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Deformed microstructure of the adiabatic shear bands in zirconium alloy impacted by split Hopkinson pressure bar at a strain rate of about 2300 s-1 was characterized systemically. Four different strains of zirconium alloy subjected to impact loading at same strain rate were designed by means of strain stopper rings. At a strain of 0.30, the transformed bands were distinguished at the tip of crack. The transformed bands mainly composed of the ultrafine and equiaxed grains with the mean diameter of about 100~300 nm were found by a dual beam FIB/TEM system. Besides ultrafine grains in the transformed bands, nanometer fine grain was observed and confirmed by HRTEM. Thus, the transformed bands mainly composed of the mixed microstructure including nanometer and ultrafine grains were confirmed, and n phase transformation and amorphization in transformed bands take place.

We report a method for in situ atomic-scale observation of electrochemical delithiation in a working all-solid-state battery using a state-of-the-art chip based in situ transmission electron microscopy (TEM) holder and focused ion beam milling to prepare an all-solid-state lithium-ion battery sample. A battery consisting of LiCoO 2 cathode, LLZO solid state electrolyte and gold anode was constructed, delithiated and observed in an aberration corrected scanning transmission electron microscope at atomic scale. We found that the pristine single crystal LiCoO 2 became nanosized polycrystal connected by coherent twin boundaries and antiphase domain boundaries after high voltage delithiation. This is different from liquid electrolyte batteries, where a series of phase transitions take place at LiCoO 2 cathode during delithiation. Both grain boundaries become more energy favorable along with extraction of lithium ions through theoretical calculation. We also proposed a lithium migration pathway before and after polycrystallization. This new methodology could stimulate atomic scale in situ scanning/TEM studies of battery materials and provide important mechanistic insight for designing better all-solid-state battery.