161 resultados para ELECTRON MICROSCOPY


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The ultramicrostructure of phases with n = 1, 2 and 3 in the hypothetical series Bi2WnO3n+3 has been investigated by high resolution electron microscopy and energy dispersive X-ray emission spectroscopy. For n = 1 and 2, well ordered phases with the predicted compositions have been obtained, but for n = 3, a severely disordered assemblage containing intergrowths of the two known structures and strips of the n = 3 member is produced. No evidence for ordered structures with n > 2 has yet been obtained.

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The thermal decomposition characteristics of rice husk have been investigated by dynamic thermoanalytical techniques: DTA, TG, DTG and isothermal heating. The observed thermal behaviour is explained on the basis of a superposition of the decomposition of cellulose and lignin, which are the major organic constituents of rice husk. Morphological features of silica in husk as well as the ash are examined by scanning electron microscopy. Silica in the residual ash has been characterised by X-ray diffraction and infrared spectroscopy. Controlled thermal decomposition of rice husk has been shown to be a convenient method for the liberation of silica.

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Surface activity of solution deposited (SD) amorphous films of As2S3 has been investigated. Silver and copper are readily deposited on such films from appropriate aqueous ionic solutions. The metals diffuse into the films upon irradiation with energetic photons. Structure and properties of SD films have been investigated using electron microscopy, optical spectroscopy and differential scanning calorimetry. The amorphous films tend to crystallize upon metal diffusion. The stability of amorphous films, the deposition of metals on their active surfaces and the photo-induced diffusion may all be attributed to the presence or production of charged defects in amorphous chalcogenide films.

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The ultramicrostructure of phases with n = 1, 2 and 3 in the hypothetical series Bi2WnO3n+3 has been investigated by high resolution electron microscopy and energy dispersive X-ray emission spectroscopy. For n = 1 and 2, well ordered phases with the predicted compositions have been obtained, but for n = 3, a severely disordered assemblage containing intergrowths of the two known structures and strips of the n = 3 member is produced. No evidence for ordered structures with n > 2 has yet been obtained.

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The present study is to investigate the interaction of strong shock heated oxygen on the surface of SiO2 thin film. The thermally excited oxygen undergoes a three-body recombination reaction on the surface of silicon dioxide film. The different oxidation states of silicon species on the surface of the shock-exposed SiO2 film are discussed based on X-ray Photoelectron Spectroscopy (XPS) results. The surface morphology of the shock wave induced damage at the cross section of SiO2 film and structure modification of these materials are analyzed using scanning electron microscopy and ion microscopy. Whether the surface reaction of oxygen on SiO2 film is catalytic or non-catalytic is discussed in this paper.

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The integration of hydrophobic and hydrophilic drugs in the polymer microcapsule offers the possibility of developing a new drug delivery system that combines the best features of these two distinct classes of material. Recently, we have reported the encapsulation of an uncharged water-insoluble drug in the polymer membrane. The hydrophobic drug is deposited using a layer-by-layer (LbL) technique, which is based on the sequential adsorption of oppositely charged polyelectrolytes onto a charged substrate. In this paper, we report the encapsulation of two different drugs, which are invariably different in structure and in their solubility in water. We have characterized these dual drug vehicular capsules by confocal laser scanning microscopy, atomic force microscopy, visible microscopy, and transmission electron microscopy. The growth of a thin film on a flat substrate by LbL was monitored by UV−vis spectra. The desorption kinetics of two drugs from the thin film was modeled by a second-order rate model.

