High-purity, single-phase CdSiP2 polycrystalline materials were synthesized directly from the constituent elements by a new method without graphite boat sealed in silica ampoule. The problem of explosions was solved by careful control of the heating and cooling cycle and adopting the two-zone rocking furnace with specially designed temperature profile. Mechanical and temperature oscillations as well as gradient cooling were introduced in the synthesis process. The mechanism and advantages of this new method are discussed. X-ray diffraction (XRD) analysis and Energy dispersive X-ray (EDX) microanalysis both indicated that the synthesized compound is high-quality CdSiP2 polycrystalline material. (C) 2011 Elsevier B.V. All rights reserved.