Low temperature molten-salt synthesis of nanocrystalline cubic Sr2SbMnO6

Sr2SbMnO6 (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li2SO4-0.365 Na2SO4 (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 degrees C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with similar to 60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95 +/- 5 kJ mol(-1). The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties.

Unravelling the self-assembly of hydrogen bonded NDI semiconductors in 2D and 3D

Supramolecular ordering of organic semiconductors is the key factor defining their electrical characteristics. Yet, it is extremely difficult to control, particularly at the interface with metal and dielectric surfaces in semiconducting devices. We have explored the growth of n-type semiconducting films based on hydrogen-bonded monoalkylnaphthalenediimide (NDI-R) from solution and through vapor deposition on both conductive and insulating surfaces. We combined scanning tunneling and atomic force microscopies with X-ray diffraction analysis to characterize, at the submolecular level, the evolution of the NDI-R molecular packing in going from monolayers to thin films. On a conducting (graphite) surface, the first monolayer of NDI-R molecules adsorbs in a flat-lying (face-on) geometry, whereas in subsequent layers the molecules pack edge-on in islands (Stranski–Krastanov-like growth). On SiO2, the NDI-R molecules form into islands comprising edge-on packed molecules (Volmer–Weber mode). Under all the explored conditions, self-complementary H bonding of the imide groups dictates the molecular assembly. The measured electron mobility of the resulting films is similar to that of dialkylated NDI molecules without H bonding. The work emphasizes the importance of H bonding interactions for controlling the ordering of organic semiconductors, and demonstrates a connection between on-surface self-assembly and the structural parameters of thin films used in electronic devices.

A germanium/single-walled carbon nanotube composite paper as a free-standing anode for lithium-ion batteries

Paper-like free-standing germanium (Ge) and single-walled carbon nanotube (SWCNT) composite anodes were synthesized by the vacuum filtration of Ge/SWCNT composites, which were prepared by a facile aqueous-based method. The samples were characterized by X-ray diffraction, field emission scanning electron microscopy, and transmission electron microscopy. Electrochemical measurements demonstrate that the Ge/SWCNT composite paper anode with the weight percentage of 32% Ge delivered a specific discharge capacity of 417 mA h g-1 after 40 cycles at a current density of 25 mA g-1, 117% higher than the pure SWCNT paper anode. The SWCNTs not only function as a flexible mechanical support for strain release, but also provide excellent electrically conducting channels, while the nanosized Ge particles contribute to improving the discharge capacity of the paper anode.

A direct borohydride fuel cell employing Prussian Blue as mediated electron-transfer hydrogen peroxide reduction catalyst

A direct borohydride-hydrogen peroxide fuel cell employing carbon-supported Prussian Blue (PB) as mediated electron-transfer cathode catalyst is reported. While operating at 30 °C, the direct borohydride-hydrogen peroxide fuel cell employing carbon-supported PB cathode catalyst shows superior performance with the maximum output power density of 68 mW cm−2 at an operating voltage of 1.1 V compared to direct borohydride-hydrogen peroxide fuel cell employing the conventional gold-based cathode with the maximum output power density of 47 mW cm−2 at an operating voltage of 0.7 V. X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Analysis (EDAX) suggest that anchoring of Cetyl-Trimethyl Ammonium Bromide (CTAB) as a surfactant moiety on carbon-supported PB affects the catalyst morphology. Polarization studies on direct borohydride-hydrogen peroxide fuel cell with carbon-supported CTAB-anchored PB cathode exhibit better performance with the maximum output power density of 50 mW cm−2 at an operating voltage of 1 V than the direct borohydride-hydrogen peroxide fuel cell with carbon-supported Prussian Blue without CTAB with the maximum output power density of 29 mW cm−2 at an operating voltage of 1 V.

