Mesocarbon microbeads (MCMB) are known to be one of the most important carbonaceous anode materials. In this study, novel mesocarbon microbeads (NMCMB) were prepared by two-step treatment including thermal polymerization and heat treatment under vacuum, which was then applied as anode materials for lithium ion batteries (LIBs). The morphologies, structures, and other properties of NMCMB were investigated by scanning electron microscope (SEM), X-ray diffractometer (XRD), thermogravimetric analyses (TGA), Raman spectroscopy, and N-2 adsorption-desorption isotherms. The results indicated that NMCMB had rough surface, high specific surface, and better thermal stability. After carbonized, NMCMB have relatively higher disorder degree and bigger interlayer distance. As the anode material of LIBs, NMCMB exhibit better electrochemical performance than MCMB, and provide a high reversible specific capacity of 379 mAh g(-1) at a current density of 50 mA g(-1), with almost 100% capacity retention for up to 50 cycles at 100 mA g(-1), and a good rate performance (256 mAh g(-1) at 1 A g(-1)). This synthetic method paves a new way to improve electrochemical performance of MCMB, which may expand MCMB utilizationaEuro,for LIBs.