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Summary: The low cost, low over‐potential loss, good catalytic properties for hydrogen evolution reaction (HER), high corrosion stability, commercially available, and could be applied in pH‐neutral solution and ambient temperature are important properties for the cathode materials when it is applied in microbial electrolysis cell (MEC) technology. This study has two‐pronged objectives: the first is to investigate the feasibility of titanium (Ti) and graphite felt (GF) coated with nickel (Ni), and the second is to generate hydrogen from the fermentation effluent (FE). The electrodeposition (ED) method was used to deposit Ni catalyst onto Ti (Ni/Ti) and GF (Ni/GF) surfaces. The scanning electron microscopy (SEM) and energy dispersive X‐ray (EDX) spectroscopy were used to characterize the cathode morphology and element composition. The catalytic properties of Ni/Ti and Ni/GF could be evaluated using the linear sweep voltammetry tests. The maximum volumetric H2 production rates of MEC using Ni/Ti and Ni/GF cathodes were obtained at 0.39 ± 0.01 and 0.33 ± 0.03 m3 H2 m−3 d−1 respectively. The Ni/Ti and Ni/GF cathodes could be used as alternative cathodes while producing hydrogen from FE. [ABSTRACT FROM AUTHOR]

• Catalytic properties of Ni-Fe and GF/Pt were characterized using LSV tests. • Tafel slope was determined based on the data points in the onset potential. • EGF can be used as substrate for hydrogen production. • Ni-Fe shows comparable performance with GF/Pt cathode in BES application. The high cost of Pt-based cathode, and its possibility of being poisoned by the presence of buffer in the electrolyte are two paramount issues in the BES system. The Ni-Fe has become one of the good alternatives because it has excellent catalytic properties, inexpensive, commercially available and low toxicity to microorganisms. In this study, Ni-Fe foam applied as a cathode in dual-chamber BES, while effluent of glucose fermentation as a substrate in the anode side. The characteristic of Ni-Fe surface was analyzed by using field emission scanning electron microscopy. Whereas, the catalytic property of Ni-Fe was evaluated by using linear sweep voltammetry test. The maximum hydrogen production rate and yield obtained were 500 ± 80 m3/m3/d and 470.2 ± 11.2 mL/g COD, respectively. The results show that the Ni-Fe has comparable performance to GF/Pt. Hence it could be used as an alternative cathode in BES application. [ABSTRACT FROM AUTHOR]