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We incorporate various gold nanoparticles (AuNPs) capped with different ligands in two-dimensional films and three-dimensional aggregates derived from N-stearoyl-L-alanine and N-lauroyl-L-alanine, respectively. The assemblies of N-stearoyl-L-alanine afforded stable films at the air-water interface. More compact assemblies were formed upon incorporation of AuNPs in the air-water interface of N-stearoyl-L-alanine. We then examined the effects of incorporation of various AuNPs functionalized with different capping ligands in three-dimensional assemblies of N-lauroyl-L-alanine, a compound that formed a gel in hydrocarbons. The profound influence of nanoparticle incorporation into physical gels was evident from evaluation of various microscopic and bulk properties. The interaction of AuNPs with the gelator assembly was found to depend critically on the capping ligands protecting the Au surface of the gold nanoparticles. Transmission electron microscopy (TEM) showed a long-range directional assembly of certain AuNPs along the gel fibers. Scanning electron microscopy (SEM) images of the freeze-dried gels and nanocomposites indicate that the morphological transformation in the composite microstructures depends significantly on the capping agent of the nanoparticles. Differential scanning calorimetry (DSC) showed that gel formation from sol occurred at a lower temperature upon incorporation of AuNPs having capping ligands that were able to align and noncovalently interact with the gel fibers. Rheological studies indicate that the gel-nanoparticle composites exhibit significantly greater viscoelasticity compared to the native gel alone when the capping ligands are able to interact through interdigitation into the gelator assembly. Thus, it was possible to define a clear relationship between the materials and the molecular-level properties by means of manipulation of the information inscribed on the NP surface.

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Cobalt doped zinc oxide nanoparticles were prepared through simple wet chemical method. X-ray diffraction studies confirm the prepared particles are in wurtzite structure. Scanning Electron Microscopy studies show the shape and morphology of the particles. To identify the presence of cobalt in ZnO, Energy Dispersive X-ray analysis was done. Optical absorption measurements show the presence of exciton peak at 375 nm. Photoluminescence studies were done with the excitation wavelength of 330 nm, which shows the emission because of exciton recombination and oxygen vacancy.

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Poly(vinyl alcohol)-matrix reinforced with nanodiamond (ND) particles, with ND content up to 0.6 wt%, were synthesized. Characterization of the composites by transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS) reveal uniform distribution of the ND particles with no agglomeration in the matrix. Differential scanning calorimetry reveals that the crystallinity of the polymer increases with increasing ND content, indicating a strong interaction between ND and PVA. Nano-indentation technique was employed to assess the mechanical properties of composites. Results show that even small additions of ND lead to significant enhancement in the hardness and elastic modulus of PVA. Possible micromechanisms responsible for the enhancement of the mechanical properties are discussed.

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The wurtzite phase of ZnS nanocrystal has been prepared by annealing in 200-600 degrees C temperature range, its cubic phase of 2-3 nm size. prepared through soft chemical method. Results of isochronal experiments of 2 h at different temperatures indicate that visible transformation to wurtzite from cubic ZnS appears at a temperature of 400 degrees C, which is about three times smaller than that of bulk ZnS phase transition temperature. The phases, nanostructures, and optical absorption characteristics are obtained through X-ray diffraction. transmission electron microscopy, and UV-visible absorption spectroscopy. A stable and green photoluminescence emission peaked at 518 nm is observed from the 600 degrees C annealed samples, under ultraviolet light excitation.

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We report the formation of dynamic, reversible cross-linked dendritic megamers and their dissociation to monomeric dendrimers, through a thiol-disulfide interchange reaction. For this study, poly(alkyl aryl ether) dendrimers up to three-generations presenting thiol functionalities, were prepared. The series from zero to three generations of dendrimers were installed with 3, 6, 12, and 24 thiol functionalities at their peripheries. Upon synthesis, cross-linking of the dendrimer was accomplished through disulfide bond formation. The cross-linking of dendrimers was monitored through optical density changes at 420 nm. Dense cross-linking led to visible precipitation of dendritic megamers and the morphologies of the megamers were characterized by transmission electron microscopy. The disulfide cross-links between megamer monomers could be dissociated readily upon reduction of disulfide bond by dithiothreitol reagent. Preliminary studies show that dendritic megamers encapsulate C-60 and the efficiency of encapsulation increased with increasing generation of dendritic megamer.

