Glassy carbon (GC) discs and platinum microcylindrical electrodes were modified with a layer of nickel(II) tetrakis 3-methoxy-4 hydroxyphenyl porphyrin (poly-TMHPP-Ni) of different loadings (Γ) between 0.6 and 10 nmol/cm2, and subsequently with a Nafion layer. The topography and in some cases the thickness of films were measured by means of contact mode AFM. SEM and optical microscopy observations were used for the comparative studies on a larger scale. The useful range of the coverage with modifying polymer was investigated. The optimal value of loading for the sensor was found to be in the range of 6-8 nmole of poly-TMHPP-Ni per cm2. We observed the Nafion layer uniformity in nanometric scale.