Kinetics analysis for the sintering of bulk MgB₂ superconductor

The pertaining kinetic characteristics during the sintering of bulk polycrystalline MgB₂ superconductors is essentially important for the improvement of properties. Here Differential Thermal Analysis was adopted to record the heat effect during the preparation of bulk MgB₂ samples. The reaction between Mg and B powders starts before the melting point of pure Mg and the evolution for the fractions of MgB₂ were determined as a function of sintering temperatures. After fitting with different kinetic mechanism functions assumed, the sintering process of bulk MgB₂ superconductors was attributed to a solid-state interface-reaction controlled mechanism with an apparent activation energy of 4.54 × 10⁵ J mol⁻¹. Combined with microstructural observations by scanning electron microscopy and phase identification by X-ray diffraction, the formation process of MgB₂ phase was classified into two different stages: (i) solid-solid reaction stage, in which Mg and B powder starts to react and the growth of MgB₂ grain is restricted by the pinning effects of pores; (ii) solid–liquid reaction stage, in which the molten Mg melt promotes the reaction process and the regular hexagon bulk MgB₂ grain forms in a solution-reprecipitation and growth mode.