Studies on structural and electrical properties of sprayed SnO2 : Sb films

Thin films of antimony-doped tin oxide (SnO2:Sb) were prepared by spray pyrolysis using stannous chloride (SnCl2) and antimony trichloride (SbCl3) as precursors. The antimony doping was varied from 0 to 4 wt%. Scanning electron microscopy (SEM) revealed the surface morphology to be very smooth, yet grainy in nature. X-ray diffraction (XRD) shows films to have preferred orientation, which varies with the extent of antimony doping: undoped films prefer the (2 1 1) orientation, while the (3 0 1) orientation is preferred for doping levels of 0.5 and 1.0 wt%. For higher doping levels, the (2 0 0) orientation is preferred. This difference in preferred orientations is reflected in the SEM of the films. Atomic force microscopy (AFM) reveals that film roughness is not affected by antimony doping. The minimum sheet resistance (2.17 ohm/square) achieved in the present study is lower than values reported to date in SnO2:Sb films prepared from SnCl2 precursor. The Hall mobility of undoped SnO2 films was found to be 109.52 cm(2)/V s, which reduces to 2.55 cm(2)/ Vs for the films doped with 4 wt% of Sb. On the other hand, the carrier concentration, which is 1.23 x 10(19) cm(-3) in undoped films, increases to 2.89 x 10(21) cm(-3) for the films doped with 4 wt% of Sb. (c) 2004 Elsevier B.V. All rights reserved.

Photocatalytic degradation of dyes over combustion synthesized Ce1-xFexVO4

Fe-substituted CeVO4 was synthesized by the solution combustion technique and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, UV-vis spectroscopy, transmission electron microscopy and BET surface area analyzer. These compounds crystallized in tetragonal zircon structure with Fe substituted in ionic state for Ce3+ ions. The degradation of anionic and cationic dyes was studied over Fe-substituted CeVO4 compounds. The compounds showed high photocatalytic activity towards dye degradation. The effect of amount of substitution was studied by varying the Fe substitution from 1 to 10%. The rates decreased with increasing substitution of Fe in CeVO4 and 1% Fe substituted CeVO4 showed the highest photocatalytic activity. (C) 2010 Elsevier B.V. All rights reserved.

The significance of brittle reaction layers in fusing of dental ceramics to titanium

This thesis comprises four intercomplementary parts that introduce new approaches to brittle reaction layers and mechanical compatibility of metalloceramic joints created when fusing dental ceramics to titanium. Several different methods including atomic layer deposition (ALD), sessile drop contact angle measurements, scanning acoustic microscopy (SAM), three-point bending (TPB, DIN 13 927 / ISO 9693), cross-section microscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS) were employed. The first part investigates the effects of TiO2 layer structure and thickness on the joint strength of the titanium-metalloceramic system. Samples with all tested TiO2 thicknesses displayed good ceramics adhesion to Ti, and uniform TPB results. The fracture mode was independent of oxide layer thickness and structure. Cracking occurred deeper inside titanium, in the oxygen-rich Ti[O]x solid solution surface layer. During dental ceramics firing TiO2 layers dissociate and joints become brittle with increased dissolution of oxygen into metallic Ti and consequent reduction in the metal plasticity. To accomplish an ideal metalloceramic joint this needs to be resolved. The second part introduces photoinduced superhydrophilicity of TiO2. Test samples with ALD deposited anatase TiO2 films were produced. Samples were irradiated with UV light to induce superhydrophilicity of the surfaces through a cascade leading to increased amount of surface hydroxyl groups. Superhydrophilicity (contact angle ~0˚) was achieved within 2 minutes of UV radiation. Partial recovery of the contact angle was observed during the first 10 minutes after UV exposure. Total recovery was not observed within 24h storage. Photoinduced ultrahydrophilicity can be used to enhance wettability of titanium surfaces, an important factor in dental ceramics veneering processes. The third part addresses interlayers designed to restrain oxygen dissolution into Ti during dental ceramics fusing. The main requirements for an ideal interlayer material are proposed. Based on these criteria and systematic exclusion of possible interlayer materials silver (Ag) interlayers were chosen. TPB results were significantly better in when 5 μm Ag interlayers were used compared to only Al2O3-blasted samples. In samples with these Ag interlayers multiple cracks occurred inside dental ceramics, none inside Ti structure. Ag interlayers of 5 μm on Al2O3-blasted samples can be efficiently used to retard formation of the brittle oxygen-rich Ti[O]x layer, thus enhancing metalloceramic joint integrity. The most brittle component in metalloceramic joints with 5 μm Ag interlayers was bulk dental ceramics instead of Ti[O]x. The fourth part investigates the importance of mechanical interlocking. According to the results, the significance of mechanical interlocking achieved by conventional surface treatments can be questioned as long as the formation of the brittle layers (mainly oxygen-rich Ti[O]x) cannot be sufficiently controlled. In summary in contrast to former impressions of thick titanium oxide layers this thesis clearly demonstrates diffusion of oxygen from sintering atmosphere and SiO2 to Ti structures during dental ceramics firing and the following formation of brittle Ti[O]x solid solution as the most important factors predisposing joints between Ti and SiO2-based dental ceramics to low strength. This among other predisposing factors such as residual stresses created by the coefficient of thermal expansion mismatch between dental ceramics and Ti frameworks can be avoided with Ag interlayers.

