pp 89-95 April 2010 Thin Films and Nanomatter
Large quantities of single-crystalline ZnO nanorods and nanotubes have been prepared by the microwave irradiation of a metalorganic complex of zinc, in the presence of a surfactant. The method is simple, fast, and inexpensive (as it uses a domestic microwave oven), and yields pure nanostructures of the hexagonal würtzite phase of ZnO in min, and requires no conventional templating. The ZnO nanotubes formed have a hollow core with inner diameter varying from 140–160 nm and a wall of thickness, 40–50 nm. The length of nanorods and nanotubes varies in the narrow range of 500–600 nm. These nanostructures have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The ZnO nanorods and nanotubes are found by SAED to be single-crystalline. The growth process of ZnO nanorods and nanotubes has been investigated by varying the surfactant concentration and microwave irradiation time. Based on the various results obtained, a tentative and plausible mechanism for the formation of ZnO nanostructures is proposed.
pp 97-102 April 2010 Thin Films and Nanomatter
A detailed chemisorption mechanism is proposed for the atomic layer deposition (ALD) of aluminium oxide nano layers using trimethyl aluminum (TMA) and water as precursors. Six possible chemisorption mechanisms, complete ligand exchange, partial ligand exchange, simple dissociation, complete dissociation via ligand exchange, complete dissociation and association, are proposed and related parameters like ligand to metal ratio (L/M), concentrations of metal atoms and methyl groups adsorbed are calculated and compared against reported values. The maximum number of methyl groups that can get attached on the surface is calculated in a different way which yields a more realistic value of 6.25 per nm2 substrate area. The dependence of the number of metal atoms adsorbed on OH concentration is explained clearly. It is proposed that a combination of complete ligand exchange and complete dissociation is the most probable chemisorption mechanism taking place at various OH concentrations.
pp 103-110 April 2010 Thin Films and Nanomatter
Chromium nitride (CrN) thin films were deposited on stainless steel (grade: SA304) substrate by using d.c. reactive magnetron sputtering and the influence of process parameters such as substrate temperature, pressure, and power on their microstructural characteristics were investigated in the present work. The CrN films were characterized with X-ray diffraction (XRD) to reveal the formation of different phases and its texture. The films showed the (111) preferred orientation but its intensity decreased, while intensity of peak (200) increased with increase in working pressure. The mixture of CrN and Cr2N phases were identified at low working pressure and temperature. The preferred orientations of CrN thin films are strongly influenced by sputtering conditions, thickness, and the induced residual stress in the films as observed in the present work. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used to characterize the morphology and surface topography of thin films, respectively. The study shows that the hardness of films strongly depends on the grain size and the film density, which are influenced by combined effect of the working pressure, temperature, and power of the sputtering process.
pp 111-117 April 2010 Thin Films and Nanomatter
Patterned thin films, ZnO, are successfully prepared on glass substrates by the sol–gel method using dip-coating technique. The films, formed of ZnO nanocrystallites with hexagonal crystal structure, are characterized by means of scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The as obtained ZnO films are studied with respect to photo-initiated bleaching of malachite green in aqueous solutions. The bleaching process is investigated at various initial concentrations of malachite green in the aqueous solutions by using ZnO films of different thicknesses. The obtained results are promising for the development of ZnO photocatalysts by the sol–gel method.
pp 119-122 April 2010 Thin Films and Nanomatter
Nb-doped ZnO films with (002) orientation have been grown on glass substrates by rf magnetron sputtering followed by vacuum annealing at 400°C for 3 h. The microstructures and surface figures of the Nbdoped ZnO films were investigated with X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. And its optical and electrical properties were measured at room temperature using a four-point probe technique and 756-type spectrophotometer, respectively. X-ray diffraction (XRD) revealed that the films are highly textured along the 𝑐 axis and perpendicular to the surface of the substrate. After annealing at 400°C for 180 min under vacuum, transmittance of about 90% in visible region for Nb doped ZnO films was confirmed by the optical transmission spectra, and the low resistivity of 5.47 × 10-3 𝛺.cm was obtained.
pp 123-127 April 2010 Thin Films and Nanomatter
According to the Mott and Nabarro’s model, the contribution to the critical shear stress of the material caused by the interaction between edge dislocations and nanoscale cylindrical inhomogeneities with interface stresses is obtained. The influence of the radius and the volume fraction of the inhomogeneity as well as the interface stresses on the critical shear stress is investigated. The important result is that, if the interface stress is considered, a maximum of the contribution to the critical shear stress produced by this interaction may be obtained when the radius of the inhomogeneity reaches a critical value.
pp 129-134 April 2010 Ceramics and Glasses
Polycrystalline sample of Ba3Sr2DyTi3V7O30 was prepared at 950°C using a high-temperature solid-state reaction technique. X-ray structural analysis indicated the formation of a single-phase orthorhombic structure with lattice parameters: 𝑎 = 12.2719 (39) Å, 𝑏 = 8.9715(39) Å and 𝑐 = 19.7812(39) Å. Microstructural study showed densely packed uniform distribution of grains over the surface of the sample. The a.c. impedance plots were used as tools to analyse the electrical response of the sample as a function of frequency at different temperatures (30–500°C). These plots revealed the presence of grain boundary effect, from 200°C onwards. Complex impedance analysis showed non-Debye type of dielectric relaxation. The Nyquist plots showed the negative temperature coefficient of resistance character of Ba3Sr2DyTi3V7O30. A hopping mechanism of electrical transport processes in the system is evident from the modulus analysis. The activation energy of the compound (calculated both from loss and modulus spectrum) is the same, and hence the relaxation process may be attributed to the same type of charge carrier.
