Ti50Fe45Sn5 amorphous alloys powder was prepared by mechanical alloying (MA) in a high-energy planetary ball mill. The non-crystallization degree was tested by X-ray diffraction (XRD). It was shown from the XRD results that a higher ball to powder weight ratio (BPR) is advantageous in preparing amorphous alloys powder. The microstructure and shape of the powder was observed by scanning electron microscope (SEM). It was shown from the SEM results that the as-milled amorphous alloys powder is flake shape and assembles together to be agglomeration structure, which is a typical morphology of amorphous powders prepared by MA. Thermodynamic properties and crystallization kinetics behavior of the as-milled amorphous alloys powder were measured by differential scanning calorimeter (DSC). The supercooled liquid region △Tx is broad (up to 119K) and the reduction glass transforming temperature Trg (0.78) is great, which shows that the as-milled amorphous alloys powder has a strong glass-forming ability and the thermal stability of the powder is excellent.