Self-Assembly of Biopolymers on Colloidal Particles via Hydrogen Bonding

Fabrication of multilayer microcapsules via layer-by-layer approach through hydrogen bonding has attracted enormous interest due to its strong response to pH. In this communication, we have prepared hydrogen-bonded multilayer microcapsule without using any cross-linking agent by using DNA base pair (adenine and thymine) modified biocompatible polymers. The growth of the self-assembly on colloidal (melamine formaldehyde: MF) particles has been monitored with zeta potential measurement. The capsules were obtained on dissolution of MF particles at 0.1N HCl. The capsules were characterized with scanning electron microscopy. Moreover, we have observed the salt induced microscopic change in self-assembly of this system on the surface of colloidal particles.

Characterization of a continuous CO2 laser-welded Fe-Cu dissimilar couple

Continuous CO2 laser welding of an Fe-Cu dissimilar couple in a butt-weld geometry at different process conditions is studied. The process conditions are varied to identify and characterize the microstructural features that are independent of the welding mode. The study presents a characterization of the microstructure and mechanical properties of the welds. Detailed microstructural analysis of the weld/base-metal interface shows features that are different on the two sides of the weld. The iron side can grow into the weld with a local change in length scale, whereas the interface on the copper side indicates a barrier to growth. The interface is jagged, and a banded microstructure consisting of iron-rich layers could be observed next to the weld/Cu interface. The observations suggest that solidification initiates inside the melt, where iron and copper are mixed due to convective flow. The transmission electron microscopy (TEM) of the weld region also indicates the occasional presence of droplets of iron and copper. The microstructural observations are rationalized using arguments drawn from a thermodynamic analysis of the Fe-Cu system.

Morphogenesis of Mammalian Endoplasmic Reticulum and Golgi Apparatus throughout the Cell Cycle

