In this study, for the first time two electrochemical synthesis techniques including cyclic voltammetry (CV) and linear sweep voltammetry (LSV) were used for MOF synthesis. The Ni3(BTC)2 electrocatalyst was synthesized and deposited without any binder, for a short time and at ambient temperature on the nickel foam substrate. Morphology studies showed that the LSV method leads to preserving the 3D structure of nickel foam which promotes the catalytic activity. It should be noted that two parameters, such as voltage range and scan rate, were optimized during the LSV method. Moreover, X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy were used to confirm the MOF's structural integrity. Furthermore, the Brunauer-Emmett-Teller (BET) method verified the porous structure of NiBTC MOF. Additionally, the performance of bare and modified nickel foams was also examined for the hydrogen evolution reaction (HER) which demonstrated the tremendous potential of NiBTC/Ni foam in HER catalytic activity.