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Carbon-supported Pt-TiO2 (Pt-TiO2/C) catalysts with varying at. wt ratios of Pt to Ti, namely, 1:1, 2:1, and 3:1, are prepared by the sol-gel method. The electrocatalytic activity of the catalysts toward oxygen reduction reaction (ORR), both in the presence and absence of methanol, is evaluated for application in direct methanol fuel cells (DMFCs). The optimum at. wt ratio of Pt to Ti in Pt-TiO2/C is established by fuel cell polarization, linear sweep voltammetry, and cyclic voltammetry studies. Pt-TiO2/C heattreated at 750 degrees C with Pt and Ti in an at. wt ratio of 2:1 shows enhanced methanol tolerance, while maintaining high catalytic activity toward ORR. The DMFC with a Pt-TiO2/C cathode catalyst exhibits an enhanced peak power density of 180 mW/cm(2) in contrast to the 80 mW/cm(2) achieved from the DMFC with carbon-supported Pt catalyst while operating under identical conditions. Complementary data on the influence of TiO2 on the crystallinity of Pt, surface morphology, and particle size, surface oxidation states of individual constituents, and bulk and surface compositions are also obtained by powder X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, energy dispersive analysis by X-ray, and inductively coupled plasm optical emission spectrometry.

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The coat protein gene of physalis mottle tymovirus (PhMV) was over expressed in Escherichia coli using pET-3d vector. The recombinant protein was found to self assemble into capsids in vivo. The purified recombinant capsids had an apparent s value of 56.5 S and a diameter of 29(±2) nm. In order to establish the role of amino and carboxy-terminal regions in capsid assembly, two amino-terminal deletions clones lacking the first 11 and 26 amino acid residues and two carboxy-terminal deletions lacking the last five and ten amino acid residues were constructed and overexpressed. The proteins lacking N-terminal 11 (PhCPN1) and 26 (PhCPN2) amino acid residues self assembled into T = 3 capsids in vivo, as evident from electron microscopy, ultracentrifugation and agarose gel electrophoresis. The recombinant, PhCPN1 and PhCPN2 capsids were as stable as the empty capsids formed in vivo and encapsidated a small amount of mRNA. The monoclonal antibody PA3B2, which recognizes the epitope within region 22 to 36, failed to react with PhCPN2 capsids while it recognized the recombinant and PhCPN1 capsids. Disassembly of the capsids upon treatment with urea showed that PhCPN2 capsids were most stable. These results demonstrate that the N-terminal 26 amino acid residues are not essential for T = 3 capsid assembly in PhMV. In contrast, both the proteins lacking the C-terminal five and ten amino acid residues were present only in the insoluble fraction and could not assemble into capsids, suggesting that these residues are crucial for folding and assembly of the particles.

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Zinc micro and nanostructures were synthesized in vacuum by condensing evaporated zinc on Si substrate at different gas pressures. The morphology of the grown Zn structures was found to be dependent on the oxygen partial pressure. Depending on oxygen partial pressure it varied from two-dimensional microdisks to one-dimensional nanowire. The morphology and structural properties of the grown micro and nanostructures were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Transmission electron microscopy (TEM) studies on the grown Zn nanowires have shown that they exhibit core/shell-like structures, where a thin ZnO layer forms the shell. A possible growth mechanism behind the formation of different micro and nanostructures has been proposed. In addition, we have synthesized ZnO nanocanal-like structures by annealing Zn nanowires in vacuum at 350 °C for 30 min.

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Composites of Polystyrene-multi wall carbon nanotubes (PS-MWNTs) were prepared with loading up to 7 wt% of MWNTs by simple solvent mixing and drying technique. MWNTs with high aspect ratio similar to 4000 were used to make the polymer composites. A very high degree of dispersion of MWNTs was achieved by ultrasonication technique. As a result of high dispersion and high aspect ratio of the MWNTs electrical percolation was observed at rather low weight fraction similar to 0.0021. Characterization of the as prepared PS-MWNTs composites was done by Electron microscopy (EM), X-ray diffraction technique (XRD) and Thermogravimetery analysis (TGA).