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Inactive lithium (Li) formation is the immediate cause of capacity loss andcatastrophic failure of Li metal batteries. However, the chemical component andthe atomic level structure of inactive Li have rarely been studied due to thelack of effective diagnosis tools to accurately differentiate and quantify Li+in solid electrolyte interphase (SEI) components and the electrically isolatedunreacted metallic Li0, which together comprise the inactive Li. Here, byintroducing a new analytical method, Titration Gas Chromatography (TGC), we canaccurately quantify the contribution from metallic Li0 to the total amount ofinactive Li. We uncover that the Li0, rather than the electrochemically formedSEI, dominates the inactive Li and capacity loss. Using cryogenic electronmicroscopies to further study the microstructure and nanostructure of inactiveLi, we find that the Li0 is surrounded by insulating SEI, losing the electronicconductive pathway to the bulk electrode. Coupling the measurements of the Li0global content to observations of its local atomic structure, we reveal theformation mechanism of inactive Li in different types of electrolytes, andidentify the true underlying cause of low Coulombic efficiency in Li metaldeposition and stripping. We ultimately propose strategies to enable the highlyefficient Li deposition and stripping to enable Li metal anode for nextgeneration high energy batteries.

Quantifying Inactive Lithium in Lithium Metal Batteries