Polyacrylonitrile (PAN) is well-known to undergo structural changes in the presence of oxygen at high temperatures as shown in Scheme I. Recent attention is focused on surface or interfacial reactions between PAN and metals. An ex-situ infrared reflection-absorption study of PAN films obtained by electropolymerization on a nickel substrate showed that cyclization had been completed after 24 h at 200 °C, reticulation had been completed at 300 °C, and dehydrogenation and denitrogenation started well above 300 °C.2 An XPS and IR study of PAN films on aluminum and copper surfaces illustrated that a double-coupled conjugated system (III in Scheme I) was formed after pyrolysis on A1 at 300 °C or on Cu at 200 0C for 2 h.3 These temperatures are respectively about