In this work, effect of various process-control agents (PCAs) on the mechanical alloying of amorphous alloy of $Al_{85}Y_8Ni_5Co_2$ has been investigated. The dependence of the particle shape, size and crystallization behavior of the amorphous alloy powders on the type of PCAs and their concentrations was investigated by using X-ray diffraction, field-emission scanning electron microscopy and differential scanning calorimetry. It was found that the additive of toluene could affect positively the amorphization and thermally induced crystallization processes, as well as the size refinement, morphology and particle-size distribution of as-milled powders in comparison with alloy obtained without PCA.