Molten salts are well thought-out as the incredibly promising medium for chemical and electrochemical synthesis of compounds. Hence a stab has been made on the electrochemical synthesis of CeB6 using molten salt technique. The electrolyte consisted of lithium fluoride (LiF), boron trioxide (B2O3) and cerium chloride (CeCl3) Electrochemical experiments were carried out in an inconal reactor in an argon atmosphere. Electrolysis was executed in a high-density graphite crucible, which doles out as the electrolyte clutching vessel as well as the anode. The cathode was made up of a molybdenum rod. The electrolysis was carried out at 900 degrees C at different current densities intended for the synthesis of CeB6 crystals. After the electrolysis, the cathode product was removed and cleaned using dilute HCl solution. The crystals were scrutinized by X-ray diffraction (XRD) to make out the phase and the purity. It has been observed that CeB6 crystals are synthesized at all current densities and the product has traces of impurities. (C) 2008 Elsevier B.V. All rights reserved.