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The valorization technique successfully transformed waste polyethylene terephthalate (PET) into valuable carbon nanomaterial (CN)/graphene, while doped and undoped ZnO nanopowders were synthesized via sol–gel methods. Utilizing XRD, BET, TEM, EDX, FTIR, and TGA analyses, the synthesis of sp² 2D sheet, pristine, and doped ZnO nanostructures was confirmed. Solid-state gas sensor devices, tested under 51% relative humidity (RH), 30 °C ambient temperature, and 0.2 flow rate, exhibited a 3.4% enhanced response to H₂ gas compared to CO₂ at 50 ppm concentrations over time. Notably, the ZnO/CN sensor surpassed CN and ZnO alone, attributed to CN dopant integration with decreasing order of response performance as ZnO/CN > CN > ZnO. This study underscores the efficacy of valorization techniques in generating high-value carbon nanomaterials and their efficacy in bolstering gas sensor performance, with ZnO/CN demonstrating superior response capabilities.