Phase composition of the rapidly quenched melt of YBa2Cu3O7-y+20 mol% Y2BaCuO5

Samples of YBa2Cu3O7-y+20 mol% Y2BaCuO5, with thicknesses ranging between 50-250 μm, have been melt processed and rapidly quenched from temperatures between 985 and 1100°C by immersing them in liquid nitrogen. The phase composition and microstructures of these samples have been characterised using a combination of X-ray diffractometry, optical microscopy and scanning electron microscopy with energy dispersive X-ray spectroscopy. The quenched melt of samples quenched from temperatures greater than 985°C appears relatively homogeneous but consists of Ba2Cu3Ox (BC1.5) and BaCu2O2 (BC2) regions. At about 985°C, BaCuO2 (BC1) crystallises from the melt and most of the BC1.5 decomposes into BC1 and CuO or into BC1 and BC2. The crystallisation of BC1 induces segregation of elements in the melt and this is very significant for the melt texturing of YBCO.

Gas sensing of ruthenium implanted tungsten oxide thin films

Different amounts of Ru were implanted into thermally evaporated WO3 thin films by ion implantation. The films were subsequently annealed at 600oC for 2 hours in air to remove defects generated during the ion implantation. The Ru concentrations of four samples have been quantified by Rutherford Backscattering Spectrometry as 0.8, 5.5, 9 and 11.5 at%. The un-implanted WO3 films were highly porous but the porosity decreased significantly after ion implantation as observed by Transmission Electron Microscopy and Scanning Electron Microscopy. The thickness of the films also decreased with increasing Ru-ion dose, which is mainly due to densification of the porous films during ion implantation. From Raman spectroscopy two peaks at 408 and 451 cm-1 (in addition to the typical vibrational peaks of the monoclinic WO3 phase) associated with Ru were observed. Their intensity increased with increasing Ru concentration. X-Ray Photoelectron Spectroscopy showed a metallic state of Ru with binding energy of Ru 3d5/2 at 280.1 eV. This peak position remained almost unchanged with increasing Ru concentration. The resistances of the Ru-implanted films were found to increase in the presence of NO2 and NO with higher sensor response to NO2. The effect of Ru concentration on the sensing performance of the films was not explicitly observed due to reduced film thickness and porosity with increasing Ru concentration. However, the results indicate that the implantation of Ru into WO3 films with sufficient film porosity and film thickness can be beneficial for NO2 sensing at temperatures in the range of 250°C to 350°C.

Monoclinic β-MoO3 nanosheets produced by atmospheric microplasma : application to lithium-ion batteries

Porous high surface area thin films of nanosheet-shaped monoclinic MoO 3 were deposited onto platinized Si substrates using patch antenna-based atmospheric microplasma processing. The films were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) and electrochemical analysis. The electrochemical analysis shows original redox peaks and high charge capacity, and also indicates a reversible electrochemical behaviour particularly beneficial for applications in Li-ion batteries. SEM shows that the films are highly porous and consist of nanosheets 50-100 nm thick with surface dimensions in the micrometre range. HRTEM reveals that the MoO3 nanosheets consist of the monoclinic beta phase of MoO3. These intricate nanoarchitectures made of monoclinic MoO3 nanosheets have not been studied previously in the context of applications in Li-ion batteries and show superior structural and morphological features that enable effective insertion of Li ions.

Reduced graphene oxide growth on 316L stainless steel for medical applications

We report a new method for the growth of reduced graphene oxide (rGO) on the 316L alloy of stainless steel (SS) and its relevance for biomedical applications. We demonstrate that electrochemical etching increases the concentration of metallic species on the surface and enables the growth of rGO. This result is supported through a combination of Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), density functional theory (DFT) calculations and static water contact angle measurements. Raman spectroscopy identifies the G and D bands for oxidized species of graphene at 1595 cm(-1) and 1350 cm(-1), respectively, and gives an ID/IG ratio of 1.2, indicating a moderate degree of oxidation. XPS shows -OH and -COOH groups in the rGO stoichiometry and static contact angle measurements confirm the wettability of rGO. SEM and AFM measurements were performed on different substrates before and after coronene treatment to confirm rGO growth. Cell viability studies reveal that these rGO coatings do not have toxic effects on mammalian cells, making this material suitable for biomedical and biotechnological applications.