pp 135-144 April 2010 Ceramics and Glasses
Zircon (zirconium silicate, ZrSiO4) is the main opacifier of glossy, opaque, white-coloured, fritbased wall tile glazes. However, zirconia containing frits employed in the preparation of these glazes raise the production cost limiting zircon usage as a raw material at an industrial scale. Therefore, there have been several searches on seeking for alternative frit compositions with lower or without zirconia content. Consequently, positive outcomes were recently reported. With the present study, 1.5–5% of borax concentrator waste replaced certain level of acid boric for B2O3 content in a low zircon containing frit recipe. It is confirmed that waste contribution did not distort the surface properties of the fast single-fired wall tile opaque glazes. Zircon was found to be the main crystal phase of the glazes in laboratory trials. Industrial applications revealed that shorter firing cycles lead to zircon and petedunnite (CaZnSi2O6) formation in the CW-4 glaze.
pp 145-148 April 2010 Ceramics and Glasses
The infrared spectra (IR) of various glass compositions in the glass system, [(Pb𝑥Sr1–𝑥)O.TiO2]– [2SiO2.B2O3]–[BaO.K2O]–[La2O3], were recorded over a continuous spectral range (400–4000 cm-1) to study their structure systematically. IR spectrum of each glass composition shows a number of absorption bands. These bands are strongly influenced by the increasing substitution of SrO for PbO. Various bands shift with composition. Absorption peaks occur due to the vibrational mode of the borate network in these glasses. The vibrational modes of the borate network are seen to be mainly due to the asymmetric stretching relaxation of the B–O bond of trigonal BO3 units. More splitting is observed in strontium-rich composition.
pp 149-155 April 2010 Polymers
A matrix composed of polyvinyl-alcohol (PVA) mixed with different concentration ratios of the granular strontium chloride (SrCl2.6H2O) were prepared by casting technique method at room temperature (about 30°C). The electric and dielectric properties such as a.c. electrical conductivity by a conventional method, using Keithly 616 digital electrometer, dielectric constant, and dielectric loss were measured. Calculated equilibrium properties such as lattice constant, bulk modulus and elastic constants are in good agreement with experimental results. The calculated activation energy values agree well with experiment only when the SrCO2 molecules are allowed to displace under strain, indicating the importance of inner strain relaxation. From the elastic constants, theoretical values of the Young’s modulus, shear modulus, Poisson’s ratio, of SrCl2 are obtained. In addition mechanical properties such as Young’s modulus, creep relaxation, and energy stored properties for these samples were also determined at room temperature.
pp 157-163 April 2010 Polymers
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 Nafion 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 Nafion content as low as 5 wt.% in the catalyst layer. Accordingly, the present study provides a novel alternative support for platinized PEFC electrodes.
pp 165-168 April 2010 Polymers
Materials with small particle size are being extensively used in composites and hybrid materials. Exfoliated clay–polymer hybrids show enhanced properties. Exfoliation of clay platelets can be affected by selecting dispersing agents. In the present work, clay dispersed by natural dispersant (soap stone powder), cetyl trimethyl ammonium bromide (CTAB) dispersed clay and acid clay (amorphous clay) are taken. They are then polymerized with poly methyl methacrylate (PMMA) by solution intercalation method. The thermal stability of these different clay–PMMA hybrids have been studied and compared with that of pure PMMA by differential scanning calorimeter (DSC). The bonding of clay with PMMA has been studied by IR. Morphology of clay–PMMA hybrids has been shown by SEM and XRD which indicate partially exfoliated structure in T606-4 and intercalated structures in T606-6 and T606-2.
pp 169-178 April 2010 Magnetic Properties
Charge-order driven magnetic ferroelectricity is shown to occur in several rare earth manganates of the general formula, Ln1–𝑥A𝑥MnO3 (Ln = rare earth, A = alkaline earth). Charge-ordered manganates exhibit dielectric constant anomalies around the charge-ordering or the antiferromagnetic transition temperature. Magnetic fields have a marked effect on the dielectric properties of these compounds, indicating the presence of coupling between the magnetic and electrical order parameters. Magneto-dielectric properties are retained in small particles of the manganates. The observation of magneto-ferroelectricity in these manganates is in accordance with theoretical predictions.
pp 179-183 April 2010 Alloys
The effect of H+ ion implantation on surface morphology of the titanium alloy, Ti–6Al–4V, was studied, following H+ ion implantation of 150 keV and 250 keV energy to fluence of 2.6 × 1018 cm-2 and 2.5 × 1019 cm-2, respectively at ambient temperature. No detectable change was observed in surface features of either of the above specimen immediately after the implantation. However, vein like features (VLF) were observed to appear on the surface of the sample, implanted at 150 keV to a fluence of 2.6 × 1018 cm-2, following natural ageing at room temperature for 150 days. Subsequent annealing of the above naturally aged sample, at 423 K for 150 min under vacuum (10-3 torr), led to development of a macroblister.
In sharp contrast in the other sample, implanted by H+ ions of higher energy (250 keV) to higher fluence of 2.5 × 1019 cm-2, neither there was any effect of natural ageing following the implantation nor that of subsequent annealing at 423 K and ageing on its surface morphology.
pp 185-190 April 2010 Fly Ash
In the present work the reaction between fly ash and lime in fly ash–lime compacts under water curing and steam curing conditions was studied thoroughly in relation to the processing conditions. Fly ash from different sources were collected, characterized, mixed with lime in different ratios and compacted. The compacts were cured with water and steam separately. The reduction in the free CaO content in these compacts was measured as a function of curing time and curing process. Role of two ionic additives, FeCl3 and MgCl2, on the reaction between fly ash and lime was also investigated by measuring the free CaO content. Kinetics of these reactions was studied by determining the reaction order and rate constants with respect to the free CaO content and it was observed that the curing conditions and additives affected the reaction kinetics significantly.
Volume 43, 2020
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