Extracting the composition of nanocrystals of mechanically alloyed systems using Mössbauer spectroscopy

Determining the composition at the nanoscale generally requires the use of experimental techniques such as 3D atom probe or nanoanalysis, which have limited availability, involve high economic cost and, moreover, imply aggressive sample preparations. However, the combination of Mössbauer spectrometry (MS), X-ray diffraction (XRD) and magnetization measurements can supply very detailed information on the average values of composition of tiny elements of the microstructure such as nanocrystals and boundary regions. Unlike nanoscale techniques, those techniques are widely accessible to most of the scientific community and do not require any special sample preparation, especially for powder samples. Two methods are proposed: the first method uses the ratio between the high field contributions to the MS spectra to extract the composition of the nanocrystals and allows us to follow its evolution; the second method uses average values of the hyperfine field and XRD data to study nanocrystalline samples. These procedures have been applied to two FeNb(B) powder samples obtained by mechanical alloying. The proposed procedures can be easily extended to systems containing other isotopes suitable for Mössbauer spectroscopy or to data from nuclear magnetic resonance experiments.