Experimental resultson preparation of nanoparticles on the basis of GaSe crystals, analysis of structure and investigation of their electric, optical and photoluminescent characteristics are presented. Nanoparticles and thin GaSeand InSe films on a glass substrate were grown by hydro-chemical sedimentation method from a solution, containing sodium selenosulphide, gallium chloride and indium chloride. As substrates we choose a glass and GaSe crystals grown by a Bridgman method. By means of X-ray diffraction analysis (XRD), atomic force microscope (AFM), energy dispersive analysis of X-rays (EDAX), and a scanning electronic microscope (SEM) researches of the internal constitution and structure of the received samples have been conducted. Absorption spectra have been measured using JOBIN-YVON monochromator with diffraction lattice with subsequent detecting by FEU-100. Photoluminescence spectra were investigated by means of Cary Eclipse spectrophotometer. Using X-ray analysis it is established that nanoparticles belong to -modification of GaSe (а=3,75Å, с=15,94 Å) with hexagonal structure. Dependence of electrical conductivity on temperature for GaSe and InSe on GaSe substrate and current-voltage characteristics for GaSe and InSe on a glass substrate and GaSe substrate have been investigated. On the basis of spectral dependence the band-gap energy for nano-particles and activation energy for impurity the levels located in the band-gap have been defined.