Combustion synthesis and properties of Ce1-xPrxO2-delta red ceramic pigments

Praseodymium-doped ceria red pigments, Ce1−xPrxO2−δ, x=0–0.5 have been prepared by the thermal decomposition of the redox compound Ce1−xPrx(N2H3COO)3·3H2O as well as by the combustion of aqueous solutions containing cerous nitrate, praseodymium nitrate and oxalyl dihydrazide (ODH)/ammonium acetate. Formation of the pigment has been confirmed by its characteristic red colour and reflectance spectra which shows the reflection edge not, vert, similar690 nm corresponding to charge transfer from the ligand orbitals to the localised 4f1 of Pr4+. The particulate properties of praseodymium-doped ceria pigments obtained from the combustion of redox compounds and redox mixtures are compared.

Radiation resistance of PFN and PNM-PT relaxor ferroelectrics

The relaxor ferroelectric compositions Pb(Fe1/2Nb1/2)O-3 (PEN) and [Pb(Mg1/3Nb2/3)O-3](0.8)-[PbTiO3](0.2) (PMN-PT) are studied for their radiation response to the high energy heavy ions (50 MeV Li3+, fluence 1 X 10(13)-1 X 10(14) ions/cm(2)) in terms of their structural, dielectric and piezoelectric properties. There was no change in the crystallinity of both the compositions after irradiation as seen from the XRD. The PEN composition did not show much change in the dielectric constant but the value of T-m decreased by 8degreesC. The PMN-PT composition showed an increase in the dielectric constant with increase in the irradiation fluence from 1 x 10(13) to 1 X 10(14) ions/cm(2) with no change in the value of T-m. The piezoelectric coefficient decreased in both the samples after irradiation. Among the compositions studied, PEN is observed to be more radiation resistant to changes in structural and dielectric properties than PM-PT. (C) 2003 Elsevier Ltd. All rights reserved.

Fe–Cr/Al2O3 metal-ceramic composites: Nature and size of the metal particles formed during hydrogen reduction

Fe-Cr/Al2O3 metal-ceramic composites prepared by hydrogen reduction at different temperatures and for different periods have been investigated by a combined use of Mössbauer spectroscopy, x-ray diffraction, transmission electron microscopy, and energy-dispersive x-ray spectroscopy in order to obtain information on the nature of the metallic species formed. Total reduction of Fe3+ does not occur by increasing the reduction time at 1320 K from 1 to 30 h, and the amount of superparamagnetic metallic species is essentially constant (about 10%). Temperatures higher than 1470 K are needed to achieve nearly total reduction of substitutional Fe3+. Interestingly, iron favors the reduction of chromium. The composition of the Fe-Cr particles is strongly dependent on their size, the Cr content being higher in particles smaller than 10 nm.

Compositionally modulated Pb(Mg1/3Nb2/3)O-3-PbTiO3 relaxor thin films deposited by pulsed excimer laser ablation technique

Thin films of (1-x)Pb(Mg1/3Nb2/3)O-3 - xPbTiO(3) (x = 0.1 to 0.3)(PMN-PT) were deposited on the platinum coated silicon substrate by pulsed excimer laser ablation technique. A template layer of LaSr0.5Co0.5O3 (LSCO) was deposited on platinum substrate prior to the deposition of PMN-PT thin films. The composition and the structure of the films were modulated via proper variation of the deposition parameter such as substrate temperature, laser fluence and thickness of the template layers. We observed the impact of the thickness of LSCO template layer on the orientation of the films. A room temperature dielectric constant varying from 2000 to 4500 was noted for different composition of the films. The dielectric properties of the films were studied over the frequency range of 100 Hz - 100 kHz over a wide range of temperatures. The films exhibited the relaxor- type behavior that was characterized by the frequency dispersion of the temperature of dielectric constant maxima (T-m) and also diffuse phase transition. C1 Indian Inst Sci, Mat Res Ctr, Bangalore, Karnataka 560012 India.

