This work is focused on graphene preparation using the segregation method with Co/SiC structure, the method being a viable low temperature synthesis approach. The graphene preparation was carried out with the cobalt layer of 300 nm thickness; the technological process is based on an optimization of parameters (temperature and duration) of annealing which is a crucial step of the synthesis. 850 C as an annealing temperature and 10 s as an annealing duration have been found to be the most optimal. The prepared graphene is close to the bi-layer graphene structure with its parameters. Structural parameters of the prepared graphene were determined from spectra obtained by Raman spectroscopy. (C) 2014 Elsevier B.V. All rights reserved.