T. Takeichi et al., CARBONIZATION AND GRAPHITIZATION OF POLYIMIDE FILMS - POLYAMIDE ACID METHYL-ESTER OF PMDA PDA AS A PRECURSOR/, Journal of applied polymer science, 61(9), 1996, pp. 1571-1578
Polyamide acid was prepared from pyromellitic dianhydride (PMDA) and p
-phenylenediamine (PDA) and was then reacted with NaH and methyl iodid
e to transform into methyl ester having various degrees of esterificat
ion. Polyamide acid methyl ester was also prepared by the polymerizati
on between FDA and acid chloride of half-ester of PMDA. The cast films
were imidized as fixed on glass substrate to give polyimide films hav
ing slightly higher tensile moduli than those from polyamide acid, sug
gesting that higher orientation along the film surface was achieved. I
t should be noted that the polyimide films prepared by the latter meth
od from the meta-rich configuration had considerably low modulus. The
polyimide films were then carbonized by heating to 900 degrees C, and
the electrical conductivity of the carbonized films was measured at ro
om temperature. It was shown that the carbonized films from methyl est
er have higher electrical conductivity than the films from correspondi
ng polyamide acid. The carbonized films were further heated to 2800 de
grees C for graphitization, and their degrees of graphitization and or
ientation of the graphite crystallite as a function of esterification
ratio were studied by x-ray diffraction measurement at room temperatur
e and magnetoresistance measurement at liquid nitrogen temperature. Bo
th measurements clearly indicate that the graphite films prepared from
polyamide acid methyl ester have high degrees of graphitization and o
rientation. (C) 1996 John Wiley & Sons, Inc.