A simple miniature furnace for routine collection of single crystal x-ray data up to 1000°C on the Hilger and Watts linear diffractometer

A miniature furnace suitable for routine collection of x-ray data up to 1000°C from single crystals on the Hilger and Watts linear diffractometer, without restricting the normally allowed region of reciprocal space on the diffractometer, is described. The crystal is heated primarily by radiation from a surrounding current-heated, stationary platinum coil wound on a silica bracket. The coil is split at its middle to provide a 4 mm gap for crystal mounting and x-irradiation. The crystal, mounted on a standard goniometer head, can be rotated and centred freely, as in the room temperature case. There is no need for any radiation shields or water-cooling arrangement. Investigations up to 1500°C are possible with slight modifications of the furnace.

Cerimetry in nonaqueous media - Oxidation of ascorbic acid

The reaction between ascorbic acid and ammonium hexa nitrato cerate was studied potentiometrically in the mixed solvent glacial acetic acid acetonitrile medium. It was found that one mole of ascorbic acid consumes four equivalents of cerate in non-aqueous medium. This reaction can be made use of to estimate potentiometrically ascorbic acid with ammonium nitrato cerate in non-aqueous media, using either glass or antimony as reference electrode and platinum as indicator electrode.

Potentiometric titrations in nonaqueous cerimetry

Potassium iodide and hydroquinone can be estimated potentiometrically in nonaqueous medium using ammonium nitrato cerate as oxidant. A platinum indicator electrode coupled with either a glass electrode or an antimony electrode as reference electrode, can be used in nonaqueous medium satisfactorily, for following the potentiometric titration. Direct potentiometric titration of xanthate with ammonium nitrato cerate in nonaqueous medium yields slightly lower values than the actual values in presence of platinum indicator electrode.

A Durable PEFC with Carbon-Supported Pt-TiO2 Cathode: A Cause and Effect Study

Durability is central to the commercialization of polymer electrolyte fuel cells (PEFCs). The incorporation of TiO2 with platinum (Pt) ameliorates both the stability and catalytic activity of cathodes in relation to pristine Pt cathodes currently being used in PEFCs. PEFC cathodes comprising carbon-supported Pt-TiO2 (Pt-TiO2/C) exhibit higher durability in relation to Pt/C cathodes as evidenced by cell polarization, impedance, and cyclic voltammetry data. The degradation in performance of the Pt-TiO2/C cathodes is 10% after 5000 test cycles as against 28% for Pt/C cathodes. These data are in conformity with the electrochemical surface area and impedance values. Pt-TiO2/C cathodes can withstand even 10,000 test cycles with nominal effect on their performance. X-ray diffraction, transmission electron microscope, and cross-sectional field-emission-scanning electron microscope studies on the catalytic electrodes reflect that incorporating TiO2 with Pt helps in mitigating the aggregation of Pt particles and protects the Nafion membrane against peroxide radicals formed during the cathodic reduction of oxygen. (C) 2010 The Electrochemical Society. [DOI: 10.1149/1.3421970] All rights reserved.

PEDOT-PSSA as an alternative support for Pt electrodes in PEFCs

Poly (3,4-ethylenedioxythiophene) (PEDOT) and poly (styrene sulphonic acid) (PSSA) supported platinum (Pt) electrodes for application in polymer electrolyte fuel cells (PEFCs) are reported. PEDOT-PSSA support helps Pt particles to be uniformly distributed on to the electrodes, and facilitates mixed electronic and ionic (H+-ion) conduction within the catalyst, ameliorating Pt utilization. The inherent proton conductivity of PEDOT-PSSA composite also helps reducing Nation content in PEFC electrodes. During prolonged operation of PEFCs, Pt electrodes supported onto PEDOT-PSSA composite exhibit lower corrosion in relation to Pt electrodes supported onto commercially available Vulcan XC-72R carbon. Physical properties of PEDOT-PSSA composite have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. PEFCs with PEDOT-PSSA-supported Pt catalyst electrodes offer a peak power-density of 810 mW cm(-2) at a load current-density of 1800 mA cm(-2) with Nation content as low as 5 wt.% in the catalyst layer. Accordingly, the present study provides a novel alternative support for platinized PEFC electrodes.

