Ag7 AND Ag8 QUANTUM CLUSTERS SUPPORTED ON ALUMINA: NEW CATALYSTS FOR ORGANIC REACTIONS

2011 ◽  
Vol 10 (04n05) ◽  
pp. 839-843 ◽  
Author(s):  
ANNAMALAI LEELAVATHI ◽  
THUMU UDAYA BHASKARA RAO ◽  
THALAPPIL PRADEEP
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Solid Phase ◽  
Kinetic Studies ◽  
X Rays ◽  
First Order ◽  
First Order Kinetics ◽  
Mercaptosuccinic Acid ◽  
Transmission Electron ◽  
Quantum Clusters

Silver quantum clusters (QCs) stabilized by mercaptosuccinic acid (MSA) have been synthesized at room temperature from Ag nanoparticles through an interfacial etching process. The as-synthesized red emitting QCs were coated on alumina and the supported clusters have been characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive analysis of X-rays (EDAX) and fluorescence spectroscopy. Catalytic activity of Ag QCs supported on alumina have been exploited for the reduction of 4-nitrophenol in presence of sodium borohydride. The reaction followed pseudo-first order kinetics. The catalyst separated from the product remains active and can be recycled several times. Other nitroaromatic compounds have also been tested. Synthesis of the solid phase catalyst, applications and detailed kinetic studies of the reduction of 4-nitrophenol are reported.

scholarly journals Surface-Limited Electrodeposition of Continuous Platinum Networks on Highly Ordered Pyrolytic Graphite

Nanomaterials ◽  
2018 ◽  
Vol 8 (9) ◽  
pp. 721 ◽  
Author(s):  
Filippo Farina ◽  
Giorgio Ercolano ◽  
Sara Cavaliere ◽  
Deborah Jones ◽  
Jacques Rozière
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Pyrolytic Graphite ◽  
Reduction Reaction ◽  
X Rays ◽  
Highly Ordered Pyrolytic Graphite ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Energy Conversion Devices

Continuous thin platinum nanoplatelet networks and thin films were obtained on the flat surface of highly ordered pyrolytic graphite (HOPG) by high overpotential electrodeposition. By increasing the deposition time, the morphology of the Pt deposits can be progressively tuned from isolated nanoplatelets, interconnected nanostructures, and thin large flat islands. The deposition is surface-limited and the thickness of the deposits, equivalent to 5 to 12 Pt monolayers, is not time dependent. The presence of Pt (111) facets is confirmed by High Resolution Transmission Electron Microscopy (HRTEM) and evidence for the early formation of a platinum monolayer is provided by Scanning Transmission Electron Microscopy and Energy Dispersive X-rays Spectroscopy (STEM-EDX) and X-ray Photoelectron Spectroscopy (XPS) analysis. The electroactivity towards the oxygen reduction reaction of the 2D deposits is also assessed, demonstrating their great potential in energy conversion devices where ultra-low loading of Pt via extended surfaces is a reliable strategy.

Morphological studies of linear (AB)n multiblock copolymers and their blends

1992 ◽  
Vol 50 (1) ◽  
pp. 384-385
Author(s):  
Richard J. Spontak ◽  
Steven D. Smith ◽  
Arman Ashraf
Keyword(s):  
Electron Microscopy ◽  
Microphase Separation ◽  
Multiblock Copolymers ◽  
First Order ◽  
Morphological Studies ◽  
Transmission Electron ◽  
First Order Phase Transition ◽  
Covalently Bonded ◽  
Total Molecular Weight ◽  
First Order Phase

Block copolymers are composed of sequences of dissimilar chemical moieties covalently bonded together. If the block lengths of each component are sufficiently long and the blocks are thermodynamically incompatible, these materials are capable of undergoing microphase separation, a weak first-order phase transition which results in the formation of an ordered microstructural network. Most efforts designed to elucidate the phase and configurational behavior in these copolymers have focused on the simple AB and ABA designs. Few studies have thus far targeted the perfectly-alternating multiblock (AB)n architecture. In this work, two series of neat (AB)n copolymers have been synthesized from styrene and isoprene monomers at a composition of 50 wt% polystyrene (PS). In Set I, the total molecular weight is held constant while the number of AB block pairs (n) is increased from one to four (which results in shorter blocks). Set II consists of materials in which the block lengths are held constant and n is varied again from one to four (which results in longer chains). Transmission electron microscopy (TEM) has been employed here to investigate the morphologies and phase behavior of these materials and their blends.

