Structural Investigations on the Compositional Anomalies in Lanthanum Zirconate System Synthesized by Coprecipitation Method

The study set out to investigate the compositional inconsistency in lanthanum zirconate system revealed the presence of nonstoichiometry in lanthanum zirconate powders when synthesized by coprecipitation route. X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) investigations confirmed the depletion of La3+ ions in the system. Analysis using Vegard's law showed the La/Zr mole ratio in the sample to be around 0.45. An extra step of ultrasonication, introduced during the washing stage followed by the coprecipitation reaction, ensured the formation of stoichiometric La2Zr2O7. Noteworthy is also the difference between crystal sizes in the samples prepared by with and without ultrasonication step. This difference has been explained in light of the formation of individual nuclei and their scope of growth within the precipitate core. The differential scanning calorimetry (DSC) analyses revealed that optimum pH for the synthesis of La2Zr2O7 is about 11. The ultrasonication step was pivotal in assuring consistency in mixing and composition for the lanthanum zirconate powders.

Surface chemical studies on mica and galena using dextrin

The interactions of dextrin with biotite mica and galena have been investigated through adsorption, flotation, and electrokinetic measurements. The adsorption densities of dextrin onto mica continuously increase with increase of pH, while those onto galena show a maximum at pH 11.5. It is observed that the adsorption density of dextrin onto galena is quite high compared to that on mica. Both the adsorption isotherms exhibit Langmuirian behavior. Electrokinetic measurements portray conformational rearrangements of macromolecules with the loading, resulting in a shift of the shear plane, further away from the interface. Dissolution experiments indicate release of the lattice metal ions from mica and galena. Coprecipitation tests confirm polymer-metal ion interaction in the bulk solution. Dextrin does not exhibit any depressant action toward mica, whereas, with galena, the flotation recovery is decreased with an increase in pH beyond 9, in the presence of dextrin, complementing the adsorption results. Differential flotation results on a synthetic mixture of mica and galena show that mica can be selectively separated from galena using dextrin as a depressant for galena above pH 10. Possible mechanisms of interaction between dextrin and mica/galena are discussed.

Synthesis and enhanced green photoluminescence emission from BCT ZnS nanocrystals

Body-centered-tetragonal (BCT) ZnS nanocrystals have been synthesized, for the first time to the best of our knowledge, by using the chemical coprecipitation method at higher synthesis temperatures of 65 and 95 degrees C. It is confirmed from X-ray diffraction (XRD) studies that in the high-temperature-synthesized samples, cubic and BCT phases coexist, in contrast to the room-temperature-synthesized sample, which consists of only cubic phase with sizes of the particles lying between 2 and 3 nm. The sizes of BCT phase nanocrystals are bigger than those of cubic phase of ZnS. The presence of BCT phase of ZnS in the samples is increased from 40 to 90% when the temperature of synthesis is increased from 65 to 95 degrees C. The nanocrystalline nature and UV-Vis absorption characteristics of the prepared samples have been studied with a transmission electron microscope (TEM) and a UV-Visible pectrophotometer, respectively. The room-temperature-synthesized ZnS sample shows photoluminescence (PL) emission in the blue region with multiple peaks, whereas the high-temperature-synthesized samples show PL emissions in the visible region. The Gaussian fittings of the measured PL spectra shows that three PL peaks at 429, 477, and 525 nm are appeared in the 65 degrees C sample and two peaks at 491 and 540 nm appear in the 95 degrees C sample with the enhanced PL intensity of the green peak at 540 nm. (C) 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Characterization of coprecipitated ferroelectric Bi2 VO5·5

Fine powders of orthorhombic bismuth vandate (Bi2VO5.5) have been synthesized by coprecipitation method. Powder X-ray diffraction and electron microscopic techniques have been used to characterize these samples. The formation of the monophasic Bi2VO5.5 was confirmed. The compacted powders sintered at 1070 K have been characterized for their dielectric properties as a function of both temperature (300-900 K) and frequency (100 Hz-10 MHz) and found to be superior to those obtained by the conventional solid-state reaction route.

