The 2,5-diformylfuran (DFF) is a significant biomass derivative that is employed in a variety of industries. One approach is to synthesize it by an oxidation process of 5-hydroxymethylfurfural (HMF). The challenges in DFF manufacture come from the necessity for extreme conditions, the overoxidation issue, and the limitations of noble materials employed in neutral or acidic environments. By using mild alkaline as an electrolyte, DFF can be produced electrochemically alongside hydrogen gas generation, eliminating extreme conditions and allowing for the study of a wide range of transition metals. Moreover, the performance of bimetallic electrocatalysts has been studied, and it has been found to be more active in many kinds of processes, particularly Layered Double Hydroxides (LDHs). Electrodeposition, once widely chosen among various LDH production methods, is preferred for producing controlled and uniform thin layers. This work examines the electrocatalytic properties of NiCo-LDH and NiFe-LDH in the production of DFF. Cobalt, which has a high adsorption characteristic, is compared to iron, which has a weak adsorption characteristic towards HMF. This study demonstrates that NiCo-LDH has a higher activity but lower DFF selectivity compared to NiFe-LDH for the same amount of passed charge. Strong adsorption promotes reactant activation and reduces the energy barrier while reducing DFF selectivity due to overoxidation. To achieve optimal electrocatalyst performance, a careful balance of adsorption strength and reaction pathway management is required. Proper optimization of these parameters is required to improve efficiency and selectivity in the electrocatalytic process.