Today various types of graphene preparation are well known. The mechanical exfoliation ofHOPG graphite; nano-diamond - and SiC- based precursor methods, CVD growth using metal catalysts, such as Ni, Cu, etc. In spite that, development of new methods for fabrication of graphene - like stmctured materials is still under investigation, as a graphene families of materials prepared with different methods reveal somewhat different prope1ties. We used modified electro-chemical dispersion, called by us as electro-chemical exfoliation method, to prepare graphene containing carbon material in the state of colloid system. Luminescence studies, Raman spectroscopy, optical abso1ption, AFM, ATM, SEM and optical luminescent microscopy (OLM) were applied for characterization of both freely suspended and extracted carbon paiticles (CP) precipitated on various substrates: glass, quaitz, Si and Cu. It was shown that each precipitate is heterogeneous; it contains separated randomly padding paiticles, their aggregates and self-assembled ensembles of pa1ticles. Above placed Figure shows a set of images taken from SEM (a), ATM (b) and OLM for CP placed on Si (a, c) and Cu (b) substrates. The views of settings depend on several factors: average size of pa1ticles, material of substrate, evaporation rate and temperature. We conclude that ensemble of paiticle consists of large paiticle those posses graphite strncture and some quantity of graphene - type flaks. Photoluminescence (PL) spectra of the 1,5 investigated samples show dependences on the excitations wave lengths (see left Figure). Dependences of the PL and Raman ....: 1,0 characteristics on the concentration, pa1ticle sizes, and type of settings were also obtained and analyzed. The conclusion was made that large paiticles reveal bulk graphite Raman spectra, while small paiticles show Raman prope1ties of multilayered graphene. Moreover, just boundaiy paiticles demonstrate intensive 500 600 700 nm 800 PL radiation (see top Figure, Pait c). So, synthesized, carbon materials reveal interesting optical features and at the same time, we can state that luminescence study is a very useful analytic tool for investigation of the stmcture and physical prope1ties of micro- and nano- sized carbon materials, e.g. of graphene like cai·bon dots (flakes).