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We report the preparation of SmS@Y2O2S and Y2O2S@SmS ceramics with a core–shell nanostructure via 1123-K sulfidation of rare-earth oxides prepared by the sol–gel method, involving precipitation from starting metal nitrate solutions with NH4OH as a precipitant, followed by annealing of the resultant sulfide phases in an induction furnace at 1473 K. Using X-ray diffraction and scanning electron microscopy data, we have evaluated the average crystallite size in the materials and examined the morphology of the constituent phases in them. In addition, the short-range order in the coexisting nanostructures has been analyzed in detail using Raman spectroscopy and X-ray photoelectron spectroscopy data. [ABSTRACT FROM AUTHOR]