PEDOT-PSSA as an alternative support for Pt electrodes in PEFCs

Poly (3,4-ethylenedioxythiophene) (PEDOT) and poly (styrene sulphonic acid) (PSSA) supported platinum (Pt) electrodes for application in polymer electrolyte fuel cells (PEFCs) are reported. PEDOT-PSSA support helps Pt particles to be uniformly distributed on to the electrodes, and facilitates mixed electronic and ionic (H+-ion) conduction within the catalyst, ameliorating Pt utilization. The inherent proton conductivity of PEDOT-PSSA composite also helps reducing Nation content in PEFC electrodes. During prolonged operation of PEFCs, Pt electrodes supported onto PEDOT-PSSA composite exhibit lower corrosion in relation to Pt electrodes supported onto commercially available Vulcan XC-72R carbon. Physical properties of PEDOT-PSSA composite have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. PEFCs with PEDOT-PSSA-supported Pt catalyst electrodes offer a peak power-density of 810 mW cm(-2) at a load current-density of 1800 mA cm(-2) with Nation content as low as 5 wt.% in the catalyst layer. Accordingly, the present study provides a novel alternative support for platinized PEFC electrodes

Development of thermoelectric gas sensors for volatile organic compounds

This paper describes the design and development of a thermoelectric gas sensor suitable for the detection of Volatile Organic Compounds (VOCs). In order to enhance the seebeck coefficient of the sensor, we have deposited chromium metal films on a limited area of the glass substrate. Tin oxide thin film was deposited on top of these metal films. The resulting metal/semiconductor film exhibits a high seebeck coefficient of 400 mu V/ degrees C. Platinum catalyst film deposited on the oxide film to create the necessary temperature gradient resulted in further enhancement in the sensitivity of the sensor to target gases. The sensor shows high sensitivity to ppm-change in the concentration of target hydrocarbons at a relatively low temperature of 120 degrees C.

Simultaneous measurement of aerodynamic and heat transfer data for large angle blunt cones in hypersonic shock tunnel

Aerodynamic forces and fore-body convective surface heat transfer rates over a 60 degrees apex-angle blunt cone have been simultaneously measured at a nominal Mach number of 5.75 in the hypersonic shock tunnel HST2. An aluminum model incorporating a three-component accelerometer-based balance system for measuring the aerodynamic forces and an array of platinum thin-film gauges deposited on thermally insulating backing material flush mounted on the model surface is used for convective surface heat transfer measurement in the investigations. The measured value of the drag coefficient varies by about +/-6% from the theoretically estimated value based on the modified Newtonian theory, while the axi-symmetric Navier-Stokes computations overpredict the drag coefficient by about 9%. The normalized values of measured heat transfer rates at 0 degrees angle of attack are about 11% higher than the theoretically estimated values. The aerodynamic and the heat transfer data presented here are very valuable for the validation of CFD codes used for the numerical computation of How fields around hypersonic vehicles.

Low temperature processing and chacterization of SrBi2Nb2O9 thin films grown by pulsed laser ablation

Ex-situ grown thin films of SrBi2Nb2O9 (SBN) were deposited on platinum substrates using laser ablation technique. A low substrate-temperature-processing route was chosen to avoid any diffusion of bismuth into the Pt electrode. It was observed that the as grown films showed an oriented growth along the 'c'-axis (with zero spontaneous polarization). The as grown films were subsequently annealed to enhance crystallization. Upon annealing, these films transformed into a polycrystalline structure, and exhibited excellent ferroelectric properties. The switching was made to be possible by lowering the thickness without losing the electrically insulating behavior of the films. The hysteresis results showed an excellent square-shaped loop with results (P-r = 4 muC/cm(2) E-c = 90 kV/cm) in good agreement with the earlier reports. The films also exhibited a dielectric constant of 190 and a dissipation factor of 0.02, which showed dispersion at low frequencies. The frequency dispersion was found to obey Jonscher's universal power law relation, and was attributed to the ionic charge hopping process according to earlier reports. The de transport studies indicated an ohmic behavior in the low voltage region, while higher voltages induced a bulk space charge and resulted in non-linear current-voltage dependence.

Preparation and characterization of silane-stabilized, highly uniform, nanobimetallic Pt-Pd particles in solid and liquid matrixes

Highly uniform, stable nanobimetallic dispersions are prepared in a single si ep in the form of sols, gels, and monoliths, using organically modified silicates as the matrix and the stabilizer. The Pt-Pd bimetallic dispersions are characterized by W-vis, TEM, SEM, and XRD measurements. The evolution of silicate was followed by IR spectroscopy. XPS and CO adsorption studies reveal that the structure of the particles consists of a palladium core and a platinum shell. Electrocatalysis of ascorbic acid oxidation has been demonstrated using thin films of silicate containing the nanobimetal particles on a glassy carbon electrode.

