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A2: Medium temperature materials
We have grown Mg2Si bulk crystals by vertical gradient freezing (VGF) method using liquid encapslants. High quality Mg2Si bulk crystal has difficulty in growing from the melt due to high reactivity of Mg, which sticks to a crucible material. In addition, the vapor pressure of Mg is high and thus it easily causes the deviation from the stoichiometric composition of Mg2Si during the melt growth at around the melting point of Mg2Si (1085oC). Furthermore, the melt growth temperature for Mg2Si is closed to the boiling point of Mg (1090oC), which may cause an explosion.
The liquid encapsulant techniques can inhibit the effects of these problems by making the layer of the encapsulant surrounding the crucibles and the crystals. In this study, the crystal growth of Mg2Si has been performed by VGF method using KCl or KCl–MgCl2 as a liquid encapsulant material. Mg (99.5%) and Si (4N) powders with Mg/Si molar ratio of 2–2.5 were put into a BN coated SiO2 or an Al2O3 crucible with encapsulant powders with MgCl2/KCl molar ratio of 0–2. Then, it was pressurized to 500 Torr with Ar gas. The temperature of the electric furnace was elevated up to 1100oC and kept for 1hour and then fallen to room temperature. When the MgCl2/KCl molar ratios were above 1 and these encapsulants were dissolved in water after the crystal growth, the grown samples were removed from the crucibles without sticking to the crucible. The samples were characterized by Raman spectroscopy, EDS, XRD and Hall effect measurements. In the Raman spectra, strong peaks can be seen at 256cm-1, which originate from Mg2Si. The samples grown at Mg/Si molar ratio of 2 exhibited Mg-poor composition. Any contaminations of the grown samples with K and Cl from encapsulants were not observed. The results of Hall effect measurements are also presented.