In this paper, a rapid and simple approach was developed for the preparation of zinc pentacyanonitrosylferrate nanotubes (ZnPCNF NTs) within the cylindrical pores of anodic aluminum oxide (AAO) template by electrochemical method. The AAO was fabricated in two steps anodizing from aluminum foil. The first anodization of aluminum foil was performed in 0.2 mol L-1 H2C2O4 followed by removal of the formed porous oxide film by a solution of 6 wt% of phosphoric acid. The second anodization step was then performed using the same conditions as the previous step. Scanning electron microscope (SEM) and X-ray diffraction (XRD) method were employed to characterize the resulting highly oriented uniform hollow tube array which its diameter was in the range of 25-75 nm depending on the applied voltage and the length of nanotubes was equal to the thickness of AAO which was about 2 ?m. The growth properties of the ZnPCNF NTs array film can be achieved by controlling the structure of the template and applied potential across the cell.