AbstractThe reaction mechanism of BaCO3+CaCO3+TiO2 by solid state methods has been studied in this work using thermal analysis (DSC-TG) from 500 to 1500 °C and in situ X-ray diffraction (XRD) from room temperature to 800 °C. In the mixed powders, the CaO is firstly formed followed by presence of an intermediate Ba2TiO4 phase and finally the formation of CaTiO3, BaTiO3 and/or (Ba,Ca)TiO3, where the presence of CaO or CaTiO3 (CT) has slowed down the formation of BaTiO3 (BT). Raman microscopy of a BT-CT diffusion couple has shown that Ca2+ firstly diffuses into the BT grain boundaries and then into the BT core.
The distribution of liquid at the semi solid state is one of the most important parameters for steel thixoforging. It has a great influence on the viscosity of the material, on the flows and finally on the final shape and mechanical properties of the thixoforged parts. Both ex situ and in situ 3D X-ray microtomography characterizations have been carried out to determine the quantity and localization of liquid at high temperature of M2 steel slugs. Microtomography was first performed ex situ at room temperature on samples heated and quenched from semi-solid state. The specimens were also scanned in situ directly at high temperature. The obtained results have been compared to 2D observations using EDS technique in SEM on heated and quenched specimens. They showed a good correlation making both approaches very efficient for the study of the liquid zones at the semi-solid state
Selected compositions of the Ba–Sr–Co–Fe–O system were synthesized from powders by the solid-state reaction method. Samples were equilibrated at 1273 K for 36 000 s in air. The resulting powders were characterized by X-ray diffraction (XRD) at room temperature and by high-temperaturein situXRD. The phases present in the BaxSr1−xCoyFe1−yO3−δsystem are outlined for 1273 K in air. For most of the quaternary compositions, the cubic perovskite is formed, except for the compositions withx= 1 (excludingy= 0.4),y= 1 andx,y= 0.8, where the phases mainly show hexagonal distortions, andx, y= 0, for which a predominant cubic phase is mixed with other phases.
An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.
Cadmium sulfide (CdS) nanocrystals (NCs) were self-assembled and in-situ immobilized on the dithiocarbamate (DTCs)-functionalized polyethylene glycol terephthalate (PET) substrates between the organic (carbon disulfide diffused in n-hexane) –aqueous (ethylenediamine and Cd2+ dissolved in water) interface at room temperature. Powder X-ray diffraction measurement revealed the hexagonal structure of CdS nanocrystals. Morphological studies performed by scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) showed the island-like structure of CdS nanocrystals on PET substrates, as well as energy-dispersive X-ray spectroscopy (EDS) confirmed the stoichiometries of CdS nanocrystals. The optical properties of DTCs modified CdS nanocrystals were thoroughly investigated by ultraviolet-visible absorption spectroscopy (UV-vis) and fluorescence spectroscopy. The as-prepared DTCs present intrinsic hydrophobicity and strong affinity for CdS nanocrystals.
Structures of two K2SnX(PO4)3(X=Fe,Yb) phosphates, obtained by conventional solid state reaction techniques at 950 °C, were determined at room temperature by X-ray powder diffraction using Rietveld analysis. The two materials exhibit the langbeinite-type structure (P213 space group, Z=4). Cubic unit cell parameter values are: a=9.9217(4) Å and a=10.1583(4) Å for K2SnFe(PO4)3 and K2SnYb(PO4)3, respectively. Structural refinements show that the two crystallographically independent octahedral sites (of symmetry 3) have a mixed Sn∕X (X=Fe,Yb) population although ordering is stronger in the Yb phase than in the Fe phase.
In situ synchrotron X-ray diffraction was used to study a deformed Cu-0.88 Fe-0.24 P alloy during heating process. The measurements were performed at room temperature and also at high temperatures up to 893 K in order to determine the recovery, ageing and recrystallization process. With the increase of temperature, the angles of copper matrix peaks moved left and the FWHM (full width at half maximum) decreased slightly. Fe3P precipitates were first detected at 533 K, reached the maximum at 673 K, and re-dissolved into matrix at 853 K. A dramatic decrease in FWHM was observed accompanied by the precipitation of Fe3P phases, indicating the reduction of lattice distortion of copper matrix.
Determination of Quantity and Localization of Liquid in the Semi-Solid State Using both 3D X-Ray Microtomography and 2D Techniques for Steel Thixoforming