A two-circle powder diffractometer for synchrotron radiation on Station 2.3 at the SRS

The two-circle powder diffractometer on Station 8.3 at the SRS has recently been relocated to station 2.3, some half the distance from a dipole radiation source with the same nominal 1.2T field. The purpose of this paper is to detail the changes and modifications to the diffractometer operation

A two-circle powder diffractometer for synchrotron radiation with a closed loop encoder feedback system

A high-angular-resoln. 2-circle powder diffractometer equipped with long diffracted-beam collimators was built at Daresbury Lab. The diffractometer has encoders mounted directly on the 2θ and ω axes. These give a nominal angular resoln. of 0.1 and 1.0 mdeg resp. Repeated scans of single powder peaks have demonstrated a reproducibility of 0.1 mdeg 2θ. Measurements on 5 independent peaks of W give a self consistency of 1 (1) × 10-5 Å. An example data set from synthetic olivine Mg2SiO4 was refined using the Rietveld method and the results compare very well with single-crystal structure refinements. [on SciFinder(R)

Tungsten Bronze Barium Neodymium Titanate (Ba 6–3 Nd 8+2 Ti 18 O 54 ): An Intrinsic Nanostructured Material and Its Defect Distribution

We investigated the structure of the tungsten bronze barium neodymium titanates Ba6–3nNd8+2nTi18O54, which are exploited as microwave dielectric ceramics. They form a complex nanostructure, which resembles a nanofilm with stacking layers of ∼12 Å thickness. The synthesized samples of Ba6–3nNd8+2nTi18O54 (n = 0, 0.3, 0.4, 0.5) are characterized by pentagonal and tetragonal columns, where the A cations are distributed in three symmetrically inequivalent sites. Synchrotron X-ray diffraction and electron energy loss spectroscopy allowed for quantitative analysis of the site occupancy, which determines the defect distribution. This is corroborated by density functional theory calculations. Pentagonal columns are dominated by Ba, and tetragonal columns are dominated by Nd, although specific Nd sites exhibit significant concentrations of Ba. The data indicated significant elongation of the Ba columns in the pentagonal positions and of the Nd columns in tetragonal positions involving a zigzag arrangement of atoms along the b lattice direction. We found that the preferred Ba substitution occurs at Nd[3]/[4] followed by Nd[2] and Nd[1]/[5] sites, which is significantly different to that proposed in earlier studies. Our results on the Ba6–3nNd8+2nTi18O54 “perovskite” superstructure and its defect distribution are particularly valuable in those applications where the optimization of material properties of oxides is imperative; these include not only microwave ceramics but also thermoelectric materials, where the nanostructure and the distribution of the dopants will reduce the thermal conductivity