This study aims to synthesize biocomposite by combining banana stem activated carbon (AC) and ZnO Nanoparticles (NPs) to evaluate their adsorption potential towards hexavalent chromium (Cr (VI)) (20 mg/L). The AC used was successfully synthesized by an impregnation method using phosphoric acid (H3PO4) for 24 h, followed by a carbonization method. ZnO NPs were synthesized using the direct precipitation method using zinc acetate dihydrate (0.2 M) and KOH (0.4 M) as precursors. The AC/ZnO NPs biocomposite was fabricated using the mechanical alloying method at a frequency of 10 Hz for 30 min. The FTIR results show that both adsorbents, namely pure AC and AC/ZnO NPs have abundant functional groups. XRD results show the adsorbent is amorphous with pure AC at 89.95% and AC/ZnO NPs biocomosite at 56.49%. SEM results showed that the morphology of AC resembled crushed bovine bone marrow, and the morphology of ZnO NPs showed a marshmallow-like shape. The UV–vis spectrometer test results show that at the absorption peak of 350 nm the Cr (VI) removal efficiency slowly decreases and disappears at a dose variation of 1.5 g pure AC, 2 g biocomposite AC/ZnO NPs, and 2 g pure AC with Cr (VI) removal efficiency of 99.61%, 99.64%, and 99.83% respectively. Finally, we can report that the high degradation ability for Cr (VI) can be related to thesharp peak of –C=O group, reduced ΔLO−TO, and smaller average crystallite size in AC/ZnO NPs biocomposite.