CaFe2O4 nanocrystalline powders were synthesized through sol-gel treatment in which the stoichiometric mixing of various nitrates involving calcium and iron in presence of citric acid was performed. Subsequently, the as prepared sample was annealed at various temperatures in order to obtain the fine distribution of size including the bulk counterpart. The samples were then characterized using powder X-ray diffraction followed by Fe-57 Mossbauer spectroscopy, SQUID as well as vibrating sample magnetometry. The results of spectroanalyses revealed that the samples were formed in single phase cubic spinel structure and exhibits room temperature superparamagnetism, except the bulk one, which crystallizes in characteristic orthorhombic structure of CaFe2O4 and displays trivial coercivity and remanent magnetization at room temperature. (C) 2012 Elsevier B. V. All rights reserved.