R. Kostecki et al., RAMAN-SPECTROSCOPY AND ELECTRON-MICROSCOPY OF HEAT-TREATED PETROLEUM COKES FOR LITHIUM-INTERCALATION ELECTRODES, Journal of the Electrochemical Society, 144(9), 1997, pp. 3111-3117
Raman spectroscopy, coupled with high-resolution transmission electron
microscopy (HRTEM) and x-ray diffraction analysis, were used to chara
cterize the physical properties of carbonaceous materials obtained by
heat-treatment of petroleum coke at 1800, 2100, and 2350 degrees C. Th
e effects of heat-treatment and air milling process (to obtain an aver
age particle size of 10 mu m) on the physical and microstructural prop
erties of the carbon particles were examined. The Raman intensities of
the D and G bands were used to estimate the crystallite size, L-a, an
d x-ray diffraction was used to obtain L-c and the d(002) spacing of t
he petroleum cokes. Heat-treatment of the petroleum coke at temperatur
es above 2100 degrees C produces a L-a value of about 100 Angstrom, in
terplanar distance, L-c, of >600 Angstrom, and d(002) spacing of 3.358
Angstrom, close to that of graphite. HRTEM showed that a distinct ord
ering of the layer planes occurs with heat-treatment, and a perceptibl
e difference in the surface morphology is evident with petroleum coke
that is heat-treated at 2350 degrees C and then air milled. The electr
ochemical results for lithium intercalation/deintercalation of the pet
roleum cokes in 0.5 M LiN(CF3SO2)(2)/ethylene carbonate:dimethyl carbo
nate electrolyte revealed that heat-treatment at 2350 degrees C improv
es the reversible Li storage capacity of the petroleum coke, and that
air milling after heat-treatment produces a petroleum coke with high r
eversible capacity, equivalent to Li0.93C6.