Amorphous Fe75Si15B5M5 powders with M = Ti, Ta and Zr, were synthesized by mechanical alloying and their thermal stability, crystalline state, particles morphology and magnetic properties were investigated in this study. It is found that the time to achieve amorphisation during milling increases by the substitution of any of the above transition metals 5% for silicon. The particle size distribution is dependent on the mechanical properties of the transitional metals used. Crystallisation temperature of the alloys was enhanced with up to 24% compared to the reference ternary alloy Fe75Si20B5. Magnetic measurements revealed a higher saturation magnetisation in the case of the amorphous alloy containing titanium than for the reference amorphous alloy. XRD patterns for the samples heated up to 900 degrees C reveal the presence of carbides as a result of powder contamination by the process control agent (PCA). (C) 2016 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.