In recent years, the fabrication of ultra thin films of redox compounds received considerable interest in materials chemistry[ I ]. The film thickness controllability, coinposit ion and in net ional adjustability at an atomic or molecular level are effective parameters in activity and stability of redox materials. As a result polyoxornetalate have become promising candidates for Functional ultra thin films on a variety of substrate surFuces due to rich redox chemistry and catalytic ability[2-4]. In the present study, novel kind of multilayer flrn containing silicornolybdates and transition metal complexes of Ru, Fe, and Cu was achieved on glassy carbon electrode modified with single & multi wall carbon nanotubes The elcctrochemical behavior of niultilayer film has been studied by cyclic voltammetry in aqueous solution. Moreover, stability and redox activity of’ the modiFied him in different pH values were investigated. The results indicates stability of the multilayer hIm increases with increasing the number of anion and cation layers and decreases with increasing pH. Due to the high stability, fast electron transfer rate constant and multi-redox site of the immobilized redox film, the modified electrode can be used as an excellent electron transfer mediator in electrocatalytic reaction, electrocatalysis. sensors and biosensors fabrication.