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Exploring the feasibility of Fe(Se,Te) conductors by ex-situ Powder-in-Tube method

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 Added by Andrea Malagoli
 Publication date 2015
  fields Physics
and research's language is English




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In this work, the feasibility condition of Powder-In-Tube (PIT) processed wires of Fe(Se,Te) superconductor has been investigated. We faced several technical issues that are extensively described and discussed. In particular, we tested different metals and alloys as external sheaths (Cu, Ag, Nb, Ta, Ni, Fe, cupronickel, brass) concluding that the only sheath that does not affect substantially the Fe(Se,Te) phase is Fe. On the other hand, Fe sheath introduces excess iron in the Fe(Se,Te) phase, which affects the superconducting properties; we investigated the effects of the thermal treatments and of the powder composition in order to avoid it. The maximum Jc value obtained in our samples is 4*10^2 A/cm2, comparable to other published values of PIT conductors of the 11 family. We conclude that the fabrication of Fe(Se,Te) wires by PIT method is quite challenging and other approaches should be developed.



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Among the recently discovered Fe-based superconducting compounds, the (K,Ba)Fe2As2 phase is attracting large interest within the scientific community interested in conductor developments. In fact, after some years of development, critical current densities Jc of about 105 A/cm2 at fields up to more than 10 T have been obtained in powder in tube (PIT) processed wires and tapes. Here we explore the crucial points in the wire/tape fabrication by means of the ex-situ PIT method. We focus on scaling up processes which are crucial for the industrial fabrication. We analyzed the effects on the microstructure of the different heat and mechanical treatments. By an extensive microstructural analysis correlated with the transport properties we addressed the issues concerning the phase purity, the internal porosity and crack formation in the superconducting core region. Our best conductors with a filling factor of about 30 heat treated at 800 C exhibited Tc = 38 K the highest value measured in such kind of superconducting tape. The microstructure analysis shows clean and well connected grain boundaries but rather poor density: The measured Jc of about 3 x 10^4 A/cm2 in self-field is suppressed by less than a factor 7 at 7 T. Such not yet optimized Jc values can be accounted for by the reduced density while the moderate in-field suppression and a rather high n-factor confirm the high homogeneity and uniformity of these tapes.
The two most common types of MgB2 conductor fabrication technique - in-situ and ex-situ - show increasing conflicts concerning the connectivity, an effective current-carrying cross-sectional area. An in-situ reaction yields a strong intergrain coupling with a low packing factor, while an ex-situ process using pre-reacted MgB2 yields tightly packed grains, however, their coupling is much weaker. We studied the normal-state resistivity and microstructure of ex-situ MgB2 bulks synthesized with varied heating conditions under ambient pressure. The samples heated at moderately high temperatures of ~900{deg}C for a long period showed an increased packing factor, a larger intergrain contact area and a significantly decreased resistivity, all of which indicate the solid-state self-sintering of MgB2. Consequently the connectivity of the sintered ex-situ samples exceeded the typical connectivity range 5-15% of the in-situ samples. Our results show self-sintering develops the superior connectivity potential of ex-situ MgB2, though its intergrain coupling is not yet fulfilled, to provide a strong possibility of twice or even much higher connectivity in optimally sintered ex-situ MgB2 than in in-situ MgB2.
We report on the first local atomic structure study via the pair density function (PDF) analysis of neutron diffraction data and show a direct correlation of local coordinates to TC in the newly discovered superconducting FeSe1-xTex. The isovalent substitution of Te for Se such as in FeSe0.5Te0.5 increases Tc by twofold in comparison to a-FeSe without changing the carrier concentration but, on average, decreases the chalcogen-Fe bond angle. However, we find that the local symmetry is lower than the average P4/nmm crystal symmetry, because the Se and Te ions do not share the same site, leading to two distinct z-coordinates that exhibit two types of bond angles with Fe. The angle indeed increases from ~ 104.02o in FeSe to ~105.20o in FeSe0.5Te0.5 between Fe and Se. Simultaneously, ab-initio calculations based on spin density function theory yielded an optimized structure with distinct z-coordinates for Se and Te, in agreement with the experiment. The valence charge distribution in the Fe-Se bonds was found to be different from that in the Fe-Te bonds. Thus, superconductivity in this chalcogenide is closely related to the local structural environment, with direct implications on the multiband magnetism where modulations of the ionic lattice can change the distribution of valence electrons.
We demonstrate that Ta sheathed SmO1-xFxFeAs wires were successfully fabricated by the powder-in-tube (PIT) method for the first time. Structural analysis by mean of x-ray diffraction shows that the main phase of SmO1-xFxFeAs was obtained by this synthesis method. The transition temperature of the SmO0.65F0.35FeAs wires was confirmed to be as high as 52 K. Based on magnetization measurements, it is found that a globe current can flow on macroscopic sample dimensions with Jc of ~3.9x10^3 A/cm^2 at 5 K and self field, while a high Jc about 2x10^5 A/cm^2 is observed within the grains, suggesting that a significant improvement in the globle Jc is possible. It should be noted that the Jc exhibits a very weak field dependence behavior. Furthermore, the upper critical fields (Hc2) determined according to the Werthamer-Helfand-Hohenberg formula are (T= 0 K) = 120 T, indicating a very encouraging application of the new superconductors.
We demonstrate that Fe sheathed LaO0.9F0.1FeAs wires with Ti as a buffer layer were successfully fabricated by the powder-in-tube (PIT) method. Comparing to the common two-step vacuum quartz tube synthesis method, the PIT method is more convenient and safe for synthesizing the novel iron-based layered superconductors. Structural analysis by mean of x-ray diffraction shows that the main phase of LaO0.9F0.1FeAs was obtained by this synthesis method. The transition temperature of the LaO0.9F0.1FeAs wire is around 25 K. The micrograph shows a homogeneous microstructure with a grain size of 1-3 micrometers. The results suggest that the PIT process is promising in preparing high-quality iron-based layered superconductor wires.
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