The mainstream synthesis method for MXene is using aqueous fluorine-containing acidic solutions to eliminate the A-element layers from their MAX phases. However, this strategy is environmentally hazardous and impairs the material performance (e.g., supercapacitor and Li−S batteries) owing to the presence of −F terminations. Herein, we exploit a lowtemperature "soft chemistry" approach based on photo-Fenton (P.F.) reaction for the fabrication of F-free Ti 3 C 2 (Ff-Ti 3 C 2 ) with high purity of 95%. It is confirmed that the continuous generation of highly reactive oxygen species (HO • and O 2•− radicals) during the P.F. reaction weakens the metallic Ti−Al bonds in the MAX phase and promotes the formation of high concentration OH − anions, which are conducive to the sequential topochemical deintercalation of Al layers. Moreover, the strengthened charge accumulation on the Ff-Ti 3 C 2 surface creates rich electron "reservoirs" for actuating the Li−S chemistry, which not only strengthens the host−guest interactions but also propels the kinetics of the polysulfide conversion. Taking advantage of the superior mechanical robustness, better electrolyte wettability, and improved electrocatalytic activity, the resultant Ff-Ti 3 C 2 can be used as an ideal sulfur host and Li−S chemistry mediator for advanced flexible Li−S batteries.

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