Floral-like microparticle of a binary cobalt iron cyclotetraphosphate CoFeP4O12 was synthesized through solid phase reaction using cobalt carbonate, iron metal and phosphoric acid with further calcinations at the temperature of 500 degrees C. The XRD and FTIR results indicate that the prepared CoFeP4O12 has a pure monoclinic phase without the presence of any phase impurities. The floral-like microparticle and superparamagnetic behavior of the synthesized CoFeP4O12 are important properties for specific applications, which were revealed by SEM and VSM techniques, respectively. The dominant features of the synthesized CoFeP4O12 in this work are compared with M2P4O12 (M = Co and Fe) and CoFeP4O12 reported in our previous works. (C) 2009 Elsevier B.V. All rights reserved.