Phase analysis of superconducting polycrystalline MgB(2)

Superconducting MgB(2) ceramics were prepared and yield superconducting transition temperatures of about 39 K. For covering the various length scales on which inhomogeneities appear in MgB(2), electron-probe micro-analysis (EPMA) and analytical transmission electron microscopy (TEM) were applied for a phase analysis. Particularly useful were the preliminary electron spectroscopic imaging (ESI) results in the TEM. It could be shown by EPMA that the microstructure consists of a Mg-B-O matrix and boron-rich secondary phases of composition close to MgB(12). It was unclear in which form oxygen was present in the superconducting matrix. By combining the acquisition of B-K and O-K edge jump ratio images and energy-dispersive X-ray spectroscopy in the TEM, we could prove that the matrix consists of superconducting MgB(2) and MgO. Most of the MgO precipitates and grains appear with diameters between 20 and 300 nm. The size distribution of MgO was inhomogeneous and oxygen-rich areas of dimensions >1 microm were also observed. Edge jump ratio images obtained by ESI were analysed for determining the signal values and effects of multiple inelastic scattering.     

Correlation between implantation defects and dopants in Fe-implanted SiC

SiC single crystals were implanted with Fe ions and the effects of implantation temperature, Fe concentration, and subsequent swift heavy ion irradiation on both dopant and damage depth distributions were evaluated by using RBS and channelling techniques. It is found that an increase of the implantation temperature above the threshold temperature for amorphization can lead to the formation of a broad layer (∼50 nm) containing a large concentration of implanted Fe atoms (∼2 at.%) but almost free of implantation defects. This particular configuration is likely due to dynamic annealing during implantation combined with defect annihilation at the surface. It is only observed when the implanted species concentration does not exceed a critical value (which lies between 2 and 5 at.% in the present system). Post-implantation swift heavy ion irradiation leads to a further decrease of the damage level, while the Fe distribution is not affected. The Fe substitutional fraction has been evaluated in the different tested conditions. A maximum value of ∼50% is found when implantation is performed at the temperature above that required to prevent amorphization (470 K in the present system). Swift-heavy ion irradiation seems to induce Fe atoms relocation at substitutional positions.     

A simple, quick and reliable method for TEM cross-section preparation of ceramic oxide films on thin metal substrates

We present a preparation method of cross-sectional thin foils for transmission electron microscopy (TEM). Samples are 0.1-1 m thick ceramic oxide films (CeO2, CeO2-YBa2Cu3O7 and CeO2-ZrO2/YO2-YBa2Cu3O7) epitaxially grown on 30-100 m highly textured nickel substrates. This method includes gluing the sample between a copper oxide dummy and a silicon dummy, followed by mechanical polishing and conventional ion milling. TEM cross-sectional samples obtained with this selection of dummies are electron-transparent up to a few tens of m parallel to the film surface. Several layer structures were analyzed by TEM and the results are shown. The preparation technique described here can be applied to any type of oxide film deposited on thin metal substrates.