Choice of the End Functional Groups in Tri(p-phenylenevinylene) Derivatives Controls Its Physical Gelation Abilities

New supramolecular organogels based on all-trans-tri(p-phenylenevinylene) (TPV) systems possessing different terminal groups, e.g., oxime, hydrazone, phenylhydrazone, and semicarbazone have been synthesized. The self-assembly properties of the compounds that gelate in specific organic solvents and the aggregation motifs of these molecules in the organogels were investigated using UV−vis, fluorescence, FT-IR, and 1H NMR spectroscopy, electron microscopy, differential scanning calorimetry (DSC), and rheology. The temperature variable UV−vis and fluorescence spectroscopy in different solvents clearly show the aggregation pattern of the self-assemblies promoted by hydrogen bonding, aromatic π-stacking, and van der Waals interactions among the individual TPV units. Gelation could be controlled by variation in the number of hydrogen-bonding donors and acceptors in the terminal functional groups of this class of gelators. Also wherever gelation is observed, the individual fibers in gels change to other types of networks in their aggregates depending on the number of hydrogen-bonding sites in the terminal functions. Comparison of the thermal stability of the gels obtained from DSC data of different gelators demonstrates higher phase transition temperature and enthalpy for the hydrazone-based gelator. Rheological studies indicate that the presence of more hydrogen-bonding donors in the periphery of the gelator molecules makes the gel more viscoelastic solidlike. However, in the presence of more numbers of hydrogen-bonding donor/acceptors at the periphery of TPVs such as with semicarbazone a precipitation as opposed to gelation was observed. Clearly, the choice of the end functional groups and the number of hydrogen-bonding groups in the TPV backbone holds the key and modulates the effective length of the chromophore, resulting in interesting optical properties.

Characterization of Nanomaterials by Physical Methods

Much progress in nanoscience and nanotechnology has been made in the past few years thanks to the increased availability of sophisticated physical methods to characterize nanomaterials. These techniques include electron microscopy and scanning probe microscopies, in addition to standard techniques such as X-ray and neutron diffraction, X-ray scattering, and various spectroscopies. Characterization of nanomaterials includes the determination not only of size and shape, but also of the atomic and electronic structures and other important properties. In this article we describe some of the important methods employed for characterization of nanostructures, describing a few case studies for illustrative purposes. These case studies include characterizations of Au, ReO3, and GaN nanocrystals; ZnO, Ni, and Co nanowires; inorganic and carbon nanotubes; and two-dimensional graphene.

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.

Effect of mode of rolling on development of texture and microstructure in two-phase (alpha plus beta) brass

The evolution of microstructure and texture during deformation of two-phase (alpha + beta) brass was studied for different initial microstructure and texture. The deformation processing involved unidirectional and multi-step cross-rolling. The bulk textures were determined by measuring the pole figures and calculating the orientation distribution function ODF for both alpha (fcc) and beta (bcc) phases, while the microstructure and other microstructural parameters were measured through optical microscopy and scanning electron microscopy with electron back scatter diffraction (SEM-EBSD). Results indicate that textures developed after unidirectional rolling and multi-step cross-rolling are significantly different. The variation in initial texture had a pronounced effect on the development of texture in the alpha phase during subsequent deformation. (C) 2010 Elsevier B.V. All rights reserved.

Microwave Assisted Synthesis of Nanostructured Titanium Dioxide with High Photocatalytic Activity

TiO2 (anatase) was synthesized using a microwave-irradiation-assisted chemical method. The reaction conditions were varied to obtain unique nanostructures of TiO2 comprising nanometric spheres giving the materials a very porous morphology. The oxide was characterized by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric analysis (TGA). The specific surface area and porosity were quantified by the BET method, and the degradation of dyes was carried out using these materials. The photocatalytic activity of the nanometric TiO2 was significantly higher than that of commercially available TiO2 (Degussa P25) for the degradation of the dyes.

Optimization of off-oriented Ge substrates for MOVPE-grown GaAs solar cells

GaAs/Ge heterostructures having abrupt interfaces were grown on 2degrees, 6degrees, and 9degrees off-cut Ge substrates and investigated by cross-sectional high-resolution transmission electron microscopy (HRTEM), scanning electron microscopy, photoluminescence spectroscopy and electrochemical capacitance voltage (ECV) profiler. The GaAs films were grown on off-oriented Ge substrates with growth temperature in the range of 600-700degreesC, growth rate of 3-12 mum/hr and a V/III ratio of 29-88. The lattice indexing of HRTEM exhibits an excellent lattice line matching between GaAs and Ge substrate. The PL spectra from GaAs layer on 6degrees off-cut Ge substrate shows the higher excitonic peak compared with 2degrees and 9degrees off-cut Ge substrates. In addition, the luminescence intensity from the GaAs solar cell grown on 6degrees off-cut is higher than on 9degrees off-cut Ge substrates and signifies the potential use of 6degrees off-cut Ge substrate in the GaAs solar cells industry. The ECV profiling shows an abrupt film/substrate interface as well as between various layers of the solar cell structures.

