Cobalt-, nickel-, copper-, and zirconium-cluster-based metal–organic frameworks (MOFs) were synthesized via the solvothermal method using 1,4-naphthalenedicarboxylic acid (1,4-NDC) as the organic linker. The synthesized MOFs were characterized by PXRD, XPS, TEM, and the BET model. Powder X-ray diffraction (PXRD) confirmed that the MOFs possessed highly crystalline structures. These MOFs were utilized as innovative catalysts to produce hydrogen through the hydrolysis of sodium borohydride (NaBH₄), a promising hydrogen source for energy applications. Among them, Co(1,4-NDC) and Ni(1,4-NDC) catalysts exhibited the highest catalytic activity, producing the maximum hydrogen volume within 5.1 and 6.0 min of stirring at room temperature, respectively. The high catalytic activity is attributed to the small particle sizes of the cobalt and nickel clusters in the MOFs, as confirmed by TEM analysis, and …