The stacking order of graphite layers in mesocarbon microbeads (MCMB5) heat-treated between 700 and 3000°C was examined by analyses of x-ray diffraction measurements, and lithium insertion into the MCMBs has been observed using solid-state ti-nuclear magnetic resonance (7Li-NMR) spectroscopy. In MCMTBs heat-treated above 2000°C, the fully lithiated MCMBs showed two bands at ca. 45 ppm (vs. LiC1) and ca. 27 ppm in their 7Li-NMR spectra. The profile of the band at 45 ppm was very close to that for the first-stage lithium graphite intercalation compound (Li-GIC), though the other band at 27 ppm could not be assigned to any phases of Li-GICs. From these results, it is suggested that the structures of the MCMBs heat-treated above 2000°C for lithium insertion are classified as graphitic structure, which has the AB stacking order of graphite layers, and turbostratic structure with a random stacking sequence of graphite layers; the fully lithiated compositions of both structures were estimated as LiC6 and ca. Li,2C6, respectively. Although MCMB heat-treated at 700°C gave a higher capacity than LiC6, the line shift in the 7Li-NMR spectra indicated that lithium stored in the MCMB displayed an ionic character. Capacity change of the MCMBs during charge-discharge cycling up to 20 cycles and capacity loss at higher current densities (< 200 mA g') were also examined.) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 128.122.253.228 Downloaded on 2015-02-06 to IP