Investigation of Polyoxometalate-(Poly)pyrrole Heterogeneous Nanostructures as Cathodes for Rechargeable Magnesium-Ion Batteries

2018 ◽  
Author(s):  
Hakeem K. Henry ◽  
Sang Bok Lee
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Active Material ◽  
Conductive Polymer ◽  
Current Collector ◽  
Constant Current ◽  
Anodized Aluminum ◽  
Transmission Electron ◽  
Pyrrole Monomer

The PMo<sub>12</sub>-PPy heterogeneous cathode was synthesized electrochemically. In doing so, the PMo<sub>12</sub> redox-active material was impregnated throughout the conductive polymer matrix of the poly(pyrrole) nanowires. All chemicals and reagents used were purchased from Sigma-Aldrich. Anodized aluminum oxide (AAO) purchased from Whatman served as the porous hard template for nanowire deposition. A thin layer of gold of approximately 200nm was sputtered onto the disordered side of the AAO membrane to serve as the current collector. Copper tape was connected to the sputtered gold for contact and the device was sealed in parafilm with heat with an exposed area of 0.32 cm<sup>2</sup> to serve as the electroactive area for deposition. All electrochemical synthesis and experiments were conducted using a Bio-Logic MPG2 potentiostat. The deposition was carried out using a 3-electrode beaker cell setup with a solution of acetonitrile containing 5mM and 14mM of the phosphomolybdic acid and pyrrole monomer, respectively. The synthesis was achieved using chronoamperometry to apply a constant voltage of 0.8V vs. Ag/AgCl (BASi) to oxidatively polymerize the pyrrole monomer to poly(pyrrole). To prevent the POM from chemically polymerizing the pyrrole, an injection method was used in which the pyrrole monomer was added to the POM solution only after the deposition voltage had already been applied. The deposition was well controlled by limiting the amount of charge transferred to 300mC. Following deposition, the AAO template was removed by soaking in 3M sodium hydroxide (NaOH) for 20 minutes and rinsed several times with water. After synthesis, all cathodes underwent electrochemical testing to determine their performance using cyclic voltammetry and constant current charge-discharge cycling in 0.1 M Mg(ClO<sub>4</sub>)<sub>2</sub>/PC electrolyte. The cathodes were further characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and x-ray photoelectron spectroscopy (XPS).

scholarly journals Electro-Oxidation of Ammonia at Novel Ag2O−PrO2/γ-Al2O3 Catalysts

Coatings ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 257
Author(s):  
Mariam Khan ◽  
Naveed Kausar Janjua ◽  
Safia Khan ◽  
Ibrahim Qazi ◽  
Shafaqat Ali ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Electrochemical Impedance ◽  
Precipitation Method ◽  
Impregnation Method ◽  
X Rays ◽  
Kinetic And Thermodynamic Parameters ◽  
Catalytic Support ◽  
Transmission Electron ◽  
Electro Oxidation ◽  
Oxidation Of Ammonia

An Ag2O(x)−PrO2(y)/γ-Al2O3 electrocatalyst series (X:Y is for Ag:Pr from 0 to 10) was synthesized, to use synthesized samples in electrochemical applications, a step in fuel cells advancements. Ag2O(x)−PrO2(y)/γ-Al2O3/Glassy-Carbon was investigated for electrochemical oxidation of ammonia in alkaline medium and proved to be highly effective, having high potential utility, as compared to commonly used Pt-based electrocatalysts. In this study, gamma alumina as catalytic support was synthesized via precipitation method, and stoichiometric wt/wt.% compositions of Ag2O−PrO2 were loaded on γ-Al2O3 by co-impregnation method. The desired phase of γ-Al2O3 and supported nanocatalysts was obtained after heat treatment at 800 and 600 °C, respectively. The successful loadings of Ag2O−PrO2 nanocatalysts on surface of γ-Al2O3 was determined by X-rays diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), and energy dispersive analysis (EDX). The nano-sized domain of the sample powders sustained with particle sizes was calculated via XRD and scanning electron microscopy (SEM). The surface morphology and elemental compositions were examined by SEM, transmission electron microscopy (TEM) and EDX. The conductive and electron-transferring nature was investigated by cyclic voltammetry and electrochemical impedance (EIS). Cyclic voltammetric profiles were observed, and respective kinetic and thermodynamic parameters were calculated, which showed that these synthesized materials are potential catalysts for ammonia electro-oxidation. Ag2O(6)−PrO2(4)/γ-Al2O3 proved to be the most proficient catalyst among all the members of the series, having greater diffusion coefficient, heterogeneous rate constant and lesser Gibbs free energy for this system. The catalytic activity of these electrocatalysts is revealed from electrochemical studies which reflected their potentiality as electrode material in direct ammonia fuel cell technology for energy production.

scholarly journals Synthesis of Ce1−xPdxO2−δ Solid Solution in Molten Nitrate

Catalysts ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 640
Author(s):  
Hideaki Sasaki ◽  
Keisuke Sakamoto ◽  
Masami Mori ◽  
Tatsuaki Sakamoto
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Solid Solutions ◽  
Photoelectron Spectroscopy ◽  
Synthesis Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Co Precipitation ◽  
Ionic States

CeO2-based solid solutions in which Pd partially substitutes for Ce attract considerable attention, owing to their high catalytic performances. In this study, the solid solution (Ce1−xPdxO2−δ) with a high Pd content (x ~ 0.2) was synthesized through co-precipitation under oxidative conditions using molten nitrate, and its structure and thermal decomposition were examined. The characteristics of the solid solution, such as the change in a lattice constant, inhibition of sintering, and ionic states, were examined using X-ray diffraction (XRD), scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM−EDS), transmission electron microscopy (TEM)−EDS, and X-ray photoelectron spectroscopy (XPS). The synthesis method proposed in this study appears suitable for the easy preparation of CeO2 solid solutions with a high Pd content.

