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Flux free growth of large FeSe1/2Te1/2 superconducting single crystals by an easy high temperature melt and slow cooling method

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 Added by Veer Awana Dr
 Publication date 2015
  fields Physics
and research's language is English




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We report successful growth of flux free large single crystals of superconducting FeSe1/2Te1/2 with typical dimensions of up to few cm. The AC and DC magnetic measurements revealed the superconducting transition temperature (Tc) value of around 11.5K and the iso-thermal MH showed typical type-II superconducting behavior. The lower critical field being estimated by measuring the low field iso-thermal magnetization in superconducting regime is found to be above 200 Oe at 0K.



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We report flux free growth of superconducting FeSe single crystals by an easy and versatile high temperature melt and slow cooling method for first time. The room temperature XRD on the surface of the piece of such obtained crystals showed single 101 plane of Beta-FeSe tetragonal phase. The bulk powder XRD, being obtained by crushing the part of crystal chunk showed majority tetragonal and minority FeSe hexagonal crystalline phases. Detailed HRTEM images along with SAED (selected area electron diffraction) showed the abundance of both majority and minority FeSe phases. Both transport (RT) and magnetization (MT) exhibited superconductivity at below around 10K. Interestingly, the magnetization signal of these crystals is dominated by the magnetism of minority magnetic phase, and hence the isothermal magnetization (MH) at 4K was seen to be ferromagnetic (FM) like. Transport (R-T) measurements under magnetic field showed superconductivity onset at below 12K, and R = 0 (Tc) at 9K. Superconducting transition temperature (Tc) decreases with applied field to around 6K at 7Tesla, with dTc/dH of 0.4K/Tesla, giving rise to an Hc2 value of around 50 Tesla, 30 Tesla and 20 Tesla for Rn = 90, 50 and 10 percent respectively. FeSe single crystal activation energy is calculated from Thermally Activated Flux Flow (TAFF) model which is found to decreases with field.
We report synthesis of non superconducting parent compound of iron chalcogenide, i.e., FeTe single crystal by self flux method. The FeTe single crystal is crystallized in tetragonal structure with the P4/nmm space group. The detailed SEM (scanning electron microscopy) results showed that the crystals are formed in slab like morphology and are near (slight deficiency of Te) stoichiometric with homogenous distribution of Fe and Te. The coupled structural and magnetic phase transition is seen at around 70K in both electrical resistivity and magnetization measurements, which is hysteric (deltaT = 5K) in nature with cooling and warming cycles. Magnetic susceptibility (chi-T) measurements showed the magnetic transition to be of antiferromagnetic nature, which is substantiated by isothermal magnetization (M-H) plots as well. The temperature dependent electrical resistivity measured in 10kOe field in both in plane and out of plane field directions showed that the hysteric width nearly becomes double to deltaT = 10K, and is maximum for the out of plane field direction for the studied FeTe single crystal. We also obtained a sharp spike like peak in heat capacity Cp(T) measurement due to the coupled structural and magnetic order phase transitions.
Single crystals of the LnFeAsO (Ln1111, Ln = Pr, Nd, and Sm) family with lateral dimensions up to 1 mm were grown from NaAs and KAs flux at high pressure. The crystals are of good structural quality and become superconducting when O is partially substituted by F (PrFeAsO1-xFx and NdFeAsO1-xFx) or when Fe is substituted by Co (SmFe1-xCoxAsO). From magnetization measurements, we estimate the temperature dependence and anisotropy of the upper critical field and the critical current density of underdoped PrFeAsO0.7F0.3 crystal with Tc = 25 K. Single crystals of SmFe1-xCoxAsO with maximal Tc up to 16.3 K for x = 0.08 were grown for the first time. From transport and magnetic measurements we estimate the critical fields and their anisotropy, and find these superconducting properties to be quite comparable to the ones in SmFeAsO1-xFx with a much higher Tc of = 50 K. The magnetically measured critical current densities are as high as 109 A/m2 at 2 K up to 7 T, with indication of the usual fishtail effect. The upper critical field estimated from resistivity measurements is anisotropic with slopes of -8.7 T/K (H // ab-plane) and -1.7 T/K (H // c-axis). This anisotropy (= 5) is similar to that in other Ln1111 crystals with various higher Tc s.
The bulk polycrystalline sample FeSe1/2Te1/2 is synthesized by solid state reaction route in an evacuated sealed quartz tube at 750 oC. The presence of superconductivity is confirmed through magnetization/thermoelectric/resistivity studies. It is found that the superconducting transition temperature (Tc) is around 12 K. Heat capacity (Cp) of superconducting FeSe1-xTex exhibited a hump near Tc, instead of well defined Lambda transition. X-ray Photo electron spectroscopy (XPS) studies revealed well defined positions for divalent Fe, Se and Te but with sufficient hybridization of Fe (2p) and Se/Te (3d) core levels. In particular divalent Fe is shifted to higher BE (binding energy) and Se and Te to lower. The situation is similar to that as observed earlier for famous Cu based HTSc (High Tc superconductors), where Cu (3d) orbital hybridizes with O (2p). We also found the satellite peak of Fe at 712.00 eV, which is attributed to charge carrier localization induced by Fe at 2c site.
One of the most important properties of very recently reported FeSe based superconductors is the robustness of their superconductivity under applied magnetic field. The synthesis and control of superconductivity in FeSe based compounds is rather a difficult task. Synthesis and physical property characterization for optimized superconductivity of FeSe1/2Te1/2 at 13 K is reported here. The compound crystallized in a tetragonal structure with lattice parameters a = 3.8008(10) and c = 6.0187 (15) A. Magnetization measurements indicated bulk superconductivity with lower critical field (Hc1) of around 180 Oe. By applying Ginzburg Landau (GL) theory, the Hc2(0) value is estimated to be = 1840 kOe for the 90% of resistive transition. A heat capacity measurement revealed bulk superconductivity by a hump at Tc near 13 K, and an expected decrease was observed under an applied magnetic field.
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