Hollow carbon nitride microspheres have been synthesized using a novel liquid phase electrodeposition technique. The microspheres are composed of numerous nanoparticles with size of about 5-30 nm. The diameters of the spheres range from 800 nm to 1.1 mu m, and shell thickness is about 80-250 nm. This is the first attempt to synthesize carbon nitride with specific nanostructure by the electrodeposition method, which is proved to be facile and effective, and can be performed in an atmospheric environment and at a rather low temperature. The hollow carbon nitride may have potential applications as lubrication, catalysis, biomolecule adsorption, drug delivery, electronic materials, etc. in the future. (C) 2009 Elsevier B.V. All rights reserved.