La3Zr2O12固态电解质

杨悦(),马天惠,赵培雷,贾剑明   

  1. 长春工业大学 材料科学与工程学院，长春 130012
  • 收稿日期:2021-10-12 出版日期:2023-08-01 发布日期:2023-08-21
  • 作者简介:杨悦（1974-），女，教授，博士.研究方向：新型导电陶瓷制备及其性能.E-mail：yangyue@ccut.edu.cn
  • 基金资助:
    吉林省发改委项目(2020C029-3)

Preparation of cubic Li7La3Zr2O12 solid electrolyte by fast hot⁃press sintering

Yue YANG(),Tian-hui MA,Pei-lei ZHAO,Jian-ming JIA   

  1. School of Materials Science and Engineering，Changchun University of Technology，Changchun 130012，China
  • Received:2021-10-12 Online:2023-08-01 Published:2023-08-21

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摘要：

应用电场辅助下的快速热压烧结工艺在低温850 ℃的条件下制备了立方相锂离子传导Li7La3Zr2O12固态电解质。讨论了在820~900 ℃的范围内烧结温度对烧结产物相组成、微观形貌、致密度以及锂离子电导率的影响。研究结果表明：当烧结工艺条件为温度850 ℃、恒压25 MPa、保温15 min，可以获得纯立方相结构Li7La3Zr2O12，晶粒排列紧密，且最佳性能对应相对密度为93%，总离子电导率达1.14×10-4 S?cm-1。

关键词: 材料学, 固态电解质, 快速热压烧结, 烧结温度, 离子电导率

Abstract:

In this paper， a garnet-type Li7La3Zr2O12 powder was synthesized through the solid-phase reaction route， an electric field-assisted fast hot-press sintering process was used to prepare a cubic phase lithium ion conductive Li7La3Zr2O12 solid electrolyte at a low temperature of 850 ℃， and the influence of sintering temperature on phase composition， microscopic morphology， density and lithium ion conductivity was systematically studied in the range of 820~900 ℃. The results show that when the sintering process conditions are set to a low temperature of 850 ℃， a constant pressure of 25 MPa， and a holding time of 15 minutes， a pure cubic Li7La3Zr2O12 structure can be obtained， the crystal grains are arranged tightly， the measured relative density is 93%， and the total ion conductivity has reached 1.14×10-4 S cm-1.

Key words: materials science, solid electrolyte, fast hot-press sintering, sintering temperature, ion conductivity

中图分类号: 

  • TB34

图1

固相反应法LLZO预烧粉末制备流程图"

图2

Li7La3Zr2O12样品烧结行为和机理"

图3

不同温度下烧结Li7La3Zr2O12样品的XRD图谱"

图4

不同温度下烧结样品断面扫描电镜显微图以及相对密度变化图"

表1

LLZO不同烧结温度下的室温离子电导率及相对密度"

烧结温度/℃离子电导率/（S?cm-1）相对密度/%
8206.60×10-582
8501.14×10-493
9007.56×10-590

图5

不同温度烧结LLZO的典型电化学阻抗图谱"

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