Vibrational spectroscopic,conductivity, and calorimetric studies on tripotassium hydrogen diselenate

Infrared spectra of K₃H(SeO₄)₂ obtained at 300 and 77 K, conform to the pattern expected for a very strong O-H O hydrogen bond. Differential scanning calorimetry (DSC) and electrical conductivity measurements indicate the presence of a phase transition at 388 K to a state having high protonic conductivity.A. W. A. is a recipient of a La Trobe University Postgraduate Research Scholarship.     

Dielectric properties and microstructural characterization of cubic pyrochlored bismuth magnesium niobates

Cubic bismuth pyrochlores in the $\mathrm{Bi}_{2}\mathrm{O}_{3}$ –MgO– $\mathrm{Nb}_{2}\mathrm{O}_{5}$ system have been investigated as promising dielectric materials due to their high dielectric constant and low dielectric loss. Here, we report on the dielectric properties and microstructures of cubic pyrochlored $\mathrm{Bi}_{1.5}\mathrm{MgNb}_{1.5}\mathrm{O}_{7}$ (BMN) ceramic samples synthesized via solid-state reactions. The dielectric constant (measured at 1 MHz) was measured to be ${\sim}120$ at room temperature, and the dielectric loss was as low as 0.001. X-ray diffraction patterns demonstrated that the BMN samples had a cubic pyrochlored structure, which was also confirmed by selected area electron diffraction (SAED) patterns. Raman spectrum revealed more than six vibrational models predicted for the ideal pyrochlore structure, indicating additional atomic displacements of the A and $\mathrm{O}'$ sites from the ideal atomic positions in the BMN samples. Structural modulations of the pyrochlore structure along the [110] and [121] directions were observed in SAED patterns and high-resolution transmission electron microscopy (HR-TEM) images. In addition, HR-TEM images also revealed that the grain boundaries (GBs) in the BMN samples were much clean, and no segregation or impure phase was observed forming at GBs. The high dielectric constants in the BMN samples were ascribed to the long-range ordered pyrochlore structures since the electric dipoles formed at the superstructural direction could be enhanced. The low dielectric loss was attributed to the existence of noncontaminated GBs in the BMN ceramics.     

Application of focused ion beam to atom probe tomography specimen preparation from mechanically alloyed powders.

Focused ion-beam milling has been applied to prepare needle-shaped atom probe tomography specimens from mechanically alloyed powders without the use of embedding media. The lift-out technique known from transmission electron microscopy specimen preparation was modified to cut micron-sized square cross-sectional blanks out of single powder particles. A sequence of rectangular cuts and annular milling showed the highest efficiency for sharpening the blanks to tips. First atom probe results on a Fe95Cu5 powder mechanically alloyed in a high-energy planetary ball mill for 20 h have been obtained. Concentration profiles taken from this powder sample showed that the Cu distribution is inhomogeneous on a nanoscale and that the mechanical alloying process has not been completed yet. In addition, small clusters of oxygen, stemming from the ball milling process, have been detected. Annular milling with 30 keV Ga ions and beam currents >or=50 pA was found to cause the formation of an amorphous surface layer, whereas no structural changes could be observed for beam currents 相似文献   

Focused ion beam preparation of atom probe specimens containing a single crystallographically well-defined grain boundary

Needle-shaped atom probe specimens containing a single grain boundary were produced using the focused ion beam (FIB) of a two-beam FIB/SEM (scanning electron microscope) system. The presented specimen preparation approach allows the unprecedented study of a grain boundary which is well characterised in its crystallographic orientation by means of the field ion microscope (FIM) and the tomographic atom probe (TAP). The analysis of such specimens allows in particular the determination of solute excess atoms at this specific grain boundary and hence the investigation of the segregation behaviour. The crucial preparation steps are discussed in detail in the present study for the Sigma 19 a {331} 110 grain boundary of a 40 at.ppm-Bi doped Cu bi-crystal. Transmission electron microscope (TEM) images and TAP analyses of the atom probe tips demonstrate unambiguously the presence of the selectively prepared grain boundary in the apex region of some of the specimens.