Manufacturing process influence on superconducting properties of MgB2 wires prepared using laboratory made boron

Abstract

Here we report a systematic study of the superconductive properties of mono-filamentary MgB2-based wires, manufactured with four different techniques. A detailed comparison of the influence of manufacturing technique and final heat treatment on superconducting properties has been given. The boron used was synthesized in laboratory following magnesiothermic reduction of boron oxide, purified thanks to several acid leaching and heat treated at high temperature, to enhance crystalline degree and remove impurities. MgB2 conductors were manufactured using the same B precursor through four different techniques (ex situ, in situ, the MgB4 or ‘mixed’ technique (half ex situ and half in situ), and reactive liquid infiltration (Rli)). Transport critical current density was measured on the best wire for each technique, considering the literature data in order to identify the corresponding best final heat treatment. Magnetic critical current density and critical temperature were investigated at different synthesis/sintering temperatures in order to evaluate their dependence to the applied final heat treatment and the data were compared. Critical current density was evaluated on short wire pieces by magnetic measurement at 5 K in a MPMS 5.5 T Quantum Design SQUID, while critical temperature was measured with a four probe system by drop of resistivity during the cooling process of the sample in a liquid helium dewar. A detailed morphological analysis is given, with void percentage evaluation and analysis of elemental Mg diffusion across the transversal cross section. X-ray diffraction was performed on MgB2 powder extracted removing each metal sheath, in order to investigate the influence of manufacturing process on the MgB2 phase. This study shows that despite the presence of a wide void within the superconducting core (due to the Mg diffusion) in the Rli sample, this manufacturing technique allows wires with higher Jc (105 A cm−2 at 3 T when heat treatment at 700 °C is applied) than other powder in tube techniques, while the highest Tc (39.2 K at the onset) can be reached by following the mixed technique, which also shows low dependence to heat treatment for both Tc and Jc. In order to establish the presence of some impurities in the lab-made B precursor energy dispersion spectroscopy analysis, inductively coupled plasma atomic emission spectrometry and X-ray analysis were performed on B.