Effect of small changes of the composition on the crystallization process of a quaternary AlMmNi(Co,Fe) alloy series (Mm = mischmetal) obtained in amorphous state by melt-spinning technique, is studied using differential scanning calorimetry (DSC) and X-ray diffractrometry (XRD). Devitrification process takes place in several steps for all the studied alloys. Nanocrystalline microstructure appears during the first transformation stage detected by DSC. This microstructure has been characterized by XRD as nanocrystals of α-Al phase embedded in an amorphous matrix. Average grain size, D is about 15-20 nm (estimated using Scherrer formula) and crystalline volume fraction, X_C = 50-80 %. The highest X_C was found for the lowest Mm containing alloy. Annealing above the second and third transformation stages produces fully crystallized samples. At this stage only equilibrium phases were detected: α-Al, orthorombic Al₁₁Mm₃ and orthorombic Al₃Ni. Kinetics of nanocrystallization was studied in terms of non-isothermal approaches (Kissinger, Augis-Bennet, Gao-Wang and Ozawa methods). Activation energy of nanocrystallization, E_a ranges from 1,5 to 2,7 eV. The highest values were found for the alloys with the lowest Al content. Combining Gao-Wang and Ozawa methods, an idea of the value of Avrami expoinent, n, at the early (Gao-Wang) and final (constant value in Ozawa) stages of nanocrystallization is obtained: n decreases from 1-1.5 to 0.5.

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