Abstract
A high-energy ball milling technique was used for production of the equiatomic NiTi alloy. The grinding batch was prepared in two quantities of 10 and 20 g. The alloy was produced using various grinding times. Scanning electron microscopy, X-ray diffraction, hardness measurement and differential scanning calorimetry were used for materials characterization at various milling stages. The produced alloy was studied by means of microstructure, chemical and phase composition, average grain and crystallite size, crystal lattice parameters and microstrains. Increasing the batch mass to 20 g and extending the grinding time to 140 h caused the increase in the average size of the agglomerates to 700 µm while the average crystallites size was reduced to a few nanometers. Microstrains were also reduced following elongation of milling time. Moreover, when the grinding time is extended, the amount of the monoclinic phase increases at the expense of the body-centered cubic one—precursors of crystalline, the B2 parent phase and the B19′ martensite. Crystallization takes place as a multistage process, however, at temperatures below 600 °C. After crystallization, the reversible martensitic transformation occurred with the highest enthalpy value—4 or 5 J/g after 120 and 140 h milling, respectively.
Highlights
Even though more than 60 years have passed since discovering the shape memory effect, NiTi alloy is still at the top of interest [1,2]
The first visible sign of the influence of the grinding conditions on the alloy formation is the change in grain size of the alloying element powders and grains of newly formed alloy
Adjusting the grinding time to 100 h resulted in a temperature shift in the range of crystallization
Summary
Even though more than 60 years have passed since discovering the shape memory effect, NiTi alloy is still at the top of interest [1,2]. The effect of increased batch weight and extended grinding time was analyzed based on the measured diffractograms for powders in the state after direct grinding. Regardless of the grinding time, the lattice parameter of the nickel-based solid solution was much higher than in the ICDD file (Figure 5a).
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