As part of a continuing investigation on the characterization of rapidly solidified alloys, the present report describes the results of the study of the various phases observed in rapidly solidified aluminum rich, aluminum- iron alloys. Two experimental techniques, transmission electron microscopy (TEM) and nuclear gamma-ray resonance (NGR) were used to obtain valuable data and information on the microstructure and composition of selected alloys. The aluminum alloys described in this report cover a broad range of iron concentrations and consist of samples in the Fe 1 weight precent to 34 weight precent range. The interesting features of the microstructure are discussed also in these terms. Aluminum-iron alloys with 18 weight precent Fe were subjected to a series of heat treatments in order to evaluate the thermal stability of the phases. Special care has been exercised in reproducing teh microphotographs in order to preserve for the reader the unique microstructural details captured in the original observations.