Thermal,morphostructural and spectrometric characterization of an antibacterial kaolinite-based filter modified with silver for water treatment

Journal of Thermal Analysis and Calorimetry - The aim of this work is to synthesize and characterize a new structured silver–clay dried, calcined or sintered at different temperatures...     

Tetragonal to monoclinic phase transition observed during Zr anodisation

Plasma electrolytic oxidation (PEO) is a coating procedure that utilises anodic oxidation in aqueous electrolytes above the dielectric breakdown voltage to produce oxide coatings that have specific properties. These conditions facilitate oxide formation under localised high temperatures and pressures that originate from short-lived microdischarges at sites over the metal surface and have fast oxide volume expansion. Anodic ZrO₂ films were prepared by subjecting metallic zirconium to PEO in acid solutions (H₂C₂O₄ and H₃PO₄) using a galvanostatic DC regime. The ZrO₂ microstructure was investigated in films that were prepared at different charge densities. During the anodic breakdown, an important change in the amplitude of the voltage oscillations at a specific charge density was observed (i.e., the transition charge density (Q ^T)). We verified that this transition charge is a monotonic function of both the current density and temperature applied during the anodisation, which indicated that Q ^T is an intrinsic response of this system. The oxide morphology and microstructure were characterised using SEM and X-ray diffraction experiments (XRD) techniques. X-ray diffraction analysis revealed that the change in voltage oscillation was correlated with oxide microstructure changes during the breakdown process.     

A new processing method of CaZn2(OH)6·2H2O powders: Photoluminescence and growth mechanism

In this communication, we report on the formation of calcium hexahydroxodizincate dehydrate, CaZn₂(OH)₆·2H₂O (CZO) powders under microwave-hydrothermal (MH) conditions. These powders were analyzed by X-ray diffraction (XRD), Field-emission gum scanning electron microscopy (FEG-SEM), ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD patterns confirmed that the pure CZO phase was obtained after MH processing performed at 130 °C for 2 h. FEG-SEM micrographs indicated that the morphological modifications as well as the growth of CZO microparticles are governed by Ostwald-ripening and coalescence mechanisms. UV-vis spectra showed that this material have an indirect optical band gap. The pure CZO powders exhibited an yellow PL emission when excited by 350 nm wavelength at room temperature.     

Theoretical and experimental study of disordered Ba0.45Sr0.55 TiO3 photoluminescence at room temperature

Disordered and crystalline Ba_0.45Sr_0.55TiO₃ (BST) powder processed at low temperature was synthesized by the polymeric precursor method. The single-phase perovskite structure of the ceramics was identified by the Raman and X-ray diffraction techniques. Photoluminescence at room temperature was observed only in a disordered BST sample. Increasing the calcination time intensified the photoluminescence (PL), which reached its maximum value in the sample heat treated at 300 °C for 30 h. This emission may be correlated with the structural disorder. Periodic ab initio quantum-mechanical calculations using the CRYSTAL98 program can yield important information regarding the electronic and structural properties of crystalline and disordered solids. The experimental and theoretical results indicate the presence of intermediary energy levels in the band gap. This is ascribed to the break in symmetry, which is responsible for visible photoluminescence in the material’s disordered state at room temperature.     

Thermal and Crystalographic Studies of Mixture La2O3-SrO Prepared Via Reaction in the Solid State

The compound obtained via state solid reaction of the La₂O₃ and SrO oxides and expose the room atmosphere shows the crystallographic data of the compound reported as La₂SrO_x. However, thermogravimetric, differential thermal analysis and XRD with controlled temperature indicated that the stoichiometry of the compound is 2La(OH)₃-SrCO₃, which structural parameters were determined by using the Rietveld method. It was verified that when the compound exposed at room atmosphere, the mixture oxide absorbs H₂O and CO₂ producing hydroxide and carbonate of lanthanum and strontium, respectively, which thermal decomposition occurs by the same steps, producing the La₂O₃-SrO. This revised version was published online in July 2006 with corrections to the Cover Date.     

