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Lithium-ion secondary batteries (LIBs) store electric energy via Li +  deintercalation from cathode materials. The Li +  deintercalation frequently drives a first-order phase transition of the cathode material as a result of the Li-ordering or Li-concentration effect and causes a phase separation (PS) into the Li-rich and Li-poor phases. Here, we performed an  in situ  microscopic investigation of the PS dynamics in thin films of cobalt hexacyanoferrate, Li  x  Co[Fe(CN) 6 ] 0.9 , against Li +  deintercalation. The thick film ( d  = 1.5 μm) shows a characteristic macroscopic PS of several tens of μm into the green (Li 1.6 Co[Fe(CN) 6 ] 0.9 ) and black (Li .6 Co[Fe(CN) 6 ] 0.9 ) phases in the  x  range of 1.0 <  x  < 1.6. Reflecting the substrate strain, the thin film ( d  = 0.5 μm) shows no trace of the PS in the entire  x  region. Our observation suggests that the macroscopic PS plays a significant role in the charge/discharge dynamics of the cathode.

In situ observation of macroscopic phase separation in cobalt hexacyanoferrate film