scholarly journals Resonant-XRD Characterization of Nanoalloyed Au-Pd Catalysts for the Direct Synthesis of H2O2: Quantitative Analysis of Size Dependent Composition of the Nanoparticles †

2019 ◽  
Vol 9 (15) ◽  
pp. 2959 ◽  
Author(s):  
Paolo Centomo ◽  
Patrizia Canton ◽  
Claudio Burato ◽  
Carlo Meneghini ◽  
Marco Zecca

The focus of this work is on the relationship between the quantitative structural characterization of bimetallic Au-Pd nanoparticles dispersed in an amorphous polymer matrix and their catalytic activity in the direct synthesis of hydrogen peroxide (DS reaction). Resonant X-ray powder diffraction with synchrotron radiation was employed to probe selectively and to reveal fine details of the structure of bimetallic nanoparticles embedded in the support. The semi-quantitative analysis of the resonant X-ray powdered diffraction data, made on a large number of metal nanoparticles, shows that in one of the polymer-supported Au-Pd catalyst for the DS reaction (P75) featured by an overall molar Pd/Au of about 5.54, the smallest metal nanoparticles (MNPs), which account for more than 99.9% of the total MNPs number and for more than 95% of the metal surface, are formed by practically pure palladium. The relative number of bimetallic alloyed nanoparticles is very small (less than 4 × 102 ppm) and they contribute to only about 2% of the total metal surface. In a second gold-enriched catalyst (P50) with an overall molar Pd/Au of 1.84, the proportion of the bimetallic alloyed nanoparticles increased to about 97% and they account for about 99% of the metal surface. As a result of the metal intermixing, the catalytic productivity for the DS reaction increased from 97 to 109 mmolH2O2/molH2, owing to the gold-promotion of palladium.

2012 ◽  
Vol 730-732 ◽  
pp. 569-574
Author(s):  
Marta Cabral ◽  
Fernanda Margarido ◽  
Carlos A. Nogueira

Spent Ni-MH batteries are not considered too dangerous for the environment, but they have a considerable economical value due to the chemical composition of electrodes which are highly concentrated in metals. The present work aimed at the physical and chemical characterisation of spent cylindrical and thin prismatic Ni-MH batteries, contributing for a better definition of the recycling process of these spent products. The electrode materials correspond to more than 50% of the batteries weight and contain essentially nickel and rare earths (RE), and other secondary elements (Co, Mn, Al). The remaining components are the steel parts from the external case and supporting grids (near 30%) containing Fe and Ni, and the plastic components (<10%). Elemental quantitative analysis showed that the electrodes are highly concentrated in metals. Phase identification by X-ray powder diffraction combined with chemical analysis and leaching experiments allowed advancing the electrode materials composition. The cathode is essentially constituted by 6% metallic Ni, 66% Ni(OH)2, 4.3% Co(OH)2 and the anode consists mainly in 62% RENi5 and 17% of substitutes and/or additives such as Co, Mn and Al.


Author(s):  
Anatoly Frenkel

We discuss methods of Extended X-ray Absorption Fine-Structure (EXAFS) analysis that provide three-dimensional structural characterization of metal nanoparticles, both mono- and bi-metallic. For the bimetallic alloys, we use short range order measurements to discriminate between random and non-random inter-particle distributions of atoms. We also discuss the application of EXAFS to heterogeneous nanoparticle systems.


Nanomaterials ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 1129 ◽  
Author(s):  
Izabela Wysocka ◽  
Ewa Kowalska ◽  
Jacek Ryl ◽  
Grzegorz Nowaczyk ◽  
Anna Zielińska-Jurek

Noble metal nanoparticles (NMNPs) enhanced TiO2 response and extended its activity under visible light. Photocatalytic activity of TiO2 modified with noble metal nanoparticles strongly depends on the physicochemical properties of NMNPs. Among others, the differences in the size of NMNPs seems to be one of the most important factors. In this view, the effect of the metal’s nanoparticles size, type and amount on TiO2 photocatalytic and biocidal activity was investigated. TiO2 modified with mono- and bimetallic nanoparticles of Pt, Cu and Ag were prepared using chemical and thermal reduction methods. Obtained nanocomposites were characterized using transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and diffuse-reflectance spectroscopy (DR/UV-Vis) techniques. The photocatalytic activity was examined in 2-propanol oxidation and hydrogen generation processes. The mechanism of modified TiO2 excitation was evaluated in action spectrum measurements during phenol oxidation. A possibility of using less energy-consuming light sources as a set of light-emitting diodes (LEDs) selected based on action spectrum results was examined. It was found that the differences in NMNPs size were the result of the reduction method. Moreover, coupling with a second metal strongly affected and differentiated the photocatalytic and biocidal activity of the obtained TiO2-based photocatalysts.


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.


Author(s):  
V. V. Damiano ◽  
R. P. Daniele ◽  
H. T. Tucker ◽  
J. H. Dauber

An important example of intracellular particles is encountered in silicosis where alveolar macrophages ingest inspired silica particles. The quantitation of the silica uptake by these cells may be a potentially useful method for monitoring silica exposure. Accurate quantitative analysis of ingested silica by phagocytic cells is difficult because the particles are frequently small, irregularly shaped and cannot be visualized within the cells. Semiquantitative methods which make use of particles of known size, shape and composition as calibration standards may be the most direct and simplest approach to undertake. The present paper describes an empirical method in which glass microspheres were used as a model to show how the ratio of the silicon Kα peak X-ray intensity from the microspheres to that of a bulk sample of the same composition correlated to the mass of the microsphere contained within the cell. Irregular shaped silica particles were also analyzed and a calibration curve was generated from these data.


Author(s):  
H.J. Dudek

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S


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