(57)Fe transmission Mossbauer spectroscopy and X-ray diffractometry were used to study alpha- and beta-polymorphs of iron phthalocyanines (FePc) to get information about their oxygenation in connection with controlled pyrolysis of flat layered phthalocyanines initiated by radicals at relatively low temperatures, to form acicular carbide particles encaged in carbon. Mossbauer spectroscopy and XRD revealed that the oxygenation of both alpha- and beta-polymorphs of FePc was successfully achieved. New Mossbauer spectral components (doublets) appeared upon the oxygenation in both alpha and beta FePc. This can be attributed to iron microenvironments containing oxygen between the layers of iron phthalocyanines.
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