It is important to control the martensitic transformation start temperature (Ms) of Ti–Ni alloys because it determines the temperature range over which the shape memory effect and superelasticity appear. Powder metallurgy (PM) is known to provide the possibility of material-saving and automated fabrication of at least semi-finished products as well as net-shape components for NiTi alloys. In this study powder with different particle sizes was subjected by gas atomization. The evolution of the control the martensitic transformation start temperature (Ms) was studied by differential scanning calorimetry. The effect of the particle size of powders on the transformation temperatures behaviors was discussed.