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普通冷冻透射电子显微镜表征LiPxSy类固态电解质高分辨像的方法

李小菊*，隋海燕，王延涛
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2022年 第41卷 第3期: 1000-6281（2022）03-308-07     下载地址：

普通冷冻透射电子显微镜表征LiPxSy类固态电解质高分辨像的方法

李小菊*，隋海燕，王延涛

（1. 山东大学微生物技术研究院，山东青岛  266237；2. 中国科学院青岛生物能源与过程研究所，山东 青岛  266101）

摘要  本文采用配备冷冻样品杆的普通透射电子显微镜，探索固态电池中LiPxSy类电解质材料的物相结构和高分辨晶格像的表征方法。LiPxSy类电解质具有很高的导离子率，是理想的固态电解质材料，但该类电解质性质敏感，对空气的不稳定性导致其任何处理均需要惰性气体环境。试验探索表明，利用在全程液氮中冷冻转移的手段，可以有效保留LiPxSy类电解质材料的物相，但受样品表面凝结冰的影响，冷冻低剂量（low dose）模式很难获得高分辨晶格像。通过冷冻杆升温（升温过程中冷冻杆shutter需呈打开状态）、而后常温表征的手段，成功获得了LiPxSy类电解质材料较理想的高分辨晶格像。

关键词   冷冻；透射电子显微镜；固态电池电解质；高分辨晶格像

中图分类号：O766+.1；TM911.3；O514    文献标识码：Adoi:10.3969/j.issn.1000-6281.2022.03.012

 

The method for obtained HRTEM image of LiPxSy solid electrolyte by using ordinary cryo-TEM

LI Xiao-ju1*, SUI Hai-yan1, CUI Guang-lei2

(1. State Key Laboratory of Microbial Technology，Shandong University，Qingdao Shandong 266237；

2. Qingdao Institute ofBioenergy and Bioprocess Technology,Chinese Academy of Sciences, Qingdao Shandong 266101, China)

Abstract In this paper, an ordinary transmission electron microscope(TEM)and a frozen holderare used to explore the phase structure characterization of LiPxSyelectrolyte materials in solid-state batteries and the specialmethod for obtainedhigh-resolution TEM (HRTEM)images.The LiPxSymaterialsare ideal solid-state electrolytes, as they have very high ionic conductivity. However, these electrolyte materials are sensitive and unstable in air, any processing of these electrolytes requires an inert gas environment. Our result indicates that the phase of LiPxSy can be effectivelymaintained bytransferred in liquid nitrogen. However, due to the effect of the ice on the sample surface which cannot be avoided during the frozen transfer process, it is difficult to obtain HRTEM images in the frozen and low-dose mode by TEM. Through the method of warming up the frozen holder and characterizing at room temperature, ideal HRTEM images of the LiPxSy electrolyte material were obtained. It should be noted that during the warming-up process of the frozen holder, the shutter of the holder must be in open state, which is very important to obtain the HRTEM images of LiPxSy.

Keywords  frozen；transmission electron microscope(TEM)；electrolyte materials in solid-state batteries；HRTEM

 

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