Effect of boron milling on phase formation and critical current density of MgB2 bulk superconductors

This study was carried out to investigate the effect of milling of boron (B), which is one of raw materials of $MgB_2$, on the critical current density ($J_c$) of $MgB_2$. B powder used in this study is semi-amorphous B (Pavezyum, Turkey, 97% purity, 1 micron). The size of B powder was reduced by planetary milling using $ZrO_2$ balls (a diameter of 2 mm). The B powder and balls with a ratio of 1:20 were charged in a ceramic jar and then the jar was filled with toluene. The milling time was varied from 0 to 8 h. The milled B powders were mixed with Mg powder in the composition of (Mg+2B), and the powder mixtures were uniaxially pressed at 3 tons. The powder compacts were heat-treated at $700^{\circ}C$ for 1 h in flowing argon gas. Powder X-ray diffraction and FWHM (Full width at half maximum) were used to analyze the phase formation and crystallinity of $MgB_2$. The superconducting transition temperature ($T_c$) and $J_c$ of $MgB_2$ were measured using a magnetic property measurement system (MPMS). It was found that $B_2O_3$ was formed by B milling and the subsequent drying process, and the volume fraction of $B_2O_3$ increased as milling time increased. The $T_c$ of $MgB_2$ decreased with increasing milling time, which was explained in terms of the decreased volume fraction of $MgB_2$, the line broadening of $MgB_2$ peaks and the formation of $B_2O_3$. The $J_c$ at 5 K increased with increasing milling time. The $J_c$ increase is more remarkable at the magnetic field higher than 3 T. The $J_c$ at 5 K and 4 T was the highest as $4.37{\times}10^4A/cm^2$ when milling time was 2 h. The $J_c$ at 20 K also increased with increasing milling time. However, The $J_c$ of the samples with the prolonged milling for 6 and 8 h were lower than that of the non-milled sample.