Characterization of columns grown during KrF laser micromachining of Al2O3–TiC ceramics

2003 ◽  
Vol 18 (5) ◽  
pp. 1123-1130 ◽  
Author(s):  
V. Oliveira ◽  
R. Vilar
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Laser Pulses ◽  
Formation Mechanisms ◽  
X Ray ◽  
Reducing Conditions ◽  
Transmission Electron ◽  
Column Formation ◽  
Krf Laser

This paper aims to contribute to the understanding of column formation mechanisms in Al2O3–TiC ceramics micromachined using excimer lasers. Chemical and structural characterization of columns grown in Al2O3–TiC composite processed with 200 KrF laser pulses at 10 J/cm2 was carried out by scanning electron microscopy, transmission electron microscopy, x-ray photoelectron spectroscopy, and x-ray diffraction analysis. Fully developed columns consist of a core of unprocessed material surrounded by an outer layer of Al2TiO5, formed in oxidizing conditions, and an inner layer, formed in reducing conditions, composed of TiC and Al3Ti or an AlTi solid solution. Possible mechanisms of column formation are discussed.

scholarly journals Green Synthesis of Feather-Shaped MoS2/CdS Photocatalyst for Effective Hydrogen Production

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Yang Liu ◽  
Hongtao Yu ◽  
Xie Quan ◽  
Shuo Chen
Keyword(s):  
Electron Microscopy ◽  
Hydrogen Production ◽  
Photoelectron Spectroscopy ◽  
Diffuse Reflectance ◽  
Sulfur Source ◽  
X Ray ◽  
Transmission Electron ◽  
Microscopy Images ◽  
Effective Hydrogen ◽  
Better Than

MoS2/CdS photocatalyst was fabricated by a hydrothermal method for H2production under visible light. This method used low toxic thiourea as a sulfur source and was carried out at 200°C. Thus, it was better than the traditional methods, which are based on an annealing process at relatively high temperature (above 400°C) using toxic H2S as reducing agent. Scanning electron microscopy and transmission electron microscopy images showed that the morphologies of MoS2/CdS samples were feather shaped and MoS2layer was on the surface of CdS. The X-ray photoelectron spectroscopy testified that the sample was composed of stoichiometric MoS2and CdS. The UV-vis diffuse reflectance spectra displayed that the loading of MoS2can enhance the optical absorption of MoS2/CdS. The photocatalytic activity of MoS2/CdS was evaluated by producing hydrogen. The hydrogen production rate on MoS2/CdS reached 192 μmol·h−1. This performance was stable during three repeated photocatalytic processes.

scholarly journals Aluminum Nitride-Silicon Carbide Alloy Crystals Grown on SiC Substrates by Sublimation

2005 ◽  
Vol 10 ◽  
Author(s):  
Z. Gu ◽  
L. Du ◽  
J.H. Edgar ◽  
E.A. Payzant ◽  
L. Walker ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
X Ray Diffraction ◽  
Original Source ◽  
X Ray ◽  
Alloy Crystal ◽  
Transmission Electron ◽  
Crystal Substrate ◽  
Vapor Distribution ◽  
Uniform Composition

AlN-SiC alloy crystals, with a thickness greater than 500 µm, were grown on 4H- and 6H-SiC substrates from a mixture of AlN and SiC powders by the sublimation-recondensation method at 1860-1990 °C. On-axis SiC substrates produced a rough surface covered with hexagonal grains, while 6H- and 4H- off-axis SiC substrates with different miscut angles (8° or 3.68°) formed a relatively smooth surface with terraces and steps. The substrate misorientation ensured that the AlN-SiC alloy crystals grew two dimensionally as identified by scanning electron microscopy (SEM). X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed that the AlN-SiC alloys had the wurtzite structure. Electron probe microanalysis (EPMA) and x-ray photoelectron spectroscopy (XPS) demonstrated that the resultant alloy crystals had non-stoichiometric ratios of Al:N and Si:C and a uniform composition throughout the alloy crystal from the interface to the surface. The composition ratio of Al:Si of the alloy crystals changed with the growth temperature, and differed from the original source composition, which was consistent with the results predicted by thermodynamic calculation of the solid-vapor distribution of each element. XPS detected the bonding between Si-C, Si-N, Si-O for the Si 2p spectra. The dislocation density decreased with the growth, which was lower than 106 cm−2 at the alloy surface, more than two orders of magnitude lower compared to regions close to the crystal/substrate interface, as determined by TEM.

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