Compared to platinum, nickel is an inexpensive catalyst that can oxidize methanol in alkaline media. There is a desire to increase nickel loading during electrodeposition for improved performance. In this paper, a nickel cysteine complex (NiCys) is used as the precursor for electrodeposition on glassy carbon electrode surfaces. After optimization of cysteine concentration, the surface concentration of NiOOH on NiCys electrodes characterized by cyclic voltammetry in 0.1 M NaOH can reach 1.28 (± 0.32) × 10 −7 mol/cm 2 . The large amount of NiOOH on NiCys electrodes provide 5 times the methanol oxidation current compared to Ni electrodes prepared without cysteine as demonstrated by chronoamperometry at 0.7 V vs. Hg/HgO. Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy have been applied to examine surface morphologies and structures of NiCys and Ni electrodes. The analysis reveals that cysteine adjusts the solubility of Ni(OH) 2 in 0.1 M NaOH, so more uniform and smaller size nanoparticles are electrodeposited on electrode surfaces compared to Ni electrodes. Fuel cells are a promising energy conversion device to convert chemical energy in a fuel to electrical energy. Nickel-based anodic electrocatalysts are cheaper than conventional precious metal based catalysts and can oxidize various fuels e.g. alcohols, carbohydrates, amino acids and alkanes in alkaline media.1 Direct methanol fuel cells are attracting more interest, because methanol has a high theoretical energy density and is easy to handle in transportation and storage. In recent years, there has been extensive research on using nickel based catalysts to electro-oxidize methanol. Planar nickel electrodes show poor catalytic activities, 2 so some researchers have focused on dispersing nickel centers in three dimensional structures to increase methanol oxidation current. Based on this concept, many nickel complexes in alkaline solution have been electrodeposited onto glassy carbon electrode surfaces and the electrochemical properties have been examined. [2][3][4][5][6][7][8][9][10][11][12][13][14] Nickel macrocyclic complexes, such as nickel porphyrin, cyclam, annulene, salen and cyanine, have been studied. These examples show methanol oxidation currents are five to eighty times higher than their nickel control electrodes. 5,15 However, none of these studies provide a thorough description of the three dimensional structure, i.e. how nickel centers are dispersed by these nickel complexes. It is also not discussed as to how these nickel complexes relate to NiOOH (the catalytically active species) in chemical structure. Very few papers present surface morphology images.3,4 Most of these nickel complexes have NiOOH surface concentration in the range of 10 −9 to 10 −8 mol/cm 2 . One of the nickel annulene has reached the highest value of 9.7 × 10 −8 mol/cm 2 . 16 We noticed that cysteine can dissolve Ni(OH) 2 in 0.1 M NaOH, so cysteine should have a strong interac...