Published online by Cambridge University Press: 15 April 2002
The complementarity between 57Fe Mössbauer spectrometry and classical methods of powder characterizations is pointed out for determining the formula of metal-ferrite composites (Fe$_p^0$Co$_{1-p}^0$)a(CoxFe$_{3-x-t}$$\square_t$O4). It is shown that X-ray diffraction is essential to determine the composition of the metal, while TG measurements in air give an approximate value for the metal ratio. In-field spectrometry is expected as the most suitable tool to determine the Fe sites occupancy, although the complex hyperfine structure might originate some misfits. The composites formulae were therefore determined by selecting the set of refined Mössbauer parameters that were in best agreement with the TG measurements. Magnetic measurements prove the validity of such an approach.