A method is described for the electrochemical and in situ Raman spectroscopy characterization of particles of graphite and other carbonaceous materials used as lithium intercalation battery anodes. This method relies on high-pressure embedding of such particles on thermally annealed Ni foils and therefore does not require binders or other additives that may interfere with the electrochemical and spectroscopic behavior. The results obtained with embedded KS-44 graphite and MCF28 carbon microfibers in 1 M LiClO4 in 1:1 (by volume) ethylene carbonate/diethyl carbonate mixtures yielded cyclic voltammetric and in situ Raman features that were in very good agreement with those reported by others for similar materials using more conventional electrode formulations. (C) The Electrochemical Society. S1099-0062(00)01-054-3. All rights reserved.