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Abstract: Single-phase samples of Ln 2−xCaxCoO4+δ (Ln = Pr3+ − Gd3+) around x∼1 have been prepared. For the first time, the phase field for these compounds has been defined using powder X-ray diffraction and a very narrow solid solution was observed. Under our synthetic conditions, the K2NiF4 structure was not formed for the large La3+ ion, or for compositions containing the smaller rare earths ions (

Abstract: The structure of the defect pyrochlore NaW2O6+δ ·nH2−z O after ion exchange with K, Rb, Sr or Cs for Na has been investigated using thermal analysis, solid-state nuclear magnetic resonance, laboratory X-ray and neutron diffraction methods. Neutron diffraction studies show that both the A-type cations (Na+, K+, Rb+, and/or Cs+) and the water molecules reside within the channels that form in the 111 direction of the W2O6 framework and that these strongly interact. The analytical results suggest that the water and A-type cations compete for space in the tunnels within the W2O6 pyrochlore framework, with the total number of water molecules and cations being approximately constant in the six samples investigated. The interplay between the cations and water explains the non-linear dependence of the a lattice parameter on the choice of cation. It appears that the ion-exchange capacity of the material will be controlled by the amount of water initially present in the sample. [Copyright &y& Elsevier]

Abstract: Ceramics based on LnTiTaO6 (Ln =La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) were prepared using a conventional solid-state ceramic route. The structure and microstructure of the samples were analyzed using scanning electron microscopy, synchrotron X-ray powder diffraction and neutron diffraction techniques. The unit cell volume of the ceramics decreased with a decrease in ionic radius of the rare-earth ions until a phase change was seen at Ho where the space group changed from Pnma to Pbcn. The results confirmed that the boundary of the aeschynite to euxenite phase change that lies between DyTiTaO6 and HoTiTaO6 and demonstrate that this is a result of distortion of the channels in the aeschynite structure. [Copyright &y& Elsevier]

Abstract: The temperature dependence of the structure of the pyrochlore NaW2− y Mo y O6+ δ ·nH2− z O has been investigated using a variety of diffraction and spectroscopic methods. The positions of OH−/H2O molecules in the structure have been determined. Increases in temperature induce small lattice parameter changes, which are thought to result from movement of the H2O molecules in the pyrochlore lattice. [Copyright &y& Elsevier]

Abstract: The structure of one of the oxides proposed to be present in the grey phase of irradiated mixed oxide fuel, the double perovskite Ba2SrUO6 has been investigated from room temperature to 1300K using synchrotron X-ray powder diffraction methods. The divalent strontium and hexavalent uranium are found to be fully ordered in the double-perovskite arrangement of alternating octahedra sharing corner oxygen atoms. At room temperature Ba2SrUO6 adopts a monoclinic structure in space group P21/n. Heating to above 900K induces a first order transition to a rhombohedral structure, and further heating to above 1200K results in a continuous transition to a cubic structure. The sequence of structures is associated with the progressive loss of cooperative tilting of the corner sharing SrO6 and UO6 octahedra. [Copyright &y& Elsevier]

Abstract: This paper investigates the effect of both the mixing technique and heating rate during cure on the dispersion of montmorillonite (MMT) clay in an epoxy resin. The combination of sonication and using a 10°C/min heating rate during cure was found to facilitate the dispersion of nanoclay in epoxy resin. These processing conditions provided a synergistic effect, making it possible for polymer chains to penetrate in-between clay galleries and detach platelets from their agglomerates. As the degree of dispersion was enhanced, the flexural modulus and strength properties were found to decrease by 15% and 40%, respectively. This is thought to be due to individual platelets fracturing in the nanocomposite. Complementary techniques including X-ray diffraction (XRD), small angle X-ray scattering (SAXS), scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM–EDX), transmission electron microscopy (TEM) and optical microscopy were essential to fully characterise localised and spatial regions of the clay morphologies. [Copyright &y& Elsevier]