Electrophoretic deposition of Ti3Si(Al)C2 from aqueous suspension

Ti3Si(Al)C2 films were electrophoretically deposited at 3 V on indium-tin-oxide (ITO) conductive glass from Ti3Si(Al) C2 aqueous suspension with 1 vol% solid loading at pH 9 in the absence of any dispersant. The surface morphology, cross section microstructure, and preferred orientation of the films were investigated by scanning electron microscopy and X-ray diffraction. The as-deposited Ti3Si(Al)C 2 films exhibited (00l) preferred orientation and the thickness can be controlled by the deposition-drying-deposition method. These results demonstrate that electrophoretic deposition is a simple and feasible method to prepare MAX-phases green films at room temperature.

Anodic deposition of porous RuO2 on stainless steel for supercapacitor studies at high current densities

Ruthenium dioxide is deposited on stainless steel (SS) substrate by galvanostatic oxidation of Ru3+. At high current densities employed for this purpose, there is oxidation of water to oxygen, which occurs in parallel with Ru3+ oxidation. The oxygen evolution consumes a major portion of the charge. The oxygen evolution generates a high porosity to RuO2 films, which is evident from scanning electron microscopy studies. RuO2 is identified by X-ray photoelectron spectroscopy. Cyclic voltammetry and galvanostatic charge–discharge cycling studies indicate that RuO2/SS electrodes possess good capacitance properties. Specific capacitance of 276 F g−1 is obtained at current densities as high as 20 mA cm−2 (13.33 A g−1). Porous nature of RuO2 facilitates passing of high currents during charge–discharge cycling. RuO2/SS electrodes are thus useful for high power supercapacitor applications.

A one-step technique to prepare aligned arrays of carbon nanotubes

A simple effective pyrolysis technique has been developed to synthesize aligned arrays of multi-walled carbon nanotubes (MWCNTs) without using any carrier gas in a single-stage furnace at 700 °C. This technique eliminates nearly the entire complex and expensive machinery associated with other extensively used methods for preparation of CNTs such as chemical vapour deposition (CVD) and pyrolysis. Carbon source materials such as xylene, cyclohexane, camphor, hexane, toluene, pyridine and benzene have been pyrolyzed separately with the catalyst source material ferrocene to obtain aligned arrays of MWCNTs. The synthesized CNTs have been characterized by scanning electron microscopy (SEM), x-ray diffraction (XRD), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and Raman spectroscopy. In this technique, the need for the tedious and time-consuming preparation of metal catalysts and continuously fed carbon source material containing carrier gas can be avoided. This method is a single-step process where not many parameters are required to be monitored in order to prepare aligned MWCNTs. For the production of CNTs, the technique has great advantages such as low cost and easy operation.

Effect of increased manganese addition and mould type on the slurry erosion characteristics of Cr-Mn iron systems

The wear resistance of high chromium iron is well recorded. However, the same is not the case as regards the use of manganese at higher percentages in high chromium irons and its influence on wear behaviour. Hence, this work highlights the slurry wear characteristics of chromium 16–19%) iron following the introduction of manganese at two levels i.e. 5 and 10%. It is known that the wear properties are dictated by the microstructural features. To alter the structure, the cooling rate of casting has been varied by adopting two different types of moulds (i.e. sand and metal) and subsequently subjecting to thermal treatment. The as-cast and heat treated samples are examined for microstructure and then evaluated for hardness and slurry erosion properties. As the manganese content is increased from 5 to 10%, the hardness showed a decrease in value both in the as-cast and heat treated conditions. The slurry erosion loss, expectedly, showed an increase irrespective of the sample condition (i.e. mould type/heat treatment adopted). The findings are corroborated with the microstructural features obtained through optical and scanning electron microscopy.

Electrical Properties of Thermal Evaporated Cd1−xMnxS Nanocrystalline Films

Thin films of Cd1−xMnxS (0<=x<=0.5) were deposited on glass substrates by thermal evaporation. All the films were deposited at 300 K and annealed at 373, 473, and 573 K for 1 h in a high vacuum in the range 10−4 Pa. The as-deposited and the annealed films were characterized for composition, structure, and microstructure by using energy-dispersive X-ray, X-ray diffraction, scanning electron microscopy, and atomic force microscopy (AFM). The electrical properties were studied by Hall effect measurement. Electrical conductivity was studied in the temperature range 190–450 K. AFM studies showed that all the films were in nanocrystalline form with grain size varying in the range between 36 and 82 nm. Grain size studies showed a definite increase with annealing temperature. All the films exhibited wurtzite structure of the host material. The lattice parameter varied linearly with composition, following Vegard's law in the entire composition range. Grain size, electrical conductivity, Hall mobility, carrier concentration, and activation energy varied, exhibiting either maxima or minima at x=0.3.

