Thin films of 5,10,15,20-Tetraphenyl-21H,23H-porphine-nickel(II) were prepared by thermal evaporation technique onto clean quartz and glass substrates. Thermogravimetric analysis, X-Ray Diffraction, Scanning Electron Microscope, Transmission Electron Microscope and Fourier transforms infrared spectroscopy were used to investigate the structural properties of the as-prepared and annealed 5,10,15,20-Tetraphenyl-21H,23H-porphine-nickel(II) films. Morphology, crystallite size and dislocation density were enhanced by annealing and included within nanometric scale. The crystallite sizes were 98 nm for powder form and 13, 41.4 and 64.7 nm for the annealed films at 373, 473 and 573 K respectively. Fourier transforms infrared spectroscopy studies released that powder, as-prepared and annealed NiTPP films were stoichiometric. The obtained films were characterized by nanostructure property. (C) 2012 Elsevier B.V. All rights reserved.