NiTi Single Crystal Growth by Micro-Pulling-Down Method: Experimental Setup and Material Characterization

TL;DR

This paper introduces a micro-pulling-down method to grow NiTi single crystals, enabling detailed phase transition studies and precise doping, with comprehensive material characterization demonstrating its effectiveness.

Contribution

The study presents a novel micro-pulling-down apparatus for NiTi single crystal growth, allowing controlled doping and detailed characterization of phase transitions.

Findings

Successful growth of NiTi single crystals using the $$PD method.

Detailed characterization confirms high-quality crystals with well-defined phase transitions.

The method reduces oxygen contamination, improving crystal purity.

Abstract

Nickel-titanium that has an austenite to martensite phase transition has been studied extensively in the past as a shape memory alloy, but a lot remains to be learned from such phase transitions. However, single crystals are needed for a detailed characterization of the emerging phase transition. In order to produce NiTi single crystals for research purposes, we have set up a micro-pulling-down ($\mu$PD) apparatus. The $\mu$PD process is a fast and flexible method for the fabrication of small single crystals. The apparatus is operated in vacuum. By pulling the crystal down through a hole in the crucible bottom, it is possible to reduce oxygen contamination, since oxides float on top of the melt due to their low density. Here we present a detailed characterization of as-grown NiTi crystals by electron backscatter diffraction (EBSD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), hot gas extraction method and differential scanning calorimetry (DSC). The characteristics of the phase transition in NiTi are very sensitive to dopants and alloying. The $\mu$PD method facilitates the introduction of different doping elements into the crystal.