Compositionally and structurally modulated Pb(Mg1/3Nb2/3)O3-PbTiO3 relaxor thin films for microactuator application

Thin films of (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3(x = 0.1 to 0.3) (PMN-PT) were successfully grown on the platinum coated silicon substrate by pulsed excimer laser ablation technique. A thin template layer of LaSr0.5Co0.5O3 (LSCO) was deposited on platinum substrate prior to the deposition of PMN-PT thin films. The composition and the structure of the films were modulated via proper variation of the deposition parameter such as substrate temperature, laser fluence and thickness of the template layers. We observed the impact of the thickness of LSCO template layer on the orientation of the films. The crystallographic structure and compositional variation were confirmed with x-ray diffraction and energy diffraction x-ray (EDX) analysis. A room temperature dielectric constant varying from 2000 to 4500 was noted for different composition of the films. The dielectric properties of the films were studied over the frequency range of 100 Hz - 100 kHz over a wide range of temperatures. The films exhibited the relaxor-type behavior that was characterized by the frequency dispersion of the temperature of dielectric constant maxima (Tm) and also diffuse phase transition. This relaxor nature in PMN-PT thin films was attributed to freezing of the dipole moment, which takes place below a certain temperature. This phenomenon was found to be very similar to spin glass system, where spins are observed to freeze after certain temperature.

Relaxor Ferroelectric Behavior and Structural Aspects of SrNaBi2Nb3O12 Ceramics

The SrNaBi2Nb3O12 (SNBN) powder was prepared via the conventional solid-state reaction method. X-ray structural studies confirmed the phase to be a three-layered member of the Aurivillius family of oxides. The SNBN ceramics exhibited the typical characteristics of relaxor ferroelectrics, associated with broad and dispersive dielectric maxima. The variation of temperature of dielectric maxima (T-m) with frequency obeyed the Vogel-Fulcher relationship. Relaxor behavior was believed to be arising from the cationic disorder at A-site. Pinched ferroelectric hysteresis loops were observed well above T-m.

Structural and relaxor characteristics of Ca0.18Sr0.226Ba0.594Nb2O6

Polycrystalline Ca0.18Sr0.226Ba0.594Nb2O6 (CSBN18) was synthesized via the solid-state reaction route. X-ray structural studies confirmed it belonged to the tetragonal tungsten bronze family. Rietveld refinement of the X-ray data has been carried out for CSBN18 where the atomic positions and site occupancy factors for A-sites have been determined. The dielectric properties of CSBN18 ceramic were studied as a function of temperature in the 100 Hz - 1 MHz frequency range. The dielectric relaxation followed the Vogel-Fulcher relation wherein E-a = 37.4 meV; T-f = 131.5 degrees C and omega(0) = 4.31 x 10(9) rad s(-1). A high pyroelectric coefficient of similar to 250 mu C m(-2).K was obtained around the transition temperature (similar to 150 degrees C). This is significantly higher than that reported for polycrystalline SrxBa1-xNb2O6 (SBN). However, the piezoelectric coefficient (d(33)) of the title composition was as low as 6 pC N-1.

Porous wide band gap BiNbO4 ceramic nanopowder synthesised by low temperature solution-based method for gas sensing applications

In this study, we report the gas sensing behavior of BiNbO4 nanopowder prepared by a low temperature simple solution-based method. Before the sensing behaviour study, the as-synthesized nanopowder was characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, UV-diffuse reflectance spectroscopy, impedance analysis, and surface area measurement. The NH3 sensing behavior of BiNbO4 was then studied by temperature modulation (50-350 degrees C) as well as concentration modulation (20-140 ppm). At the optimum operating temperature of 325 degrees C, the sensitivity was measured to be 90%. The cross-sensitivity of as-synthesized BiNbO4 sensor was also investigated by assessing the sensing behavior toward other gases such as hydrogen sulphide (H2S), ethanol (C2H5OH), and liquid petroleum gas (LPG). Finally, selectivity of the sensing material toward NH3 was characterized by observing the sensor response with gas concentrations in the range 20-140 ppm. The response and recovery time for NH3 sensing at 120 ppm were about 16 s and about 17 s, respectively.