Structural, optical and electrical characteristics of transparent bismuth vanadate films deposited on indium tin oxide coated glass substrates

Bismuth vanadate (BVO) thin films were fabricated on indium tin oxide (ITO) coated glass substrates using pulsed laser ablation technique and investigated their structural, optical and electrical properties. The use of the indium tin oxide coated glass substrate resulted in reducing the leakage current characteristics of crystalline BVO thin films. The X-ray diffraction (XRD) studies confirmed the monophasic nature of the post annealed (500 A degrees C/1 h) films. The atomic force microscopy indicated the homogeneous distribution of crystallites in the as-deposited films. The as-deposited and the post annealed films were almost 90% transparent (380-900 nm) as confirmed by optical transmission studies. Dielectric constant of around 52 was attained accompanied by the low dielectric loss of 0.002 at 10 kHz for post annealed films. The leakage current of the post annealed BVO films on ITO coated glass substrates measured at room temperature was 8.1 x 10(-8) A at an applied electric field of 33 kV/cm, which was lower than that of the films with platinum and SrRuO3 as the bottom electrodes.

Mesoporous Carbon and Poly(3,4-ethylenedioxythiophene) Composite as Catalyst Support for Polymer Electrolyte Fuel Cells

In situ polymerization of 3,4-ethylenedioxythiophene with sol-gel-derived mesoporous carbon (MC) leading to a new composite and its subsequent impregnation with Pt nanoparticles for application in polymer electrolyte fuel cells (PEFCs) is reported. The composite exhibits good dispersion and utilization of platinum nanoparticles akin to other commonly used microporous carbon materials, such as carbon black. Pt-supported MC-poly(3,4-ethylenedioxythiophene) (PEDOT) composite also exhibits promising electrocatalytic activity toward oxygen reduction reaction, which is central to PEFCs. The PEFC with Pt-loaded MC-PEDOT support exhibits 75% of enhancement in its power density in relation to the PEFC with Pt-loaded pristine MC support while operating under identical conditions. It is conjectured that Pt-supported MC-PEDOT composite ameliorates PEFC performance/durability on repetitive potential cycling. (C) 2010 The Electrochemical Society. DOI: 10.1149/1.3486172] All rights reserved.

Selective-Area Atomic Layer Deposition

Atomic layer deposition (ALD) is a method to deposit thin films from gaseous precursors to the substrate layer-by-layer so that the film thickness can be tailored with atomic layer accuracy. Film tailoring is even further emphasized with selective-area ALD which enables the film growth to be controlled also on the substrate surface. Selective-area ALD allows the decrease of a process steps in preparing thin film devices. This can be of a great technological importance when the ALD films become into wider use in different applications. Selective-area ALD can be achieved by passivation or activation of a surface. In this work ALD growth was prevented by octadecyltrimethoxysilane, octadecyltrichlorosilane and 1-dodecanethiol SAMs, and by PMMA (polymethyl methacrylate) and PVP (poly(vinyl pyrrolidone) polymer films. SAMs were prepared from vapor phase and by microcontact printing, and polymer films were spin coated. Microcontact printing created patterned SAMs at once. The SAMs prepared from vapor phase and the polymer mask layers were patterned by UV lithography or lift-off process so that after preparation of a continuous mask layer selected areas of them were removed. On these areas the ALD film was deposited selectively. SAMs and polymer films prevented the growth in several ALD processes such as iridium, ruthenium, platinum, TiO2 and polyimide so that the ALD films did grow only on areas without SAM or polymer mask layer. PMMA and PVP films also protected the surface against Al2O3 and ZrO2 growth. Activation of the surface for ALD of ruthenium was achieved by preparing a RuOX layer by microcontact printing. At low temperatures the RuCp2-O2 process nucleated only on this oxidative activation layer but not on bare silicon.

Electrical transport in magnesium aluminate

The conductivity of MgAl2O4 has been measured at 1273, 1473 and 1673 K as a function of the partial pressure of oxygen ranging from 105 to 10−14 Pa. The MgAl2O4 pellet, sandwiched between two platinum electrodes, was equilibrated with a flowing stream of either Ar + O2, CO + CO2 or Ar + H2 + H2O mixture of known composition. The gas mixture established a known oxygen partial pressure. All measurements were made at a frequency of 1 kHz. These measurements indicate pressure independent ionic conductivity in the range 1 to 10−14 Pa at 1273 K, 10−1 to 10−12 Pa at 1473 K and 10−1 to 10−4 Pa at 1673 K. The activation energy for ionic conduction is 1·48 eV, close to that for self-diffusion of Mg2+ ion in MgAl2O4 calculated from the theoretical relation of Glyde. Using the model, the energy for cation vacancy formation and activation energy for migration are estimated.

A study of chemically prepared small metal clusters in the nonmetallic regime

Small gold clusters [mean diameter (d)[less, similar] 1.4 nm], unlike larger clusters, show a higher Au(4f) binding energy relative to the bulk value and the presence of a conductance gap in tunnelling measurements, just as the molecular cluster compound, Au55(PPh3)12Cl6; small platinum clusters show similar nonmetallic features.