Influence of magnetic clusters on electrical and magnetic properties of In1-xMnxSb/GaAs dilute magnetic semiconductor grown by liquid phase epitaxy

In1-xMnxSb films have been grown with different Mn doping concentrations (x = 0.0085, 0.018, 0.029 and 0.04) beyond the equilibrium 14 solubility limit by liquid phase epitaxy. We have studied temperature dependent resistivity, the Hall effect, magnetoresistance and magnetization for all compositions. Saturation in magnetization observed even at room temperature suggests the existence of ferromagnetic clusters in the film which has been verified by scanning electron microscopy studies. The anomalous Hall coefficient is found to be negative. Remnant field present on the surface of the clusters seems to affect the anomalous Hall effect at very low fields (below 350 Gauss). In the zero field resistivity, a variable-range hopping conduction mechanism dominates below 3.5 K for all samples above which activated behavior is predominant. The temperature dependence of the magnetization measurement shows a magnetic ordering below 10 K which is consistent with electrical measurements. (c) 2007 Elsevier Ltd. All rights reserved.

Enhanced adsorption capacity of activated alumina by impregnation with alum for removal of As(V) from water

Alum-impregnated activated alumina (AIAA) was investigated in the present work as an adsorbent for the removal of As(V) from water by batch mode. Adsorption study at different pH values shows that the efficiency of AIAA is much higher than as such activated alumina and is suitable for treatment of drinking water. The adsorption isotherm experiments indicated that the uptake of As(V) increased with increasing As(V) concentration from 1 to 25 mg/l and followed Langmuir-type adsorption isotherm. Speciation diagram shows that in the pH range of 2.8–11.5, arsenate predominantly exists as H2AsO4− and HAsO42− species and hence it is presumed that these are the major species being adsorbed on the surface of AIAA. Intraparticle diffusion and kinetic studies revealed that adsorption of As(V) was due to physical adsorption as well as through intraparticle diffusion. Effect of interfering ions revealed that As(V) sorption is strongly influenced by the presence of phosphate ion. The presence of arsenic on AIAA is depicted from zeta potential measurement, scanning electron microscopy (SEM) and energy-dispersive analysis of X-ray (EDAX) mapping study. Alum-impregnated activated alumina successfully removed As(V) to below 40 ppb (within the permissible limit set by WHO) from water, when the initial concentration of As(V) is 10 mg/l.

Generalized survival in step fluctuations

The properties of the generalized survival probability, that is, the probability of not crossing an arbitrary location R during relaxation, have been investigated experimentally (via scanning tunneling microscope observations) and numerically. The results confirm that the generalized survival probability decays exponentially with a time constant tau(s)(R). The distance dependence of the time constant is shown to be tau(s)(R)=tau(s0)exp[-R/w(T)], where w(2)(T) is the material-dependent mean-squared width of the step fluctuations. The result reveals the dependence on the physical parameters of the system inherent in the prior prediction of the time constant scaling with R/L-alpha, with L the system size and alpha the roughness exponent. The survival behavior is also analyzed using a contrasting concept, the generalized inside survival S-in(t,R), which involves fluctuations to an arbitrary location R further from the average. Numerical simulations of the inside survival probability also show an exponential time dependence, and the extracted time constant empirically shows (R/w)(lambda) behavior, with lambda varying over 0.6 to 0.8 as the sampling conditions are changed. The experimental data show similar behavior, and can be well fit with lambda=1.0 for T=300 K, and 0.5

Gelatin hydrogel electrolytes and their application to electrochemical supercapacitors

