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Currently, two-dimensional materials are being actively pursued in catalysis and other fields due their abundance of defects, which results in enhanced performance relative to their bulk defect-free counterparts. To date, the exploitation of defects in two-dimensional materials to enhance photothermal therapies has received little attention, motivating a detailed investigation. Herein, we successfully fabricated a series of novel CoFe-based photothermal agents (CoFe-x) by heating CoFe-layered double hydroxide (CoFe-LDH) nanosheets at di