In this study, a bimetallic Co–Fe nanocatalyst supported on carbon quantum dots (CQDs) is introduced as an effective catalyst for promoting hydrogen generation upon hydrolysis of sodium borohydride. Hydrothermal synthesis routes were used to produce CQDs support. All samples were subjected to analysis using XRD, UV–Vis, Raman, FTIR, FESEM, EDX, and nitrogen adsorption-desorption techniques. Benefiting from the higher surface area (51 m2gr), pore volume (0.200 mLgr), and good dispersion of Co–Fe nanoparticles over the CQDs support, the CoFe/CQD spherical nanocatalysts with 5 wt.% iron content exhibited the highest catalytic activity of 20200 mL/min.gcat within only 1 min of reaction. The kinetics studies revealed a low activation energy of 48 kJ/mol over this optimum catalyst. In addition, it was found that the catalytic performance of this catalyst was decreased after 4 runs of recycling experiments. Catalyst degradation and leaching of the active phase were likely responsible for the decline in catalyst performance.