Defect structures in MgB2 wires introduced by hot isostatic pressing

The microstructures of MgB2 wires prepared by the powder-in-tube technique and subsequent hot isostatic pressing were investigated using transmission electron microscopy. Large amount of crystalline defects including small angle twisting, tilting, and bending boundaries, in which high densities of dislocations reside, were found forming sub-grains within MgB2 grains. It is believed that these defects resulted from particle deformation during the hot isostatic pressing process and are effective flux pinning centers that contribute to the high critical current densities of the wires at high temperatures and at high fields.

Mg(B,O)2 precipitation in MgB2

MgB2 samples prepared by solid-state reaction were investigated using high-resolution transmission electron microscopy (HREM), X-ray energy-dispersive spectroscopy (EDX), electron energy-loss spectroscopy (EELS), and energy-filtered imaging. Large amounts of coherent precipitates with a size range from about 5 nm up to about 100 nm were found in the MgB2 crystallite matrices. The precipitates are of different shapes including sphere, ellipsoid, and faceted polyhedron depending on the size of the precipitates. EDX and EELS analyses confirm that smaller precipitates contain magnesium, boron and oxygen while larger faceted precipitates contain mainly magnesium and oxygen, implying that the oxygen content increases with precipitate size. HREM and electron diffraction investigations found that the precipitates have the same crystal lattice structure as that of MgB2 but with various composition modulations depending on the composition of the precipitates. The precipitates transform to the MgO phase after long exposure to residual oxygen in flowing Ar gas at high temperatures. The effect of the precipitates in different size ranges on flux pinning is discussed.

The degradation of MgB2 under ambient environment

The superconductivities of samples prepared by several procedures were found to degrade under ambient environment. The degradation mechanism was studied by measuring the change of surface chemical composition of dense MgB2 pellets (prepared by hot isostatic pressure, HIPed) under atmospheric exposure using X-ray Photoelectron Spectroscopy (XPS). Results showed that samples with poor connectivity between grains and with smaller grain sizes degrade with time when exposed to ambient conditions. In these samples, the Tc did not change with time, but the superconducting transition became broader and the Meissner fraction decreased. In contrast, our well-sintered and the HIPed samples remained stable for several months under ambient condition. The degradation was found to be related to surface decomposition as observed by XPS. We observed the formation of oxidized Mg, primarily in the form of a Mg hydroxide, the increase of C and O contents, and the reduction of B concentration in the surface layer of MgB2 samples.

The influence of microstructures and crystalline defects on the superconductivity of MgB2

This work studies the influence of microstructures and crystalline defects on the superconductivity of MgB2, with the objective to improve its flux pinning. A MgB2 sample pellet that was hot isostatic pressed (HIPed) was found to have significantly increased critical current density (Jc) at high fields than its un-HIPed counterpart. The HIPed sample had a Jc of 10000 A/cm2 in 50000 Oe (5 T) at 5K. This was 20 times higher than that of the un-HIPed sample, and the same as the best Jc reported by other research groups. Microstructures observed in scanning and transmission electron microscopy indicate that the HIP process eliminated porosity present in the MgB2 pellet resulting in an improved intergrain connectivity. Such improvement in intergrain connectivity was believed to prevent the steep Jc drop with magnetic field H that occurred in the un-HIPed MgB2 pellet at H > 45000 Oe (4.5 T) and T = 5 K. The HIP process was also found to disperse the MgO that existed at the grain boundaries of the un-HIPed MgB2 pellet and to generate more dislocations in the HIPed the pellets. These dispersed MgO particles and dislocations improved flux pinning also at H<45000 Oe. The HIPing process was also found to lower the resistivity at room temperature.

Synthesis, characterization and ageing of MgB2

We studied the influence of sample preparation and defects in the superconducting properties samples using atomic ratios of Mg:B=1:1 and Mg:B=1:2. Samples were characterized by SEM, and XRD, and the magnetization properties were examined in a SQUID magnetometer. The presence of Mg vacancies was determined by Rietveld analysis. Most of the samples exhibited sharp superconducting transitions with Tcs between 37- 39 K. We found a strong correlation between the crystal strain and the Tc. This strain was related to the presence of Mg vacancies. In addition, results showed that some samples degraded with time when exposed to ambient conditions. In these samples the Tc did not change with time, but the superconducting transition became broader and the Meissner fraction decreased. This effect was only present in samples with poor connectivity between grains and smaller grain sizes. The degradation was related to a surface decomposition as observed by X-ray Photoelectron Spectroscopy. No correlation was found between this effect and the presence of Mg vacancies.

Effect of lattice strain and defects on the superconductivity of MgB2

The influence of lattice strain and Mg vacancies on the superconducting properties of MgB2 samples has been investigated. High quality samples with sharp superconducting transitions were synthesized. The variation in lattice strain and Mg vacancy concentrations were obtained by varying the synthesis conditions. It was found that high strain (~1%) and the presence of Mg vacancies (~ 5 %) resulted in lowering the Tc by only 2 K.