An ionic graphite intercalation compound (GIG) with FeCl4- was prepare
d electrochemically under controlled charge from an FeCl3/HCl solution
using highly oriented pyrolytic graphite (HOPG) and a graphitized pol
yimide him as hosts. From the X-ray diffraction (XRD) 001 lines, the s
tage of the GIC was determined and the unstable properties of the samp
les were examined. Gradual transformation of stage-s GIC to stage-(s 1) GIC confirmed their instability after exposure to air or pumping u
nder vaccum at 120 degrees C. Thermogravimetry analysis of the samples
and IR spectra of the gas evolving during GIC drying allowed the quan
titative estimation of the co-intercalated species (H2O, HCl) and, hen
ce, the formula of the second-stage GIC was established to be C20-36+F
eCl4-, 1.5H(2)O, 0.5HCl. Electrochemical reduction of the second-stage
FeCl4--GIC to higher stages and/or Fe-0 particles dispersed on exfoli
ated graphite was performed in aprotic solution. The influence of co-i
ntercalated molecules on the reduction behaviour of FeCl4--GIC is disc
ussed.