5-Hydroxymethylfurfural (HMF) electrooxidation for 2,5-furandicarboxylic acid (FDCA) production has become a sustainable method for value-added products at the anode. Here, an amorphous NiMo composite oxide supported on nickel foam (NF) is fabricated for HMF electrooxidation (HMFOR) via one-step electrodeposition. The synthesized NiMo/NF delivers 98.3% FE toward FDCA at 1.5 V RHE and maintains FE above 90% during 10 h. In situ Raman spectroscopy proves the formation of the active species Ni 3+ -OOH during the reaction process. Due to the introduction of high-valent Mo 6+ , the Ni 3+ active species can be stabilized and the adsorption of aldehyde in HMF can be promoted during the reaction process, thus enhancing the FDCA electrosynthesis performance.