Several methods have been tested in order to prepare the perovskite type compound MgxCyNi3 applying the mechanical alloying (MA), the self-propagating high-temperature synthesis (SHS) and the isothermal heating techniques in the different steps of preparation. These methods may be summarized as follows: method MCN-1) synthesis of the MgxCyNi3 phase through MA Of Mg2Ni (previously synthesised by isothermal heating) and selected amounts of graphite and Ni, followed by isothermal treatment; method MCN-2) synthesis of the MgxCyNi3 phase applying the SHS technique using powder compacts; method MCN-3) synthesis of an eutectic sample composed of Ni and MgNi2 by means of isothermal heating, subsequent MA with graphite and final synthesis of MgxCyNi3 by means of SHS. The methods MCN-2 and MCN-3 proved their validity to the synthesis of the desired compound with two main important results: complete conversion of the reactants into MgxCyNi3 and control of the stoichiometry in the final product. For instance method MCN-1 shows instead a very low degree of conversion of the reactants. All the phases obtained after each preparation step (MA, SHS, isothermal heating) have been characterized by means of X-ray powder diffraction (XRPD), scanning electron microscopy (SEM) coupled with electron dispersive spectroscopy (EDS). (C) 2004 Kluwer Academic Publishers.