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 (thold) for vacuum (10-5 torr) annealed and LN2 (liquid nitrogen) quenched MgB2 compound. These are single-phase compounds crystallizing in the hexagonal structure (space group P6/mmm) at room temperature. Our XRD results indicated that for phase-pure MgB2, the TH for 10-5 torr annealed and LN2 quenched samples is 750 0C. The right stoichiometry i.e., MgB2 of the compound corresponding to 10-5 Torr and TH of 750 0C is found for the hold time (thold) of 2.30 hours. With varying thold from 1- 4 hours at fixed TH (750 0C) and vacuum (10-5 torr), the c-lattice parameter decreases first and later increases with thold (hours) before a near saturation, while the a-lattice parameter first increase and later decreases beyond thold of 2.30 hours. c/a ratio versus thold plot showed an inverted bell shape curve, touching the lowest value of 1.141 which is reported value for perfect stoichiometry of MgB2. The optimized stoichimetric MgB2 compound exhibited superconductivity at 39.2 K with transition width of 0.6 K. In conclusion, the synthesis parameters for phase pure stoichimetric vacuum annealed MgB2 compound are optimized and are compared with widely reported Ta tube encapsulated samples. 
K. P. Singh, V.P.S. Awana, Md. Shahabuddin, R.B. Saxena, Rashmi Nigam,   M.A. Ansari, Anurag Gupta,, Himanshu Narayan, S. K....