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We have investigated the microstructure, normal-state electrical connectivity, and critical current density of ex-situ MgB2 polycrystalline bulks prepared by systematically varying the sintering conditions under low pressure. Samples heated at a high temperature of ~900{deg}C for a long period showed an increased packing factor, a larger intergrain contact area, and a significantly enhanced electrical connectivity, all of which indicate solid-state self-sintering of MgB2. Sintered ex-situ MgB2 bulks from a laboratory-made ball-milled powder exhibited a greatly enhanced connectivity of 28%, which is the highest connectivity of pressureless ex-situ MgB2 bulks, wires, and tapes. Surprisingly, grain growth did not occur during long-duration (~100 h) sintering in the sintered ex-situ MgB2 bulks. This is in marked contrast to in-situ processed MgB2 samples for which significant grain growth occurred during heat treatment at ~900{deg}C, producing grains that are several tens of times larger than the initial boron grains. Consequently, the critical current density as a function of the external magnetic field at 20 K progressively improved with sintering due to the relatively small grain size and good intergrain connectivity. We thus conclude that solid-state self-sintering is an effective approach for producing strongly connected, dense ex-situ MgB2 polycrystals without grain growth.
We have discovered a new homologous series of iron pnictide oxides (Fe2As2)(Can+2(Al,Ti)nOy)[n = 2,3,4]. These compounds have perovskite-like blocking layers between Fe2As2 layers. The structure of new compounds are tetragonal with space groups of P4 /nmm for n = 2 and 4 and P4mm for n = 3, which are similar to those of (Fe2As2)(Can+1(Sc,Ti)nOy)[n = 3,4,5] found in our previous study. Compounds with n = 3 and 4 have new crystal structures with 3 and 4 sheets of perovskite layers, respectively, including a rock salt layer in each blocking layer. The a-axis lengths of the three compounds are approximately 3.8 A, which are close to those of FeSe and LiFeAs. (Fe2As2)(Ca6(Al,Ti)4Oy) exhibited bulk superconductivity in magnetization measurement with Tc(onset)~36 K and resistivity drop was observed at ~39 K. (Fe2As2)(Ca5(Al,Ti)3Oy) also showed large diamagnetism at low temperatures. These new compounds indicate considerable rooms are still remaining for new superconductors in layered iron pnictides.
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