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This paper presents a novel ultrasonic-assisted electrodeposition process of Mn-doped NiCo2O4 onto a commercial nickel foam in a neutral electroplating bath (pH = 7.0) under an ultrasonic power of 1.2 V and 100 W. Different sample properties were studied based on their crystallinity through X-ray diffraction (XRD), morphology was studied through scanning electron microscopy (SEM), and photodegradation was studied through ultraviolet–visible (UV–Vis) spectrophotometry. Based on the XRD results, the dominant crystallite phase obtained was shown to be a pure single NiCo2O4 phase. The optical properties of the photocatalytic film showed a range of energy band gaps between 1.72 and 1.73 eV from the absorption spectrum. The surface hydroxyl groups on the catalytic surface of the Mn-doped NiCo2O4 thin films showed significant improvements in removing methyl red via photodegradation, achieving 88% degradation in 60 min, which was approximately 1.6 times higher than that of pure NiCo2O4 thin films. The maximum hydrogen rate of the composite films under 100 mW/cm2 illumination was 38 μmol/cm2 with a +3.5 V external potential. The electrochemical performance test also showed a high capacity retention rate (96% after 5000 charge–discharge cycles), high capacity (260 Fg−1), and low intrinsic resistance (0.8 Ω). This work concludes that the Mn-doped NiCo2O4 hybrid with oxygen-poor conditions (oxygen vacancies) is a promising composite electrode candidate for methyl red removal, hydrogen evolution, and high-performance hybrid supercapacitor applications. [ABSTRACT FROM AUTHOR]