Tuning of dielectric, pyroelectric and ferroelectric properties of 0.715Bi(0.5)Na(0.5)TiO(3)-0.065BaTiO(3)-0.22SrTiO(3) ceramic by internal clamping

This study systematically investigates the phenomenon of internal clamping in ferroelectric materials through the formation of glass-ceramic composites. Lead-free 0.715Bi(0.5)Na(0.5)TiO(3)-0.065BaTiO(3)-0.22SrTiO(3) (BNT-BT-ST) bulk ferroelectric ceramic was selected for the course of investigation. 3BaO - 3TiO(2) - B2O3 (BTBO) glass was then incorporated systematically to create sintered samples containing 0%, 2%, 4% and 6% glass (by weight). Upon glass induction features like remnant polarization, saturation polarization, hysteresis losses and coercive field could be varied as a function of glass content. Such effects were observed to benefit derived applications like enhanced energy storage density similar to 174 k J/m(3) to similar to 203 k J/m(3) and pyroelectric coefficient 5.7x10(-4) Cm-2K-1 to 6.8x10(-4) Cm-2K-1 by incorporation of 4% glass. Additionally, BNT-BT-ST depolarization temperature decreased from 457K to 431K by addition of 4% glass content. Glass incorporation could systematically increases diffuse phase transition and relaxor behavior temperature range from 70 K to 81K and 20K to 34 K, respectively when 6% and 4% glass content is added which indicates addition of glass provides better temperature stability. The most promising feature was observed to be that of dielectric response tuning. It can be also used to control (to an extent) the dielectric behavior of the host ceramic. Dielectric permittivity and losses decreased from 1278 to 705 and 0.109 to 0.107 for 6% glass, at room temperature. However this reduction in dielectric constant and loss increases pyroelectric figures of merit (FOMs) for high voltage responsivity (F-v) high detectivity (F-d) and energy harvesting (F-e) from 0.018 to 0.037 m(2)C(-1), 5.89 to 8.85 mu Pa-1/2 and 28.71 to 61.55 Jm(-3)K(-2), respectively for 4% added ceramic-glass at room temperature. Such findings can have huge implications in the field of tailoring ferroelectric response for application specific requirements. (C) 2015 Author(s).

Primary and rechargeable zinc-air batteries using ceramic and highly stable TiCN as an oxygen reduction reaction electrocatalyst

Primary and secondary zinc-air batteries based on ceramic, stable, one dimensional titanium carbonitride (TiCN) nanostructures are reported. The optimized titanium carbonitride composition by density functional theory reveals their good activity towards the oxygen reduction reaction (ORR). Electrochemical measurements show their superior performance for the ORR in alkaline media coupled with favourable kinetics. The nanostructured TiCN lends itself amenable to be used as an air cathode material in primary and rechargeable zinc-air batteries. The battery performance and cyclability are found to be good. Further, we have demonstrated a gel-based electrolyte for rechargeable zinc-air batteries based on a TiCN cathode under ambient, atmospheric conditions without any oxygen supply from a cylinder. The present cell can work at current densities of 10-20 mA cm(2) (app. 10 000 mA g(-1) of TiCN) for several hours (63 h in the case of 10 mA cm(-2)) with a charge retention of 98%. The low cost, noble metal-free, mechanically stable and corrosion resistant TiCN is a very good alternative to Pt for metal-air battery chemistry.

Structural characterization, stability and electrical properties of strontium niobate ceramic

The double perovskite oxide Sr2CrNbO6 has a cubic structure according to powder X-ray diffraction. After reducing in CO, Sr2CrNbO6 still exhibited a cubic structure refined by Rietveld technique. The TG analysis indicated that Sr2CrNbO6 loses 0.127 oxygen per formula unit from 400 to 700 degrees C in H-2. The morphology and compositions of this ceramic did not significantly change on reduction

Application of ceramic carbon materials for solid-phase extraction of organic compounds

