An ultrasonic fabrication of MoO3-g-C3N4 photocatalyst for substantially better photocatalytic recital is presented. XRD and FTIR confirmed the orthorhombic phase of MoO3-g-C3N4. The SEM manifests the oblate-like structure of g-C3N4 and nano rod-like morphology for MoO3 and MoO3-g-C3N4, respectively. The photocatalytic properties are evaluated by photoelectrochemical (PEC) and photodegradation measurements under visible light. The linear sweep voltammetry (LSV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) comprehend MoO3-g-C3N4 as a hydrogen evolution photocatalyst. The photocurrent density of MoO3-g-C3N4 is recorded beyond 7.5 mA/cm2, which is approximately 5–6 folds greater than pure MoO3 and g-C3N4. In addition, the visible light exposure showed MoO3-g-C3N4 photocatalyst could decompose methylene blue (MB) dye up to 93%. The efficient separation and transfer of charges allocated to MoO3-g-C3N4 follow Z-scheme and pseudo-first-order kinetic reaction. The creation of heterojunctions among g-C3N4 and MoO3 suppresses the unfavorable electron-hole pairs recombination process and therefore recesses charge transfer resistance, hence augmenting photocatalytic performance.