The endoplasmic reticulum (ER) and the Golgi apparatus are organelles that produce, modify and transport proteins and lipids and regulate Ca2+ environment within cells. Structurally they are composed of sheets and tubules. Sheets may take various forms: intact, fenestrated, single or stacked. The ER, including the nuclear envelope, is a single continuous network, while the Golgi shows only some level of connectivity. It is often unclear, how different morphologies correspond to particular functions. Previous studies indicate that the structures of the ER and Golgi are dynamic and regulated by fusion and fission events, cytoskeleton, rate of protein synthesis and secretion, and specific structural proteins. For example, many structural proteins shaping tubular ER have been identified, but sheet formation is much more unclear. In this study, we used light and electron microscopy to study morphological changes of the ER and Golgi in mammalian cells. The proportion, type, location and dynamics of ER sheets and tubules were found to vary in a cell type or cell cycle stage dependent manner. During interphase, ER and Golgi structures were demonstrated to be regulated by p37, a cofactor of the fusion factor p97, and microtubules, which also affected the localization of the organelles. Like previously shown for the Golgi, the ER displayed a tendency for fenestration and tubulation during mitosis. However, this shape change did not result in ER fragmentation as happens to Golgi, but a continuous network was retained. The activity of p97/p37 was found to be important for the reassembly of both organelles after mitosis. In EM images, ER sheet membranes appear rough, since they contain attached ribosomes, whereas tubular membranes appear smooth. Our studies revealed that structural changes of the ER towards fenestrated and tubular direction correlate with loss of ER-bound ribosomes and vice versa. High and low curvature ER membranes have a low and high density of ribosomes, respectively. To conclude, both ER and Golgi architecture depend on fusion activity of p97/p37. ER morphogenesis, particularly of the sheet shape, is intimately linked to the density of membrane bound ribosomes.

Effect of fuel on the formation structure, transport and magnetic properties of LaMnO3+nanopowders

Single-step low-temperature solution combustion (LCS) synthesis was adopted for the preparation of LaMnO3+ (LM) nanopowders. The powders were well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS),surface area and Fourier transform infrared spectroscopy (FTIR). The PXRD of as-formed LM showed a cubic phase but, upon calcination (900degrees C, 6 h), it transformed into a rhombohedral phase. The effect of fuel on the formation of LM was examined, and its structure and magnetoresistance properties were investigated. Magnetoresistance (MR) measurements on LM were carried out at 0, 1, 4 and 7 T between 300 and 10 K. LM (fuel-to-oxidizer ratio; = 1) showed an MR of 17% at 1 T, whereas, for 4 and 7 T, it exhibited an MR of 45 and 55%, respectively, near the TM-I. Metallic resistivity data below TM-I showed that the double exchange interaction played a major role in this compound. It was interesting to observe that the sample calcined at 1200 degrees C for 3 h exhibited insulator behavior.

Dielectric properties of (100-x)Li2B4O7-x(Ba5Li2Ti2Nb8O30) glasses and glass nanocrystal composites

Transparent glasses of various compositions in the system (100 -x)(Li2B4O7)-x(Ba5Li2Ti2Nb8O30) (5 <= x <= 20, in molar ratio) were fabricated by splat quenching technique. The glassy nature of the as-quenched samples was established by differential thermal analyses (DTA). X-ray powder diffraction studies confirmed the as-quenched glasses to be amorphous and the heat-treated to be nanocrystalline. Controlled heat-treatment of the as-quenched glasses at 500 degrees C for 8 h yielded nanocrystallites embedded in the glass matrix. High Resolution Transmission Electron Microscopy (HRTEM) of these samples established the size of the crystallites to be in the nano-range and confirmed the phase to be that of Ba5Li2Ti2Nb8O30 (BLTN) which was, initially, identified by X-ray powder diffraction. The frequency, temperature and compositional dependence of the dielectric constant and the electrical conductivity of the glasses and glass nanocrystal composites were investigated in the 100 Hz to 10 MHz frequency range. Electrical relaxations were analyzed using the electric modulus formalisms. The imaginary part of electric modulus spectra was modeled using an approximate solution of Kohlrausch-Williams-Watts relation. The frequency dependent electrical conductivity was rationalized using Jonscher's power law. The activation energy associated with the dc conductivity was ascribed to the motion of Li+ ions in the glass matrix. The activation energy associated with dielectric relaxation was almost equal to that of the dc conductivity, indicating that the same species took part in both the processes. (C) 2010 Elsevier B.V. All rights reserved.

