Abstract The idea to form C60/CuPc dispersed nanoheterojunctions by photoexcitation of a mixture of C60 and CuPc nanoparticles has been realized. The electronic structure of the nanoparticles and dispersed nanoheterojunctions formed in the mixture has been characterized by UV‐Vis spectroscopy and the comparing with known experimental ultraviolet photoelectron spectra and theoretical models of electronic structure of these molecules. For the mixture of C60 and CuPc nanoparticles in toluene and their coating layer on the quartz substrate the band offsets of the edges of CuPc VB and lowest unoccupied molecular orbital (LUMO) of C60 band are ΔE=1.55 eV and 1.4 eV, respectively. These results show clearly the presence of C60/CuPc dispersed nanoheterojunctions in the solution and on the quartz surface.