A comparative study of Pt/CeO2 catalysts for catalytic partial oxidation of methane to syngas for application in fuel cell electric vehicles

In the framework of a project aimed at developing a reliable hydrogen generator for mobile polymer electrolyte fuel cells (PEFCs), particular emphasis has been addressed to the analysis of catalysts able to assure high activity and stability in transient operations (frequent start-up and shut-down cycles). In this paper, the catalytic performance of 1 at.% Pt/ceria samples prepared by coprecipitation, impregnation and combustion, has been evaluated in the partial oxidation of methane. Methane conversion and hydrogen selectivity of 96 and 99%, respectively, associated with high stability during 100h of reaction under operative conditions (start-up and shut-down cycles), have been obtained. (C) 2002 Elsevier Science B.V. All rights reserved.

Surfactant-mediated Synthesis of Functional Metal Oxide Nanostructures via Microwave Irradiation-assisted Chemical Synthesis

Nanostructured materials have attracted considerable interest in recent years due to their properties which differ strongly from their bulk phase and potential applications in nanoscale electronic and optoelectronic devices. Metal oxide nanostructures can be synthesized by variety of different synthesis techniques developed in recent years such as thermal decomposition, sol-gel technique, chemical coprecipitation, hydrothermal process, solvothermal process, spray pyrolysis, polyol process etc. All the above processes go through a tedious synthesis procedure followed by prolonged heat treatment at elevated temperature and are time consuming. In the present work we describe a rapid microwave irradiation-assisted chemical synthesis technique for the growth of nanoparticles, nanorods, and nanotubes of a variety of metal oxides in the presence of an appropriate surfactant, without the use of any templates The method is simple, inexpensive, and helps one to prepare nanostructures in a very simple way, and in a very short time, measured in minutes. The synthesis procedure employs high quality metalorganic complexes (typically -diketonates) featuring a direct metal-to-oxygen bond in its molecular structure. The complex is dissolved in a suitable solvent, often with a surfactant added, and the solution then subjected to microwave irradiation in a domestic microwave oven operating at 2.45 GHz frequency with power varying from 160-800 W, from a few seconds to a few minutes, leading to the formation of corresponding metal oxides. This method has been used successfully to synthesize nanostructures of a variety of binary and ternary metal oxides such as ZnO, CdO, Fe2O3, CuO, Ga2O3, Gd2O3, ZnFe2O4, etc. There is an observed variation in the morphology of the nanostructures with the change of different parameters such as microwave power, irradiation time, appropriate solvent, surfactant type and concentration. Cationic, anionic, nonionic and polymeric surfactants have been used to generate a variety of nanostructures. Even so, to remove the surfactant, there is either no need of heat treatment or a very brief exposure to heat suffices, to yield highly pure and crystalline oxide materials as prepared. By adducting the metal complexes, the shape of the nanostructures can be controlled further. In this manner, very well formed, single-crystalline, hexagonal nanorods and nanotubes of ZnO have been formed. Adducting the zinc complex leads to the formation of tapered ZnO nanorods with a very fine tip, suitable for electron emission applications. Particle size and their monodispersity can be controlled by a suitable choice of a precursor complex, the surfactant, and its concentration. The resulting metal oxide nanostructures have been characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, FTIR spectroscopy, photoluminescence, and electron emission measurements.

