The mechanochemical method of synthesizing nanomaterials is known for its simple alloying technique to produce quasicrystalline and amorphous alloy phases. [1] The most tangible benefit of this method is, it does not require any heat that may adversely cause physical and chemical changes in the materials. This makes it very suitable for the synthesis of many metal alloys and ceramic composites where the prevention of any undesirable heat-induced oxidation or degradation is necessary. By optimizing milling parameters like rotational speed, ball-to-powder ratio, milling media, milling time, and also in some cases, the addition of process controlling agents, a variety of materials can be synthesized utilizing this method. Mechanochemical or mechanical alloying (MA) method for synthesizing nanomaterials involves high-energy milling technique and is generally carried out under controlled atmosphere. The major drawbacks of this method, however, are: a) discrete nanoparticles in the finest size range are difficult to prepare, and b) risks of contaminating the product from the attrition of milling media. In this method, materials go through the process of fracturing, cold welding, flattening, and fragmenting. [2] Continuous fracturing and cold welding of the milling powders during the process leads to solid state reactions between the components to form ultrafine powders of alloyed materials. The particle size distributions can be controlled by changing the aforementioned milling parameters like rotation speed, milling time, etc., and eventually nanostructured powders can be achieved effectively. [3][4][5] The syntheses of Ni-Ti-B ternary alloys from their elemental stages are not very well studied for their alloyed phase compositions and related physicochemical and mechanical properties. MA is an alternative and cost-effective method for the synthesis of these alloys with respect to the other methods, such as melt and quench process. Reviewing various features of Ni-based alloys and realizing the growing interest for Ni-Ti alloys in the vast areas of aerospace engineering and biomedical