Characterization of a chalcopyrite from Brazil by Mössbauer spectroscopy and other physicochemical techniques

We studied a chalcopyrite from a Cu ore deposit in Rio Grande do Sul, Brazil, by Mossbauer spectroscopy at room temperature and 110 K. Supporting methods to check for sample purity and to characterize further sample properties were slow-scanning X-ray powder diffraction and optical and microprobe analyses of polished sections of selected grains. Chemical analyses obtained using a scanning electron microscope equipped with an energy-dispersive X-ray spectrometer showed the sample to consist of homogeneous and essentially stoichiometric chalcopyrite (CuFeS2). Mossbauer spectra taken at both the above temperatures consist of asymmetric magnetically ordered patterns with unequal intensities of the line pairs 1–6 and 2–5, pointing to the existence of non-equivalent or multiple Fe sites. Least-squares fittings evidenced that the resonance intensity ratio of subspectrum with lower quadrupole shift (indicative of a more symmetric environment) to that with higher shift is 69:31, at room temperature, and 68:32, at 110 K. Rietveld refinement of the XRD data indicates the existence of tetragonal [a = 0.52855(1) and c = 1.0412(1) nm] and cubic [a 0 = 0.5273(2) nm] modifications in a proportion of 74:26, in good agreement with the Mossbauer data. The saturation magnetization of the sample was 32.7 J/(T kg), confirming the oxidation state of Fe as trivalent and pointing to little to no spin canting.