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HighlightsA ‘solid–liquid’ conversion for increasing the sulfur content from ~ 50 to 72% for RT Na–S batteries is developed.    The redox mechanisms of two types of sulfur: sulfur on the surface of a cathode host (155S) and sulfur in the pores of the host (300S) in ether and carbonate ester electrolytes are studied.    The function of NaNO 3  additive on modifying Na anode and confining the shuttle effect of dissolving polysulfides during ‘solid–liquid’ conversion is visualized.Supplementary Information  The online version contains supplementary material available at 10.1007/s40820-021-00648-w.

Understanding Sulfur Redox Mechanisms in Different Electrolytes for Room-Temperature Na–S Batteries