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Grain size determination of superconducting MgB2 powders from magnetization curve, image analysis and surface area measurement

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 Added by Maurizio Vignolo
 Publication date 2014
  fields Physics
and research's language is English




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The present article reports a method for the average grain size evaluation of superconducting nano-particles through their magnetic properties. The use of SQUID magnetometry to determine the average MgB2 particle size was investigated and the results compared with those achieved through other techniques. In particular the data obtained from zero field cooled magnetization measurement as function of the temperature were compared with the results obtained by scanning electron microscopy and Brunauer-Emmett-Teller techniques. The particle magnetization was measured by a commercial SQUID magnetometer in magnetic field (1 mT) and temperatures ranging from 5 to 50 K dispersing the powders in a grease medium. The grain size is obtained by fitting the data taking into account the Ginzburg-Landau temperature dependence of the London penetration depth. Variations on typical modeling parameters were explored in order to gain a better picture of the average grain size and the effectiveness of various measurement techniques. We find that it is possible to use the magnetization measurements to determine the average grain size even if the SEM image analysis allows extracting more information about the grain size distribution. Furthermore a Matlab routine has been developed in order to get automatic analysis of SEM images.



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70 - A. Dulcic , D. Paar , M. Pozek 2001
We report magnetic field dependent magnetization and microwave impedance measurements on a MgB2 superconductor prepared by high pressure synthesis. We find that the upper critical field is linearly dependent on temperature near Tc and the dc irreversibility field exponent is ~1.4. The microwave data display an excess surface resistance below Tc which is neither observed in low Tc nor in high temperature superconductors (HTSC). The real part of the complex conductivity, sigma1, shows a huge maximum below Tc and the imaginary part, sigma2, is linear for temperatures less than 20 K, which can not be simply accounted for by the weak coupling BCS model with an s-wave superconducting order parameter. We speculate that this may be due to the two gaps reported by other studies. Unlike measurements on the high temperature superconducting cuprates, we find no evidence of weak-links in the superconducting state. By inverting the magnetic field dependent impedance data, we find a vortex depinning frequency that decreases with increasing magnetic field and evidence for an anisotropic upper critical magnetic field.
67 - F. Simon , A. Janossy , T. Feher 2001
We have observed the conduction electron spin resonance (CESR) in fine powders of MgB2 both in the superconducting and normal states. The Pauli susceptibility is chi_s=2.0*10^{-5} emu/mole in the temperature range of 450 to 600 K. The spin relaxation rate has an anomalous temperature dependence. The CESR measured below T_c at several frequencies suggests that MgB_2 is a strongly anisotropic superconductor with the upper critical field, H_c2, ranging between 2 and 16 T. The high-field reversible magnetization data of a randomly oriented powder sample are well described assuming that MgB_2 is an anisotropic superconductor with H_c2^{ab} / H_{c2}^{c} approx 6--9.
The MgB2 superconductor has already demonstrated its applicative potential, in particular for DC applications such as MRI magnets, thanks to the low costs of the raw materials and to its simple production process. However further efforts have still to be made in order to broaden its employment also towards the AC applications such as SFCL, motors, transformers. The main issues are related to the reduction of the AC losses. Some of these can be faced by obtaining multifilamentary conductors with a large number of very fine filaments and, in this context, the powders granulometry can play a crucial role. We have prepared MgB2 starting powders with different granulometries and by the ex-situ P.I.T method we have realized multifilamentary wires with a number of filaments up to 361 and an average size of each filament lowered down to 30 microns. In particular we have studied the relationship between grain and filament size in terms of transport properties and show that the optimization of this ratio is possible in order to obtain suitable conductors for AC industrial applications.
72 - S.Lee , H.Mori , T.Masui 2001
Here we report the growth of sub-millimeter MgB2 single crystals of various shapes under high pressure in Mg-B-N system. Structure refinement using a single-crystal X-ray diffraction analysis gives lattice parameters a=3.0851(5) A and c=3.5201(5) A with small reliability factors (Rw =0.025, R=0.018), which enables us to analyze the Fourier and Fourier difference maps. The maps clearly show the B sp2 orbitals and covalency of the B-B bonds. The sharp superconducting transitions at Tc =38.1-38.3K were obtained in both magnetization (DTc =0.6K) and resistivity (DTc <0.3K) measurements. Resistivity measurements with magnetic fields applied parallel and perpendicular to the Mg and B sheets reveal the anisotropic nature of this compound, with upper critical field anisotropy ratio of about 2.7.
For many applications of polycrystalline high-Tc superconductors the small critical currents of the grain boundaries pose a severe problem. To solve this problem we derive novel designs for the microstructure of coated conductors.
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