Contribution of structural order-disorder to the room-temperature photoluminescence of lead zirconate titanate powders

Intense and broad visible photoluminescent (PL) band was observed at room temperature in structurally disordered PbZr_0.53Ti_0.47O₃ powders. The lead zirconate titanate PbZr_0.53Ti_0.47O₃ powders prepared by the polymeric precursor method and heat treated at different temperatures were structurally characterized at long range by means of X-ray diffraction. The PL was measured at room temperature samples heat treated at different temperatures. Experimental measurements and quantum-mechanical calculations showed that the high structural order and the high structural disorder in PbZr_0.53Ti_0.47O₃ lattice are not favorable to the intense PL emission. Only samples containing simultaneous structural order and disorder in their lattice present the intense visible PL emission at room temperature.     

Magnetic doping in Zn7−xMxSb2O12 spinels (M=Ni and Co)

In this article we present a concise report on our studies on the magnetic behavior and structural arrangements of the inverse spinel Zn_7−xM_xSb₂O₁₂ system (M=Ni, Co). Studies on the temperature dependence of the magnetization (M) of several samples in this system showed the occurrence of a spin-glass-like state in temperatures around 10 K. The capability of this system to hold magnetic ions in either octahedral and/or tetrahedral positions is responsible for the occurrence of competing ferromagnetic and antiferromagnetic interactions. This condition is likely to cause the appearance of the observed spin-glass-like behavior.     

Thermal decomposition of crystalline Ni(II)-Cr(III) layered double hydroxide: a structural study of the segregation process

A structural study of the thermal evolution of Ni(0.69)Cr(0.31)(OH)(2)(CO(3))(0.155) x nH(2)O into NiO and tetragonal NiCr(2)O(4) is reported. The characteristic structural parameters of the two coexisting crystalline phases, as well as their relative abundance, were determined by Rietveld refinement of powder x-ray diffraction (PXRD) patterns. The results of the simulations allowed us to elucidate the mechanism of the demixing process of the oxides. It is demonstrated that nucleation of a metastable nickel chromite within the common oxygen framework of the parent Cr(III)-doped bunsenite is the initial step of the cationic redistribution. The role that trivalent cations play in the segregation of crystalline spinels is also discussed.     

Correlation of reactivity with structural factors in a series of Fe(II) substituted cobalt ferrites

A series of powdered cobalt ferrites, Co_xFe_3−xO₄ with 0.66?x<1.00 containing different amounts of Fe^II, were synthesized by a mild procedure, and their Fe and Co site occupancies and structural characteristics were explored using X-ray anomalous scattering and the Rietveld refinement method. The dissolution kinetics, measured in 0.1 M oxalic acid aqueous solution at 70 °C, indicate in all cases the operation of a contracting volume rate law. The specific rates increased with the Fe^II content following approximately a second-order polynomial expression. This result suggests that the transfer of Fe^III controls the dissolution rate, and that the leaching of a first layer of ions Co^II and Fe^II leaves exposed a surface enriched in slower dissolving octahedral Fe^III ions. Within this model, inner vicinal lattice Fe^II accelerates the rate of Fe^III transfer via internal electron hopping. A chain mechanism, involving successive electron transfers, fits the data very well.     

The effects of ZnGa2O4 formation on structural and optical properties of ZnO:Ga powders

Gallium-doped zinc oxide (ZnO:Ga 1, 2, 3, 4 and 5 at%) samples were prepared in powder form by modifying the Pechini method. The formation of zinc gallate (ZnGa₂O₄) with the spinel crystal structure was observed even in ZnO:Ga 1 at% by X-ray diffraction. The presence of ZnGa₂O₄ in ZnO:Ga samples was also evidenced by luminescence spectroscopy through its blue emission at 430 nm, assigned to charge transfer between Ga³⁺ at regular octahedral symmetry and its surrounding O²⁻ ions. The amount of ZnGa₂O₄ increases as the dopant concentration increases, as observed by the quantitative phase analysis by the Rietveld method.