A non-conventional way of production has been chosen to prepare Al33Ni16Zr51 amorphous alloy: mechanical alloying which allowed the microstructure of the material to be monitored. For this type of non-equilibrium alloys, the evolution toward an equilibrium state-and the crystallization kinetics were studied by differential scanning calorimetry. The crystallization processes were interpreted in terms of several theoretical models based on nucleation and growth processes.