The MnO
2/CMSs composite was obtained by coating MnO
2 onto the surface of carbon microspheres (CMSs), which were prepared by chemical vapor deposition and oxidized by a mixture of 0.1 mol/L KMnO
4 and 0.1 mol/L HNO
3. And then MnO
2/CMSs composite was washed by H
2C
2O
4 to obtain oxidized-CMSs. The morphology and structure of all samples were characterized by FESEM, TEM, XRD and so on. The dispersion of MnO
2/CMSs in water and ethanol was also investigated. The electrochemical property of the composite was measured by cyclic voltammetry. The results show that the MnO
2/CMSs composite with appropriate capacitance performance in neutral solution was synthesized using in-situ coating technique in KMnO
4 and HNO
3 solution, the loading of MnO
2 in the composite was about 60%, and the oxidized-CMSs with oxygen-containing functional groups on their surface have good dispersion in water and ethanol.