Abstract <p>The urgent demand for sustainable energy solutions has driven the development of a sonochemical method to synthesize two-dimensional (2D) non-van der Waals (n-vdW) hematene from rust on corroded iron nails. Hematene, a 2D iron oxide nanomaterial, is known for its large surface area, plentiful electroactive sites, and superior redox behavior, which collectively make it an excellent candidate for energy storage technologies. The prepared hematene was blended with carbon black (CB) and polyvinylidene fluoride (PVDF), then deposited onto nickel foam (Ni) to develop the Hematene/CB/PVDF@Ni Foam electrode configuration. Electrochemical evaluation in a three-electrode configuration demonstrated a specific capacitance (<i>C</i>_s) of 196.71 F g⁻¹ at a current density of 0.1 A g⁻¹, indicating the potential of this green-synthesized electrode system for supercapacitor applications; furthermore, the Hematene/CB/PVDF@Ni electrode exhibited a notable energy density of 15.68 Wh kg⁻¹ and a power density of 73.69 W kg⁻¹, along with excellent CV stability, retaining 86.4% of its capacitance after 10,000 cycles. This approach not only repurposes waste materials to promote environmental sustainability but also provides a cost-effective pathway for scalable supercapacitor production.</p>