Hybrid alternate layered films of transition metal dichalcogenides and amphiphilic compounds were prepared by Langmuir-Blodgett (LB) technique. The conductivity at room temperature depended on the transition metal dichalcogenide species, showing the highest value for the hybrid LB films of MoS2 system. This methodology was successfully applied to the fabrication of the hybrid LB films using various organic amphiphiles such as cyanine dyes, phthalocyanines, azobenzene, and ferrocene derivatives, The conductivity depended on the interlayer spacing: the conductivity decreased with increasing interlayer spacing of the film. The highest electrical conductivity of the hybrid LB films was over 100 Scm(-1).