three-dimensional analysis of the positive electrode

P02278形態科学第２研究室20210603 Ⅰ: 3D-SEM observation at positive electrode of sulfide-based all-solid-state battery Three-dimensional analysis of the positive electrode mixture layer using the 3D-SEM method in a sulfide-based all-solid-state battery model samples ※Sample courtesy of Prof. Hayashi(Osaka Pref. University ) All-solid-state batteries have high safety and are expected as next-generation lithium-ion batteries. Using the 3D-SEM method, the shape and size of each part of electrode can be observed three-dimensionally. Here, we show an example of a comparative study using three kinds of model samples in which the ratio of each part of electrode (with only the active materials and solid electrolytes) was changed. Ⅱ: Extraction of each part and calculation of characteristic quantities by image analysis Each part of an electrode can be extracted by image analysis. In addition, quantitative evaluation such as volume fraction and coverage can be performed using the extracted images. Figure 1 3D reconstruction image of NMC48 wt% （About 50 μm 3 ）活物質 Active materials / Solid electrolytes Solid electrolytes Active materials : LiNi 1/3 Mn 1/3 Co 1/3 O 2 NMC48 wt%, 55 wt%, 62 wt% Solid electrolytes : Li 3 PS 4 • FIB processing and observation can be performed in an inert atmosphere. • Three‐dimensional morphological observation is possible by continuously acquiring cross‐sectional SEM images. 10 m Solid electrolyte 42.7 m Z X Y Acquired 501 images every 100 nm X Y Y Z X Z X Y Z 20 m 10 m 10 m 10 m Cross‐sectional SEM image 10 m Extracted image of active material Extracted image of solid electrolyte White： Surface of active material Red： Solid electrolyte in contact with the active material Active material Schematic diagram of samples Figure 2 Extracted images of each part of NMC48 wt% Figure 3 Extracted image of the solid electrolyte part in contact with the active material Solid electrolyte Active material Void 0.0% 10.0% 20.0% 30.0% 40.0% 50.0% 60.0% 70.0% NMC48 wt% NMC55 wt% NMC62 wt% 0.0% 10.0% 20.0% 30.0% 40.0% 50.0% 60.0% NMC48 wt% NMC55 wt% NMC62 wt% NMC48 wt% NMC55 wt% NMC62 wt% ＜ Volume fraction ＞＜ Ratio of solid electrolyte contact area to active material surface ＞ 10 m 10 m 10 m Voids Active materials Solid electrolyte

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Page 1: Three-dimensional analysis of the positive electrode

P02278形態科学第２研究室20210603

Ⅰ: 3D-SEM observation at positive electrode of sulfide-based all-solid-state battery

Three-dimensional analysis of the positive electrode mixture layer using the 3D-SEM method

in a sulfide-based all-solid-state battery model samples

※Sample courtesy of Prof. Hayashi(Osaka Pref. University )

All-solid-state batteries have high safety and are expected as next-generation lithium-ion batteries. Using the 3D-SEM method, the shape and size of each part of electrode can be observed three-dimensionally. Here, we show an example of a comparative study using three kinds of model samples in which the ratio of each part of electrode (with only the active materials and solid electrolytes) was changed.

Ⅱ: Extraction of each part and calculation of characteristic quantities by image analysis

Each part of an electrode can be extracted by image analysis. In addition, quantitative evaluation such as volume fraction and coverage can be performed using the extracted images.

Figure 1 3D reconstruction image of NMC48 wt% （About 50 μm3）

活物質

Active materials / Solid electrolytes

Solid electrolytes

Active materials : LiNi1/3Mn1/3Co1/3O2

NMC48 wt%, 55 wt%, 62 wt% Solid electrolytes : Li3PS4

• FIB processing and observation can be performed in an inert atmosphere.• Three‐dimensional morphological observation is possible by continuously

acquiring cross‐sectional SEM images.

10 m

Solid electrolyte

42.7 m

Acquired 501 images every 100 nm