CdxZn1-xS nanocrystals were synthesized by mechanochemical solid state route in a planetary laboratory mill. Structural, surface and morphological properties were investigated by XRD, XPS, SEM and TEM methods. Mechanochemical synthesis produced uniform particles with respect to microstructure. Surface weighted crystallite sizes approximately of 2 nm were calculated from XRD data by application of Warren-Averbach method. The observation of S(2p), Cd(3d) and Zn(2p) peaks in XPS spectra shows existence of CdZnS nanocrystals on the surface of samples. The SEM measurements show the aggregates of small nanocrystals. The TEM method confirms the aggregate formation of CdxZn1-xS nanocrystals with the sizes 5-10 nm. The CdxZn1-xS nanocrystals are obtained in the simple synthesis step, making the process attractive for industrial applications. (c) 2008 Elsevier B.V. All rights reserved.