The high quality and smooth micro and nanocryslalline dual layer composile diamond films were successfully prepared using H-2/CH4/Ar/CO2 plasma with a synthesis process of nucleation/MCD growth/nucleation/NCD growth. The carbon dioxide content is demonstrated to be important in controlling the NCD layer grain size and growth rate. The influences of carbon dioxide concentration on the morphology, microstructure and growth rate of the deposited NCD layer are investigated by using scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy, It is found that the additional carbonaceous sources supplied by CO2 are favourable to increase the growth rate, and meanwhile, the oxygen related species generated would enhance the etching effect not only to eliminate the non-diamond phase of NCD but also to decrease the growth rate. The appropriate addition of CO2 can increase he high quality and growth rare, decrease the surface roughness it is demonstrated that adding CO2 strongly affects the contents of various reaction species in plasma, which would determine the growth features of NCD layers. The deposited highly smooth and quality micro-/nano-crystal layered diamond film is also expected to be applicable in surface aroustic wave (SAW) devices and microelectromechanical systems (MEMS). (C) 2014 Elsevier B.V. All rights reserved.