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Register a new userFe-vacancy order and superconductivity in PbO-type tetragonal {beta}-Fe1-xSe
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Several superconducting transition temperatures in the range of 30-40 K were reported in the recently discovered intercalated FeSe sytem (A1-xFe2-ySe2, A = K, Rb, Cs, Tl). Although the superconducting phases were not yet conclusively decided, more than one magnetic phase with particular orders of iron vacancy and/or potassium vacancy were identified, and some were argued to be the parent phase. Here we show the discovery of the presence and ordering of iron vacancy in nonintercalated FeSe (PbO-type tetragonal {beta}-Fe1-xSe). Three types of iron-vacancy order were found through analytical electron microscopy, and one was identified to be nonsuperconducting and magnetic at low temperature. This discovery suggests that the rich-phases found in A1-xFe2-ySe2 are not exclusive in Fe-Se related superconductors. In addition, the magnetic {beta}-Fe1-xSe phases with particular iron-vacancy orders are more likely to be the parent phase of FeSe superconducting system, instead of the previously assigned {beta}-Fe1+{delta}Te.
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Here we establish a more complete phase diagram for FeSe system, based on experimental results of nonstoichiometric Fe1-xSe single crystals that we have developed recently, as well as nearly stoichiometric FeSe single crystals. The electronic correlation is found to be strongly enhanced in hole-dominated Fe1-xSe, as compared with electron-dominated FeSe, from the magnetic susceptibility and electrical transport measurements in the normal state. A superconducting dome is found to emerge starting from the strongly correlated hole-dominated regime with electron doping, while the tetragonal-orthorhombic phase transition at ~90 K is observed only at higher electron-doping levels in the electron-dominated regime.
The recent discovery of superconductivity with relatively high transition temperature Tc in the layered iron-based quaternary oxypnictides La[ O1-xFx] FeAs was a real surprise. The excitement generated can be seen by the number of subsequent works published within a very short period of time. Although there exists superconductivity in alloy that contains Fe element, LaOMPn (with M= Fe, Ni; and Pn=P and As) is the first system where Fe-element plays the key role to the occurrence of superconductivity. LaOMPn has a layered crystal structure with an Fe-based plane. It is quite natural to ask whether there exists other Fe based planar compounds that exhibit superconductivity. Here we report the observation of superconductivity with zero resistance transition temperature at 8K in the PbO-type alpha-FeSe compound. Although FeSe has been studied quite extensively, a key observation is that the clean superconducting phase exists only in those samples prepared with intentional Se deficiency. What is truly striking, is that this compound has the same, perhaps simpler, planar crystal sublattice as the layered oxypnictides. Furthermore, FeSe is, compared with LaOFeAs, much easier to handle and fabricate. In view of the abundance of compounds with PbO type structure, this result opens a new route to the search for unconventional superconductors.
The electronic and superconducting properties of Fe1-xSe single-crystal flakes grown hydrothermally are studied by the transport measurements under zero and high magnetic fields up to 38.5 T. The results contrast sharply with those previously reported for nematically ordered FeSe by chemical-vapor-transport (CVT) growth. No signature of the electronic nematicity, but an evident metal-to-nonmetal crossover with increasing temperature, is detected in the normal state of the present hydrothermal samples. Interestingly, a higher superconducting critical temperature Tc of 13.2 K is observed compared to a suppressed Tc of 9 K in the presence of the nematicity in the CVT FeSe. Moreover, the upper critical field in the zero-temperature limit is found to be isotropic with respect to the field direction and to reach a higher value of ~42 T, which breaks the Pauli limit by a factor of 1.8.
Experimental evidences from transport, magnetic, and magneto-optical (MO) image measurements confirmed that arsenic (As) vapor annealing was another effective way to induce bulk superconductivity with isotropic, large, and homogenous superconducting critical current density (Jc) in Fe1+yTe0.6Se0.4 single crystal. Since As is an exotic and easily detectable heavy element to Fe1+yTe0.6Se0.4 single crystal, As vapor annealing is very advantageous for the study of annealing mechanism. Detailed micro-structural and elemental analyses exclude the possibility that intercalating or doping effect may happen in the other post-annealing methods, proving that Fe reacts with As on the surface of the crystal and the reaction itself acts as a driving force to drag excess Fe out. The removal of excess Fe results in the good superconductivity performance.
We studied the electrical transport on $beta$-Fe$_{4+delta}$Se$_{5}$ single-crystal nanowires, exhibiting $sqrt{5}timessqrt{5}$ Fe-vacancy order and mixed valence of Fe. We observed a first-order metal-insulator transition of the transition temperature at $sim$28~K at zero magnetic field. The dielectric relaxation reveals that the transition is related to an energy gap expansion of $sim$12~meV, involving the charge-orbital ordering. At nearly 28~K, colossal positive magnetoresistance emerges, resulting from the magnetic-field dependent shift of the transition temperature. Through the transition, the magnetotransport behavior transits from two-dimension-like to one-dimension-like conduction. The transition temperature demonstrates anisotropy with the $c$-axis as the preferred orientation in magnetic fields, suggesting the spin-orbital coupling. Our findings demonstrate the novel magnetoresistive transition intimating a topological transition in the Fe-vacancy-ordered $beta$-Fe$_{4+delta}$Se$_{5}$ nanowires. The results provide valuable information to better understand the orbital nature and the emergence of superconductivity in FeSe-based materials.
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