Reversible polyelectrolyte capsules as carriers for protein delivery

A reversible drug delivery system based on spontaneous deposition of a model protein into preformed microcapsules has been demonstrated for protein delivery applications. Layer-by-Layer assembly of poly(allylamine hydrochloride) (PAH) and poly(methacrylic acid) (PMA) onto polystyrene sulfonate (PSS) doped CaCO3 particles, followed by core removal yielded intact hollow microcapsules having a unique property to induce spontaneous deposition of bovine serum albumin (BSA) at pH below its isoelectric point of 4.8, where it was positively charged. These capsules showed reversible pH dependent open and closed states to fluorescence labeled dextran (FITC-Dextran) and BSA (FITC-BSA). The loading capacity of BSA increased from 9.1 x 10(7) to 2.03 x 10(8) molecules per capsule with decrease in pH from 4.5 to 3.The loading of BSA-FITC was observed by confocal laser scanning microscopy (CLSM), which showed homogeneous distribution of protein inside the capsule. Efficient loading of BSA was further confirmed by atomic force microscopy (AFM) and scanning electron microscopy (SEM).The interior capsule concentration was as high as 209 times the feeding concentration when the feeding concentration was increased from 1 to 10 mg/ml. The deposition was initially controlled by spontaneous loading mechanism at lower BSA concentration followed by diffusion controlled loading at higher concentration; which decreased the loading efficiency from 35% to 7%. Circular dichroism (CD) measurements and Fourier transform infrared spectroscopy (FTIR) confirmed that there was no significant change in conformation of released BSA in comparison with native BSA. The release was initially burst in the first 0.5 h and sustained up to 5 h. The hollow capsules were found to be biocompatible with mouse embryonic fibroblast (MEF) cells during in vitro cell culture studies. Thus these pH sensitive polyelectrolyte microcapsules may offer a promising delivery system for water soluble proteins and peptides. (C) 2010 Elsevier B.V. All rights reserved.

Glucose-Triggered Drug Delivery from Borate Mediated Layer-by-Layer Self-Assembly

In this study, we report a novel approach for glucose-triggered anticancer drug delivery from the self-assembly of neutral poly(vinyln alcohol) (PVA) and chitosan. In the present study, we have fabricated multilayer thin film of PVA-borate and chitosan on colloidal particle (MF particle) and monitored the layer-by-layer growth using Zetapotential measurements. Formation of multilayer membrane on MF particle has been further characterized with transmission electron microscopy (TEM) and confocal laser scanning microscopy (CLSM). Subsequently,disintegration of multilayer thin film and microcapsules was observed in presence of glucose. We investigated the disassembly of PVA-borate and chitosan self-assembly under CLSM and atomic force microscopy. These results suggest that this multilayer thin film is very efficient for encapsulation and release of DOX molecules above certain concentration of glucose (25 mM). This glucose-sensitive self-assembly is relevant for the application of anticancer therapeutic drug delivery.

Structural studies on members of the picornavirus superfamily

The pathogenic members of the picornavirus superfamily have adverse effects on humans, their crops and their livestock. As structure is related to function, detailed structural studies on these viruses are important not only for fundamental understanding of the viral life cycle, but also for the rational design of vaccines and inhibitors for disease control. These viruses have positive sense, single-stranded RNA genomes enclosed in a protein capsid. X-ray crystallography and cryo-electron microscopy studies have revealed that the isometric members of this group have icosahedrally-symmetric capsids made up of 60 copies of each of the structural proteins. The members that infect animal cells often employ one or more cellular receptors to facilitate cell entry which in some cases is known to initiate the uncoating sequence of the genome. The nature of the interactions between individual viruses and alternative cellular receptors has rarely been probed. The capsid assembly of the members of the picornavirus superfamily is considered to be cooperative and the interactions of RNA and capsid proteins are thought to play an important role in orchestrating virus assembly. The major aims of this thesis were to solve the structures of blackcurrant reversion virus (BRV), human parechovirus 1 (HPEV1) and coxsackievirus A7 (CAV7), as well as the structure of HPEV1 complexed with two of its cellular receptors using cryo-electron microscopy, three-dimensional image reconstruction and homology modeling. Each of the selected viruses represents a taxonomic group where little or no structural data was previously available. The results enabled the detailed comparison of the new structures to those of known picornaviruses, the identification of surface-exposed epitopes potentially important for host interaction, the mapping of RNA-capsid protein interactions and the elucidation of the basis for the specificity of two different receptor molecules for the same capsid. This work will form the basis for further studies on the influence of RNA on parechovirus assembly as a potential target for drug design.

