Abstract: Carbon micro-spheres were prepared by a simple solvothermal route in a stainless steel autoclave. Absolute ethanol was used as carbon source and solvent, and nickel as catalyst, obtained by reducing Ni(Ac)₂ in absolute ethanol. Carbon microspheres were obtained at 500 °C for 48h. The samples were characterized by X-ray powder diffractometer, scanning and transmission electron microscopy, and Raman spectroscopy. Results showed that there were acicular and spherical carbon particles in the as-prepared samples. The carbon microspheres had diameters ranging from 1 to 2 μm. and the acicular particles had diameters ranging from 1 to 2 μm and lengths ranging from 3 to 6 μm. The yield of carbon micro-spheres was over 95% with a narrow size distribution and perfect shape.