Electrochemical dinitrogen reduction (NRR) has riveted substantial attention as a greener method to synthesize ammonia (NH 3 ) under ambient conditions. Here, B, N-containing carbon catalysts with a discrete morphology were synthesized from the metal−organic framework-ionic liquid (MOF-IL) composite for NRR in a neutral electrolyte medium (pH = 7). Morphologydependent activity is witnessed, wherein C-BN@600 with a nanotubular morphology is able to achieve a high NH 3 yield rate of 204 μg h −1 mg cat −1 and an F.E. of 16.7% with a TOF value of 0.2 h −1 at −0.2 V vs RHE. Further, a rigorous protocol is put forward for true NH 3 estimation by tracing/eliminating any source of contamination in catalysts, electrolytes, or gas supply via ultraviolet−visible (UV−vis) spectroscopy, gas-purification methods, and isotope labeling experiments. Density functional theory predicts BN to be the favorable active site for N 2 adsorption with a reduced energy barrier in the first reduction step and sequential stabilization of the B−N bond by an adjacent carbon atom.