Evolution of the Phase Composition in a Nickel-Predominant NiTi Shape Memory Alloy During High-Energy Ball Milling

Three alloys differing in their nominal chemical composition (Ni₅₀Ti₅₀, Ni₅₁Ti₄₉, and Ni₅₂Ti₄₈) were produced in the form of powders using high-energy ball milling. Their microstructure, morphology, structure, and phase composition were studied using the X-ray diffraction technique, scanning, and transmission electron microscopy. For the detailed structural analysis, the Rietveld method was used. The results show that each of the alloys consists of three fractions: fine, medium, and thick. The fractions varied in particle/agglomerate size from 200 nm to 800 μm. Additionally, they varied in phase composition. The fine fraction comprised a mixture of amorphous and nanocrystalline phases. Additionally, the medium and coarse phases showed crystalline solid solutions formed on the bases of nickel or titanium, as well as a crystalline <i>bcc</i> phase-a precursor of the parent phase (B2). The largest contribution in the alloy powders, over 80%, comes from the amorphous-nanocrystalline mixture (ANM). The increase in the nickel content resulted in an increase in ANM quantity of 3 wt.%. Similarly, the weight content of the titanium-based solid solution increased to about 7 wt.%. In contrast, the quantity of the nickel-based solid solution decreased from 3 wt.% to approximately 1 wt.% in the Ni₅₀Ti₅₀ and Ni₅₂Ti₄₈ alloys.