Batteries in situ testing in SEM

article in a collection out of WoS and Scopus

English

We present in situ battery testing holders for SEM and FIB-SEM systems. Two types of in situ holders were newly developed, which assure transfer to SEM in a protective environment (in argon or high vacuum), electrical testing and heating of battery samples in SEM. When connected to SEM stage, the holders provide electrical contacting to the sample area and allow testing (galvanostatic cycling, cyclic voltammetry and other electrochemical testing) of a battery inside SEM. Micron sized batteries can be created on the in situ holders using FIB preparation of electrodes (Fig. 1). Consequent placement of electrolyte between the electrodes is possible in the vacuum of the SEM chamber as well. We will present example of electrical testing of a lithium titanium oxide (LTO) battery created by FIB on the in situ testing holder, which uses ionic liquid as the electrolyte. MEMS heating plate can be connected in the in situ holder, allowing heating of battery materials (up to 1200°C) during in situ SEM imaging. Optionally, reactive gases such as pure hydrogen, oxygen, or hydrogen sulfide, can be injected into a small reaction volume around the sample. This technique allows for real time SEM imaging of battery materials synthesis under realistic conditions that are used during battery materials development and manufacturing. We will present examples of in situ synthesis of tungsten oxide (Fig. 2) and tungsten sulfide nanowires, which are possible materials for sulfur based batteries. Moreover, the presented holders can be used for transfer of larger air sensitive samples to and from SEM, allowing SEM imaging of larger parts of batteries in SEM as well as FIB preparation of TEM lamellae from selected parts of the battery and consequent transfer of the lamellae to TEM without contact with air.

In-situ; Li-ion; FIB; SEM; battery; ionic liquid; characterization; synthesis

NOVÁK, L.; KUNDRAT, V.; KLVAČ, O.; KAZDA, T.

4. 9. 2022

Czechoslovak Microscopy Society

Brno, Czech Republic

978-80-11-02253-2

16th Multinational Congress on Microscopy

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144

145

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https://www.16mcm.cz/wp-content/uploads/2022/09/16MCM-abstract-book.pdf