PHASE FORMATION AND SUPERCONDUCTIVITY OF Fe-TUBE ENCAPSULATED AND VACUUM-ANNEALED MgB2
We report optimization of the synthesis parameters viz. heating temperature (TH), and hold time (t hold ) for vacuum-annealed (10-5 Torr) and LN 2 (liquid nitrogen) quenched MgB 2 compound. These are single-phase compounds crystallizing in the hexagonal structure (space group P 6/mmm ) at room temperature. Our XRD results indicated that for phase-pure MgB 2, the TH for 10-5 Torr annealed and LN 2-quenched samples is 750°C. The right stoichiometry i.e., MgB 2 of the compound corresponding to 10-5 Torr and TH of 750°C is found for the hold time (t hold ) of 2.30 hours. With varying t hold from 1–4 hours at fixed TH (750°C) and vacuum (10-5 Torr), the c-lattice parameter decreases first and later increases with t hold (hours) before a near saturation, while the a-lattice parameter first increases and later decreases beyond a t hold of 2.30 hours. The c/a ratio versus t hold plot showed an inverted bell-shaped curve, touching the lowest value of 1.141, which is the reported value for perfect stoichiometry of MgB 2. The optimized stoichimetric MgB 2 compound exhibited superconductivity at 39.2 K with a transition width of 0.6 K. In conclusion, the synthesis parameters for phase pure stoichimetric vacuum-annealed MgB 2 compound are optimized and are compared with widely-reported Ta tube encapsulated samples.