Effect of calcium stoichiometry on the dielectric response of CaCu3Ti4O12 ceramics

CaxCu3Ti4O12 (x=0.90, 0.97, 1.0, 1.1 and 1.15) polycrystalline powders with variation in calcium content were prepared via the oxalate precursor route. The structural, morphological and dielectric properties of the ceramics fabricated using these powders were studied using X-ray diffraction, scanning electron microscope along with energy dispersive X-ray analysis, transmission electron microscopy, electron spin resonance (ESR) spectroscopy and impedance analyzer. The X-ray diffraction patterns obtained for the x = 0.97, 1.0 and 1.1 powdered ceramics could be indexed to a body-centered cubic perovskite related structure associated with the space group Im3. The ESR studies confirmed the absence of oxygen vacancies in the ceramics that were prepared using the oxalate precursor route. The dielectric properties of these suggest that the calcium deficient sample (x = 0.97) has a reduced dielectric loss while retaining the high dielectric constant which is of significant industrial relevance. (C) 2012 Elsevier Ltd. All rights reserved.

Texture and Microstructural Evolution in Pearlitic Steel During Triaxial Compression

This article presents the deformation behavior of high-strength pearlitic steel deformed by triaxial compression to achieve ultra-fine ferrite grain size with fragmented cementite. The consequent evolution of microstructure and texture has been studied using scanning electron microscopy, electron back-scatter diffraction, and X-ray diffraction. The synergistic effect of diffusion and deformation leads to the uniform dissolution of cementite at higher temperature. At lower temperature, significant grain refinement of ferrite phase occurs by deformation and exhibits a characteristic deformation texture. In contrast, the high-temperature deformed sample shows a weaker texture with cube component for the ferrite phase, indicating the occurrence of recrystallization. The different mechanisms responsible for the refinement of ferrite as well as the fragmentation of cementite and their interaction with each other have been analyzed. Viscoplastic self-consistent simulation was employed to understand deformation texture in the ferrite phase during triaxial compression.

Texture and microstructure evolution during cold rolling of Cu-Fe laminates prepared by accumulative roll bonding

Multi-layered materials have been made from Cu-Fe with approximately equal volume fractions using the Accumulated Roll Bonding (ARB) technique with less than 1 μm thickness of the individual layers. The so-obtained multi-layers have been subjected to deformation by cold rolling to 25, 50, 75, 87 and 93% reduction in thickness. A detailed characterization has been carried out using X-ray diffraction (line profile analysis and texture measurement) and electron (scanning and transmission) microscopy. It has been found that Fe layers are disintegrated whereas Cu retains its continuity within a layer. Microstructural Characterization from X-Ray Line profile Analysis (XRDLPA) through Variance Method reveals that large amount of strain is initially carried by Cu layers during deformation. In the Cu-Fe layer, the texture is comparatively weaker in Cu layer and strong in Fe layers. Brass Component increases up to 75% reduction and then decreases, while the ratio of Cu/S and Bs/S remains almost constant through out the deformation. After 50% reduction, dynamic recovery is predominant as indicated by the increase in the amount of low angle grain boundaries and decrease in dislocation density. The presence of R component indicates continuous dynamic recovery and recrystallization (CDRR) at the advanced stage of deformation.

Characterization and microhardness of Co-W coatings electrodeposited at different pH using gluconate bath: a comparative study

Electrodeposition of Co-W alloy coatings has been carried out with DC and PC using gluconate bath at different pH. These coatings are characterized for their structure, morphology and chemical composition by X-ray diffraction, field emission scanning electron microscopy, differential scanning calorimetry and X-ray photoelectron spectroscopy (XPS). Alloy coatings plated at pH8 are crystalline, whereas coatings electrodeposited at pH5 are nanocrystalline in nature. XPS studies have demonstrated that as-deposited alloy plated at pH8 with DC contain only Co2+ and W6+ species, whereas that alloy plated at pH5 has significant amount of Co-0 and W-0 along with Co2+ and W6+ species. Again, Co2+ and W6+ are main species in all as-deposited PC plated alloys in both pH. Co-0 concentration increases upon successive sputtering of all alloy coatings. In contrast, mainly W6+ species is detected in the following layers of all alloys plated with PC. Alloys plated at pH5 show higher microhardness compared to their pH8 counterparts.

Organogels from Dimeric Bile Acid Esters: In Situ Formation of Gold Nanoparticles

A new class of steroid dimers (bile acid derivatives) linked through ester functionalities were synthesized, which gelled various aromatic solvents. The organogels formed by the three dimeric ester molecules showed birefringent textures and fibrous nature by polarizing optical microscopy and scanning electron microscopy, respectively. A detailed rheological study was performed to estimate the mechanical strengths of two sets of organogels. In these systems, the storage modulus varied in the range of 0.8-3.5 X 10(4) at 1% w/v of the organogelators. The exponents of scaling of the storage modulus and yield stress of the two systems agreed well with those expected for viscoelastic soft colloidal gels with fibrillar flocs. The nanofibers in the organogel were utilized to engineer gold nanoparticles of different sizes and shapes and generate new gel-nanoparticle hybrid materials.