A synthesis mechanism of nanoparticulate zirconia-modified Al 2-x Fe x O 3 solid solutions has been studied with the application of X-ray diffraction, IR spectroscopy, DTA, particle-size analysis and chemical analysis. The solid solutions have been prepared via heat treatment of ammonium hydroxycarbonate complexes. The nanoparticles are shown to consist of crystalline rhombohedral α-Al 2-x Fe x O 3 , monoclinic and tetragonal (M-ZrO 2 and T-ZrO 2 ). The synthesized mixed oxide offers a high polishing ability (3 to 4.5 times as high), as demonstrated in polishing of titanium, and ensures surface roughness values R a ranging between 0.019 and 0.009 μm.