Nanometer-scale thin film of Ni supported on glassy carbon (nm-Ni/GC) was prepared by electrochemical deposition through cyclic voltammetry (CV). The properties of nm-Ni/GC were studied by electrochemicalin situ FTIR reflection spectroscopy using CO adsorption as probe reaction. It has revealed that the nm-Ni/GC exhibits abnormal infrared effects (AIREs). The study has extended the investigation of the AIREs that we have discovered initially on nanostructured film materials of platinum group metals and alloys to nanostructured film materials of iron group metals.