Single-Shot Preparation of Crystalline Nanoplate LiFePO4 by a Simple Polyol Route

Nanoplate LiFePO4 is synthesized by a polyol route starting from only two reactants, namely, FePO4 and LiOH. The crystalline compound forms by refluxing a tetraethylene glycol solution consisting of FePO4 and LiOH at 335 degrees C without further heating of the reaction product.The nanoplates have average dimensions of 30 nm width and 160 nm length, as measured from transmission electron microscopy micrographs.The surface area of the LiFePO4 sample is 38 m(2) g(-1). Also, the sample is porous with a broadly distributed pore around 50 nm. The electrodes fabricated out of the nanoplate of LiFePO4 exhibit a high electrochemical activity. Discharge capacity values measured are 160 and 100 mAh g(-1) at 0.15C and 3.45C, respectively. A stable capacity of about 155 mAh g(-1) is measured at 0.2C over a 50 charge-discharge cycle. (C) 2010 The Electrochemical Society. [DOI: 10.1149/1.3425730] All rights reserved.

Charge transport properties of water dispersible multiwall carbon nanotube-polyaniline composites

The transmission electron microscopy images of in situ prepared multiwall carbon nanotubes (MWNTs)and polyaniline (PANI) composites show that nanotubes are well dispersed in aqueous medium, and the nanofibers of PANI facilitate intertube transport. Although low temperature transport indicates variable range hopping (VRH) mechanism, the dc and ac conductivity become temperature independent as the MWNT content increases. The onset frequency for the increase in conductivity is observed to be strongly dependent on the MWNT weight percent, and the ac conductivity can be scaled onto a master curve. The negative magnetoresistance is attributed to the forward interference scattering mechanism in VRH transport. (C) 2010 American.

Annealing response of the intermetallic alloy Ti-22Al-25Nb

A hot rolled two-phase Ti-22Al-25Nb (at.%) alloy containing the orthorhombic (O) and beta(B2) phases was subjected to thermal treatment under different conditions. The experiment was aimed to examine the recrystallization response of the beta(B2) phase (static and dynamic) to microstructure and crystallographic texture evolution using scanning electron microscopy coupled with electron backscattered diffraction (SEM-EBSD). Specimens rolled in the two-phase (O + beta(B2)) region consisted of highly deformed beta(B2) grains. The texture was close to that of the typical bcc deformation texture with a few additional texture components. A subsequent heat treatment of these rolled specimens in single beta(B2) phase region was characterized by static recrystallized beta(B2) grains with the final texture partly inherited from as-rolled material. In contrast, specimens rolled in the single beta(B2) region produced beta(B2) grains with the texture similar to that of completely dynamic recrystallized one. (C) 2010 Elsevier Ltd. All rights reserved.

Deformation and crystallization of Zr-based amorphous alloys in homogeneous flow regime

The purpose of this study is to experimentally investigate the interaction of inelastic deformation and microstructural changes of two Zr-based bulk metallic glasses (BMGs): Zr41.25Ti13.75Cu12.5Ni10Be22.5 (commercially designated as Vitreloy 1 or Vit1) and Zr46.75Ti8.25Cu7.5Ni10Be27.5 (Vitreloy 4, Vit4). High-temperature uniaxial compression tests were performed on the two Zr alloys at various strain rates, followed by structural characterization using differential scanning calorimetry (DSC) and transmission electron microscopy (TEM). Two distinct modes of mechanically induced atomic disordering in the two alloys were observed, with Vit1 featuring clear phase separation and crystallization after deformation as observed with TEM, while Vit4 showing only structural relaxation with no crystallization. The influence of the structural changes on the mechanical behaviors of the two materials was further investigated by jump-in-strain-rate tests, and flow softening was observed in Vit4. A free volume theory was applied to explain the deformation behaviors, and the activation volumes were calculated for both alloys.