Chlorofluorocarbons (CFCs) which emitted to the atmosphere have been recognized to cause damage to the ozone layer. Alternative materials to replace the CFC's role are those which have properties of the magneto caloric effect (MCE) like Heusler alloys. In this paper, we report results of synthesis studies of the magneto caloric materials based on Ni-Mn-Al which possesses the structure of Heusler alloy. Crystallographically, the alloy is a single phase system with a general formula of X2YZ which possesses the L21 (the Strukturberichte-SB) crystal structure. An iron substituted Ni44Fe6Mn32Al18 alloy was successfully casted by means of melting in a vacuum arc melting furnace. Series of microstructure as cast alloy which studied under SEM observation and EDAX analysis reveals that the cast sample consisted of at least 4 phases. These are the main phase of Ni-Mn-Al system with the additional minor phases of Al rich, Al-oxide and Al deficit main phases, respectively. Annealing process at 900 °C in oxygen free atmosphere for 48 hours have transformed dendritic structure into equaixed grain with fine particle scattered on the entire grain surfaces.