Nickel-free titanium alloys are a promising research direction in the field of biomedical materials. Current literature reports indicate that there is a possibility of using the Ti-Ta alloys in medicine since these alloys have had satisfactory results as far as biocompatibility, resistance to corrosion and mechanical properties are concerned, which is an important aspect while considering the use of this alloy for long-lasting bone implants. This article presents the results of a high-energy milling process with the use of Ti and Ta powders. The ball-milling process was carried out for various times, including 20, 40, 60, 80, and 100 h. The samples were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The research confirmed partial synthesis of the materials during the process of high energy ball milling.