Mesocarbon microbeads (MCMB) with narrow size distribution, excellent sphericity and no obvious conglutination have been prepared with a coal tar pitch containing quinoline insolubles (QI) as the raw material. Optical microscopy and scanning electron microscopy (SEM) are used to examine the structure of the MCMB. It has been found that SEM technique shows the structural information of MCMB clearly in the form of micrographs even when the structure of MCMB is complex, while the optical technique is useful for analysis of the regular structure of the mesophase spheres but cannot be effectively used to analyze either the complex structure of the green MCMB or the structures of the further heat-treated ones at different temperatures. According to the characteristics of the carbon layers, the structures of the as-prepared MCMB in the present experiment could be classified as (1) Parallel Layer type structure and (2) Bent Layer type structure with the carbon layers gathering at one or two points in the MCMB. In the experiments, SEM is also utilized to investigate the structures of MCMB that are heat-treated at different temperatures. It has been found that the MCMB without any further heat-treatment show no layered-carbons, while the ones heat-treated at temperature higher than 1000℃ exhibit obvious layered carbons across their sections. When increasing the heat-treatment temperature, the carbon layers become thinner and flatter.