Reversible melting and equilibrium phase formation of (Bi,Pb)2Sr2Ca2Cu3O10+d

The decomposition and the reformation of the (Bi,Pb)2Sr2Ca2Cu3O10+d (?Bi,Pb(2223)?) phase have been investigated in-situ by means of High-Temperature Neutron Diffraction, both in sintered bulk samples and in Ag-sheathed monofilamentary tapes. Several decomposition experiments were performed at various temperatures and under various annealing atmospheres, under flowing gas as well as in sealed tubes, in order to study the appropriate conditions for Bi,Pb(2223) formation from the melt. The Bi,Pb(2223) phase was found to melt incongruently into (Ca,Sr)2CuO3, (Sr,Ca)14Cu24O41 and a Pb,Bi-rich liquid phase. Phase reformation after melting was successfully obtained both in bulk samples and Ag-sheathed tapes. The possibility of crystallising the Bi,Pb(2223) phase from the melt was found to be extremely sensitive to the temperature and strongly dependent on the Pb losses. The study of the mass losses due to Pb evaporation was complemented by thermogravimetric analysis which proved that Pb losses are responsible for moving away from equilibrium and therefore hinder the reformation of the Bi,Pb(2223) phase from the melt. Thanks to the full pattern profile refinement, a quantitative phase analysis was carried out as a function of time and temperature and the role of the secondary phases was investigated. Lattice distortions and/or transitions were found to occur at high temperature in Bi,Pb(2223), Bi,Pb(2212), (Ca,Sr)2CuO3 and (Sr,Ca)14Cu24O41, due to cation diffusion and stoichiometry changes. The results indicate that it is possible to form the Bi,Pb(2223) phase from a liquid close to equilibrium conditions, like Bi(2212) and Bi(2201), and open new unexplored perspectives for high-quality Ag-sheathed Bi,Pb(2223) tape processing.Comment: 45 pages (including references,figures and captions), 13 figures Submitted to Supercond. Sci. Techno

Preparation and characterization of Au/ZrO2 composite obtained by oxidation of thin film ZrxAuy alloy

We present the preliminary results of a study aiming at preparing Au/ZrO2 mixed nanosized particles from thin films. In a first step, pure Zr and Au layers are alternatively deposited by RF sputtering on Si and W substrates under vacuum. Then, the intermetallic compounds are formed at high temperature under an inert atmosphere or in vacuum. The resulting samples are characterized by X-ray diffraction and by scanning electron microscopy. Keywords : Intermetallic compounds, Gold nanoparticles, Thin films, Gas sensor

Heat capacity of the ZrAu compound obtained by high-temperature drop calorimetry.

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