Monocrystalline fibres of undoped PrAlO3 and PrAlO3:0.1 Mn, have been grown by the pulling-down method under nitrogen atmosphere. The as-grown crystal doped with Mn had a visible brown core surrounded by a green ring, whereas this effect was weaker for the undoped PrAlO3. A coloration of the brown core was caused by a presence of Pr4+ ions. The presence of the Pr4+ ions was confirmed by XPS and magnetic studies. The XPS chemical analysis showed the increased concentration of oxygen in the crystals with the brown core. The most probable valency of manganese is Mn4+. It is located in Al3+ sites.
The Pechini sol-gel method was applied to obtain LiMn2–xTxO4 (T = Ni, Fe; x = 0.1 to 0.5) nanopowders. Crystal and electronic structures, chemical composition and magnetic properties of the materials were characterized by X-ray diffraction, XPS, SEM/EDX microscopy, prompt gamma-ray activation analysis (PGAA), Mössbauer spectroscopy and magnetic susceptibility, respectively. XRD measurements showed that the LiMn2–xNixO4 were single phase for x = 0.1 and 0.2. Three samples with higher Ni content contained some addition of a second phase. Analysis of the oxidation state of the dopants by XPS revealed ionic Ni2+ and Fe3+. Mössbauer spectroscopy also confirmed 3+ oxidation state of iron and its location in octahedral sites, which excluded the inverse spinel configuration. XPS examinations showed that Mn3+ ions dominated in the iron substituted series whereas the Mn4+ was dominant in the nickel series.