Gelatin hydrogel electrolytes (GHEs) with varying NaCl concentrations have been prepared by cross-linking an aqueous solution of gelatin with aqueous glutaraldehyde and characterized by scanning electron microscopy, differential scanning calorimetry, cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic chronopotentiometry. Glass transition temperatures for GHEs range between 339.6 and 376.9 K depending on the dopant concentration. Ionic conductivity behavior of GHEs was studied with varying concentrations of gelatin, glutaraldehyde, and NaCl, and found to vary between 10(-3) and 10(-1) S cm(-1). GHEs have a potential window of about 1 V. Undoped and 0.25 N NaCl-doped GHEs follow Arrhenius equations with activation energy values of 1.94 and 1.88 x 10(-4) eV, respectively. Electrochemical supercapacitors (ESs) employing these GHEs in conjunction with Black Pearl Carbon electrodes are assembled and studied. Optimal values for capacitance, phase angle, and relaxation time constant of 81 F g(-1), 75 degrees, and 0.03 s are obtained for 3 N NaCl-doped GHE, respectively. ES with pristine GHE exhibits a cycle life of 4.3 h vs 4.7 h for the ES with 3 N NaCl-doped GHE. (c) 2007 The Electrochemical Society.

Investigations on the influence of graphite filler on dry sliding wear and abrasive wear behaviour of carbon fabric reinforced epoxy composites

In this experimental study, the dry sliding wear and two-body abrasive wear behaviour of graphite filled carbon fabric reinforced epoxy composites were investigated. Carbon fabric reinforced epoxy composite was used as a reference material. Sliding wear experiments were conducted using a pin-on-disc wear tester under dry contact condition. Mass loss was determined as a function of sliding velocity for loads of 25, 50, 75, and 100 N at a constant sliding distance of 6000 m. Two-body abrasive wear experiments were performed under multi-pass condition using silicon carbide (SiC) of 150 and 320 grit abrasive papers. The effects of abrading distance and different loads have been studied. Abrasive wear volume and specific wear rate as a function of applied normal load and abrading distance were also determined. The results show that in dry sliding wear situations, for increased load and sliding velocity, higher wear loss was recorded. The excellent wear characteristics were obtained with carbon-epoxy containing graphite as filler. Especially, 10 wt.% of graphite in carbon-epoxy gave a low wear rate. A graphite surface film formed on the counterface was confirmed to be effective in improving the wear characteristics of graphite filled carbon-epoxy composites. In case of two-body abrasive wear, the wear volume increases with increasing load/abrading distance. Experimental results showed the type of counterface (hardened steel disc and SiC paper) material greatly influences the wear behaviour of the composites. Wear mechanisms of the composites were investigated using scanning electron microscopy. Wear of carbon-epoxy composite was found to be mainly due to a microcracking and fiber fracture mechanisms. It was found that the microcracking mechanism had been caused by progressive surface damage. Further, it was also noticed that carbon-epoxy composite wear is reduced to a greater extent by addition of the graphite filler, in which wear was dominated by microplowing/microcutting mechanisms instead of microcracking.

Phase diagram of the system Ca-Ti-O at 1200 K

Phase relations in the system Ca-Ti-O have been established by equilibration of several samples at 1200 K for prolonged periods and identification of phases in quenched samples by optical and scanning electron microscopy, XRD and EDS. Samples representing 20 compositions in the ternary system were analyzed. There was negligible solid solubility of Ca in the phases along the binary Ti-O, and of Ti in CaO. Four ternary oxides were identified: CaTiO3, Ca4Ti3O10 and Ca3Ti2O7 containing tetravalent titanium, and CaTi2O4 containing trivalent titanium. Tie-lines link calcium titanite (CaTi2O4) with the three calcium titanates (CaTiO3, Ca4Ti3O10 and Ca3Ti2O7), CaO, oxygen excess TiO1+delta and stoichiometric TiO. Tie-lines connect CaTiO3 with TiO2-x, Magneli phases TinO2n-1 (28 >= n >= 4), Ti3O5, Ti2O3 and TiO1+delta. CaO was found to coexist with TiO, and Ti-O solid solutions alpha and beta. The phase diagram is useful for understanding the mechanisms and kinetics of direct calciothermic reduction of TiO2 to metal and electrochemical reduction of TiO2 using graphite anode and molten CaCl2 electrolyte.