Purpose: The main aims of this work are the production attempt of Ni50Ti50 and Ni52Ti41Nb7 powder alloys by mechanical alloying method, the presentation of the influence of mechanical alloying time on the structure of obtained alloys and the finding of thermal effects during the heating to temperature of 700oC.Design/methodology/approach: The test material was the mixture of pure nickel, titanium and niobium powders. The powders were ground for the 5, 25 and 40 hrs. The mechanical alloying process was conducted in a high energy SPEX mill under inert argon atmosphere. The microscopic observation of the shape and size of the powdered material particles was carried out by the scanning electron microscope. The changes of the powder structure were tested by means of the X-ray diffractometer. The thermal properties of the powder alloys were examined by DSC method.Findings: Based on the presented experiment results it is clear that producing of assumption powder alloys by mechanical alloying method is possible, but special attention is needed during the selecting of process parameters. The application of used method gives possibility to produce crystalline and amorphous phase in Ni-Ti and Ni-Ti-Nb powder alloys.Research limitations/implications: The experiments in this work are made only on a laboratory scale. Further investigations should be concentrate on the developing of powder consolidation method and refinement particles during high energy ball milling.Practical implications: Ni-Ti alloys exhibit unique shape-memory effects, good corrosion resistance, high wear resistance, biocompatibility and superplasticity. Ni-Ti intermetallic compounds have been widely used in a different fields: mechanical, electric and biomedical applications, aeronautics and astronautics fields.Originality/value: The Ni-Ti and Ni-Ti-Nb powder alloys produced by mechanical alloying method can be use to produce bulk materials with desirable mechanical, physical and chemical properties.