Balancing　the　adsorption　of　OH⁻　and　5-hydroxymethylfurfural　(HMF)　is　crucial　in　optimizing　the　competing　HMF　oxidation　reaction　and　oxygen　evolution　reaction,　especially　given　the　polymerization　tendency　of　HMF　in　alkaline　solutions.　Herein,　we　present　an　innovative　approach　for　rapidly　synthesizing　a　NiFe　bimetallic　metal-organic　framework　(MOF)　induced　by　electron-withdrawing　carbon　quantum　dot　(EW-CQD)　via　electron　beam　irradiation　within　2　​min.　EW-CQD　serve　as　structural　regulators,　expanding　the　NiFe-MOF　interlayer　spacing,　increasing　reactive　site　availability,　and　more　effectively　balancing　the　adsorption　of　OH−　and　HMF,　thereby　significantly　boosting　the　oxidation　activity　of　HMF.　The　resulting　EW-CQD-MOF　exhibits　a　low　potential　of　1.36　​V　vs.　RHE　at　10　​mA　​cm⁻2　and　maintains　excellent　durability　over　120　​h.　Comprehensive　in　situ　characterization　elucidates　the　HMF　oxidation　reaction　pathway,　showing　high　selectivity　towards　2,5-furandicarboxylic　acid　(FDCA)　under　ambient　conditions,　with　an　impressive　HMF　conversion　rate　of　94%　and　FDCA　selectivity　of　96%　within　6　​h.　These　findings　underscore　the　critical　role　of　structural　optimization　and　adsorption　balance　in　catalytic　performance　enhancement　and　offer　valuable　insights　for　designing　high-efficiency　catalysts,　advancing　sustainable　catalytic　processes.　©　2025　Central　South　University.