Diamond spherical shell thick film was prepared by high power DC-plasma jet CVD. Atom force microscopy, scanning electron microscopy, Raman spectroscopy and roughness-profile-meter were used to characterize microstructure, morphology, impurities and orientation evolution of diamond spherical shell thick film. The results show that, when nucleation begins, grains grow random orientation. The grain size of spherical diamond film prepared is compact, clear, uniform, continuous and no remarkable bigger grain over the whole surface of film. On the growth surface, (100) facets were dominant, and the cross-section SEM indicated that film columnar spreading grew from the substrate surface to the diamond film surface. The roughness of the growth surface was much more than that of the nucleation surface. To adjust some important parameters as methane concentrate, depositing time, and matrix temperature, and high quality diamond spherical shell thick film was deposited.