CuS hollow spheres have been successfully synthesized through a facile microemulsion-template-interfacial-reaction route using copper naphthenate as metal precursor and thioacetamide as the source of S2-. In this way, hollow spheres could be obtained directly since the reaction of two reactants respectively dissolved in two different phases of an oil-in-water (o/w) microemulsion only occurs at the oil/water interface. Therefore, it is a key for forming hollow spheres to optimize the interfacial reaction rate by controlling reaction conditions. Furthermore, the size of the hollow spheres can be tailored by changing the content of oil phase. In this study, the average diameter of the CuS hollow spheres can be adjusted from 110 to 280 nm by changing the content of oil phase from 0.5 ml to 1.5 ml. In addition, the reaction temperature is a very important factor for forming CuS hollow spheres and the appropriate reaction temperature is about 50 degrees C. (C) 2011 Elsevier Inc. All rights reserved.