A new class of materials, which rely on the dispersion strengthening of SiC particles in addition to precipitation strengthening by nano-precipitates is being developed for the application in molten salt nuclear reactors. A battery of dispersion and precipitation strengthened (DPS) NiMo-based alloys containing varying amount of SiC (0.5–2.5 wt.%) was prepared via a mechanical alloying (MA) route followed by spark plasma sintering (SPS), rapid cooling, high-temperature annealing and water quenching. Lab X-ray Diffraction (XRD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the microstructural characterization of this new type of alloys. It is shown that the NiMo matrix of these alloys is effectively reinforced by dispersion of SiC from the initial powder mixture and nano-Ni 3 Si precipitates, which precipitated during the sintering/annealing process. Furthermore, the matrix is strengthened by solid-solution of Mo in Ni. As a result, these newly developed NiMo alloys take advantage of dispersion, precipitation and solid solution strengthening, which leads to their superior mechanical properties. [ABSTRACT FROM AUTHOR]

Copper-doped nanosized zeolite A crystals were synthesized by an in situ templating approach using [Cu(EDTA)] 2− -complex. The structural properties of the copper containing zeolite crystals were characterized by a suite of different techniques including SEM–EDX, ESR, mid-IR and Far-IR, Raman, in situ XRD and non-ambient neutron powder diffraction. The SEM investigations on the morphology show spheroidal zeolite A crystals with average size ∼200 nm. The asymmetric ESR spectrum shows that the Cu 2+ ion is in a tetragonal-distorted octahedral crystal field. FT-IR and Raman spectroscopies provide information on coordination environment of the copper ion. The band due to stretching vibration of C–N bond, where N is coordinated to the copper ion (C–N–Cu), was observed at 1109 cm −1 in the mid-infrared region. The Raman band due to the Cu–O bond is present at 630 cm −1 indicating the coordination of the Cu 2+ -cation to COO − -group of the EDTA-ion. The XRD data shows an enlarged d -spacing between the adjacent zeolite lattice planes due to the presence of the [Cu(EDTA)] 2− -complex in comparison to template-free LTA zeolite structure. LeBail fitting approach on temperature-dependent in situ X-ray and neutron diffraction profiles have demonstrated the expansion of the zeolite cell during the thermal treatment followed by subsequent contraction with the decomposition of the organic template. [ABSTRACT FROM AUTHOR]

The β -phase of Au 7 Cu 5 Al 4 undergoes a reversible shape-memory phase transformation for which several conflicting martensite phases have been reported. Here we show the significance of the cooling temperature used to obtain the martensite. If Au 7 Cu 5 Al 4 is cooled from the parent phase condition to cryogenic temperatures, e.g. below 200 K, the martensitic phase is orthorhombic (space group Pcmn , a = 4.4841 Å, b = 5.8996 Å, c = 17.8130 Å); however, when this composition is cooled to only ∼260 K it will in general consist of a mixture of orthorhombic and monoclinic phase (the latter has space group P 2 1 / m , a = 4.4742 Å, b = 5.9265 Å, c = 13.3370 Å, β = 91.425°). In contrast, a sample with decreased Al content (Au 7 Cu 5.7 Al 3.3 ) transforms fully to monoclinic phase if cooled to ∼260 K. [ABSTRACT FROM AUTHOR]

Abstract: The β-phase of Au7Cu5Al4 undergoes a reversible shape-memory phase transformation, however there has been some uncertainty regarding the crystal structure or structures of the parent phase. Here we show that, under equilibrium conditions, the parent phase possesses the L21 structure between its A p (about 79°C) and ∼630°C, and the B2 primitive cubic structure between ∼630°C and its melting point. It melts directly from B2 into the liquid state and hence never achieves the random bcc A2 structure that has been previously mooted. Splat-cast samples of the alloy are martensitic, proving that development of equilibrium order and defect concentration are not pre-requisites for the A → M transformation to occur. [Copyright &y& Elsevier]