BaFe2As2 (Ba-122) and (Ba0.6K0.4)Fe2As2 (K-doped Ba-122) powders were successfully synthesized from the elements using a reaction method, which incorporates a mechanochemical reaction using high-impact ball milling. Mechanically-activated, self-susta
ining reactions (MSR) were observed while milling the elements together to form these compounds. After the MSR, the Ba-122 phase had formed, the powder had an average grain size < 1 {mu}m, and the material was effectively mixed. X-ray diffraction confirmed Ba-122 was the primary phase present after milling. Heat treatment of the K-doped MSR powder at high temperature and pressure yielded dense samples with high phase purity but only granular current flow could be visualized by magneto optical imaging. In contrast, a short, low temperature, heat treatment at ambient pressure resulted in global current flow throughout the bulk sample even though the density was lower and impurity phases were more prevalent. An optimized heat treatment involving a two-step, low temperature, heat treatment of the MSR powder produced bulk material with very high critical current density above 0.1 MAcm-2 (4.2 K, 0 T).
In order to understand why the inter- and intra-granular current densities of polycrystalline superconducting oxypnictides differ by three orders of magnitude, we have conducted combined magneto-optical and microstructural examinations of representat
ive randomly oriented polycrystalline Nd and Sm single-layer oxypnictides. Magneto optical images show that the highest Jc values are observed within single grains oriented with their c axes perpendicular to the observation plane, implying that the intragranular current is anisotropic. The much lower intergranular Jc is at least partially due to many extrinsic factors, because cracks and a ubiquitous wetting As-Fe phase are found at many grain boundaries. However, some grain boundaries are structurally clean under high resolution transmission electron microscopy examination. Because the whole-sample global Jc(5K) values of the two samples examined are 1000-4000 A/cm2, some 10-40 times that found in random, polycrystalline YBa2Cu3O7-x, it appears that the dominant obstruction to intergranular current flow of many present samples is extrinsic, though some intrinsic limitation of current flow across grain boundaries cannot yet be ruled out.
Early studies have found quasi-reversible magnetization curves in polycrystalline bulk rare-earth iron oxypnictides that suggest either wide-spread obstacles to intergranular current or very weak vortex pinning. In the present study of polycrystallin
e samarium and neodymium rare-earth iron oxypnictide samples made by high pressure synthesis, the hysteretic magnetization is significantly enhanced. Magneto optical imaging and study of the field dependence of the remanent magnetization as a function of particle size both show that global currents over the whole sample do exist but that the intergranular and intragranular current densities have distinctively different temperature dependences and differ in magnitude by about 1000. Assuming that the highest current density loops are restricted to circulation only within grains leads to values of ~5 MA/cm2 at 5 K and self field, while whole-sample current densities, though two orders of magnitude lower are 1000-10000 A/cm2, some two orders of magnitude higher than in random polycrystalline cuprates. We cannot yet be certain whether this large difference in global and intragrain current density is intrinsic to the oxypnictides or due to extrinsic barriers to current flow, because the samples contain significant second phase, some of which wets the grain boundaries and produces evidences of SNS proximity effect in the whole sample critical current.