Ceramic carbon materials were developed as new sorbents for solid-phase extraction of organic compounds using chlorpromazine as a representative. The macroporosity and heterogeneity of ceramic carbon materials allow extracting a large amount of chlorpromazine over a short time. Thus, the highly sensitive and selective determination of chlorpromazine in urine sample was achieved by differential pulse voltammograms after only 1-min extraction. The total analysis time was less than 3 min. In comparison with other electrochemical and electrochemi-luminescent methods following 1-min extraction, the proposed method improved sensitivity by about 2 and 1 order of magnitude, respectively. The fast extraction, diversity, and conductivity of ceramic carbon materials make them promising sorbents for various solid-phase extractions, such as solid-phase microextraction, thin-film microextraction, and electrochemically controlled solidphase extraction. The preliminary applications of ceramic carbon materials in chromatography were also studied.

Electrochemiluminescent detection based on solid-phase extraction at tris(2,2 '-bipyridyl)ruthenium(II)-modified ceramic carbon electrode

A sensitive electrochemiluminescent detection scheme by solid-phase extraction at Ru(bpy)(3)(2+)-modified ceramic carbon electrodes (CCEs) was developed. The as-prepared Ru(bpy)(3)(2+)-modified CCEs show much better long-term stability than other Nafion-based Ru(bpy)(3)(2+)-modified electrodes and enjoy the inherent advantages of CCEs. The log-log calibration plot for dioxopromethazine is linear from 1.0 x 10(-9) to 1.0 x 10(-4) mol L-1 using the new detection scheme. The detection limit is 6.6 x 10(-10) mol L-1 at a signal-to-noise ratio of 3. The new scheme improves the sensitivity by similar to 3 orders of magnitude, which is the most sensitive Ru(bpy)(3)(2+) ECL method. The scheme allows the detection of dioxopromethazine in a urine sample within 3 min. Since Ru(bpy)(3)(2+) ECL is a powerful technique for determination of numerous amine-containing substances, the new detection scheme holds great promise in measurement of free concentrations, investigation of protein-drug interactions and DNA-drug interactions, pharmaceutical analysis, and so on.

Glassy carbon ceramic composite electrodes

A new carbon composite electrode material, based on dispersing glassy carbon (GC) microparticles into methyltrimethoxysilane-derived sol, is described in the present paper. The resulting glassy carbon ceramic composite electrodes (GCCEs) combine the electrochemical properties of GC with the advantages of composite electrodes, and thus offer high electrochemical reactivity, low background current and are easy to prepare, modify and renew. The new material has a low double-layer capacitance and a wide potential window. Scanning electron microscopy (SEM) images indicate significant difference in the structure of GCCE and carbon ceramic composite electrode (CCE). The electrochemical properties and advantages of GCCE should find broad utility in electroanalysis.

Sol-gel derived carbon ceramic electrode containing methylene blue-intercalted alpha-zirconium phosphate micro particles

Methylene blue-intercalated a-zirconium phosphate (MBZrP) micro particles in deionized water were deposited onto the surface of graphite powder to prepare graphite powder-supported MBZrP, which was subsequently dispersed into methyltrimethoxysilane-derived gels to yield a conductive composite. The composite was used as electrode material to fabricate a surface-renewable, rigid, leak-free carbon ceramic composite electrode, bulk-modified with methylene blue (MB). In the configuration, alpha-zirconium phosphate was employed as a solid host for MB, which acted as a catalyst. Graphite powder ensured conductivity by percolation, the silicate provided a rigid porous backbone and the methyl groups endowed hydrophobicity and thus limited the wetting section of the modified electrode. Peak currents of the MBZrP-modified electrode were surface-confined at low scan rates but diffusion-controlled at high scan rates. Square-wave voltammetric study revealed that MBZrP immobilized in carbon ceramic matrix presented a two-electron, three-proton redox process in acidic aqueous solution with pH ranged from 0.44 to 2.94. In addition, the chemically modified electrode showed an electrocatalytic activity toward nitrite reduction at +0.15 V (vs. Ag/AgCl) in acidic aqueous solution (pH=0.44). The linear range and detection limit are 1 x 10(-6)-4 x 10(-3) mol L-1 and 1.5 x 10(-7) mol L-1, respectively.