Photoluminescence of Sr(2-x)Ln(x)CeO(4+x/2) (Ln = Eu, Sm or Yb) prepared by a wet chemical method

A wet chemical route is developed for the preparation of Sr2CeO4 denoted the carbonate-gel composite technique. This involves the coprecipitation of strontium as fine particles of carbonates within hydrated gels of ceria (CeO2.xH(2)O, 40

Low‐voltage varistors based on zinc antimony spinel Zn7Sb2O12

It is possible to prepare low‐voltage varistors from the zinc antimony spinel Zn7Sb2O12 with breakdown voltages in the range of 3–20 V and nonlinearity coefficient α=7–15. The varistor property is due to the formation of high ohmic potential barriers at the grain boundary regions on low‐ohmic n‐type grain interiors of the polycrystalline samples. The method of preparation of the spinel, synthesized by coprecipitation followed by annealing under restricted partial pressures of oxygen, controls the mixed valence states for antimony, namely, Sb3+ and Sb5+. This is critical in attaining high nonlinearity and lower breakdown voltages.

Exfoliation of copper hydroxysalt in water and the conversion of the exfoliated layers to cupric and cuprous oxide nanoparticles

P-aminobenzoate- intercalated copper hydroxysalt was prepared by coprecipitation at high pH (similar to 12). As the pH was reduced to similar to 7 on washing with water, the development of partial positive charge on the amine end of the intercalated anion caused repulsion between the layers leading to delamination and colloidal dispersion of monolayers of copper hydroxysalt in water. The dispersed copper hydroxysalt monolayers were used as precursors for the synthesis of copper(I)/(II) oxide nanoparticles at room temperature. While the hydroxysalt layers yielded spindle-shaped CuO particles when left to stand, they formed hollow spherical nanoparticles of Cu(2)O when treated with an alkaline solution of ascorbic acid.

Synthesis and characterization of Fe- and Co-based ferrite nanoparticles and study of the T-1 and T-2 relaxivity of chitosan-coated particles

In pursuit of newer and more effective contrast agents for magnetic resonance imaging, we report in this article the use of biocompatible chitosan-coated ferrite nanoparticles of different kinds with a view to determine their potential applications as the contrast agents in the field of nuclear magnetic resonance. The single-phase ferrite particles were synthesized by chemical co-precipitation (CoFe2O4 and Fe3O4) and by applying ultrasonic vibration (CoFe2O4 and Co0.8Zn0.2Fe2O4). Although magnetic anisotropy of CoFe2O4 nanoparticle leads to finite coercivity even for nanoensembles, it has been reduced significantly to a minimum level by applying ultrasonic vibration. Fe3O4 synthesized by chemical co-precipitation yielded particles which already possess negligible coercivity and remanence. Substitution of Co by Zn in CoFe2O4 increases the magnetization significantly with a small increase in coercivity and remanence. Particles synthesized by the application of ultrasonic vibration leads to the higher values of T-2 relaxivities than by chemical coprecipitation. We report that the T-2 relaxivities of these particles are of two orders of magnitude higher than corresponding T-1 relaxivities. Thus, these particles are evidently suitable as contrast agent for T-2 weighted MR images.

Graphene Oxide-MnFe2O4 Magnetic Nanohybrids for Efficient Removal of Lead and Arsenic from Water

We show that the hybrids of single-layer graphene oxide with manganese ferrite magnetic nanoparticles have the best adsorption properties for efficient removal of Pb(II), As(III), and As(V) from contaminated water. The nanohybrids prepared by coprecipitation technique were characterized using atomic force and scanning electron microscopies, Fourier transformed infrared spectroscopy, Raman spectroscopy, X-ray diffraction, and surface area measurements. Magnetic character of the nanohybrids was ascertained by a vibrating sample magnetometer. Batch experiments were carried out to quantify the adsorption kinetics and adsorption capacities of the nanohybrids and compared with the bare nanoparticles of MnFe2O4. The adsorption data from our experiments fit the Langmuir isotherm, yielding the maximum adsorption capacity higher than the reported values so far. Temperature-dependent adsorption studies have been done to estimate the free energy and enthalpy of adsorption. Reusability, ease of magnetic separation, high removal efficiency, high surface area, and fast kinetics make these nanohybrids very attractive candidates for low-cost adsorbents for the effective coremoval of heavy metals from contaminated water.