Nano-Folded Gold Electrocatalysts Enhance the Selectivity of Carbon Dioxide Reduction

2019 ◽  
Author(s):  
Kam Sang Kwok ◽  
Yuxuan Wang ◽  
Michael Cao ◽  
Hao Shen ◽  
Weinan Xu ◽  
...  

<p>The local structure and geometry of catalytic interfaces can influence the selectivity of chemical reactions. Here, using a pre-strained polymer, we uniaxially compress a thin gold film to form a nano-folded catalyst. We observe two kinds of folds and can tune the ratio of loose to tight folds by varying the extent of pre-strain in the polymer. We characterize the nano-folded catalysts using x-ray diffraction, scanning, and transmission electron microscopy. We observe grain reorientation and coarsening in the nano-folded gold catalysts. Electroreduction of carbon dioxide with these nano-folded catalysts reveals an enhancement of Faradaic efficiency for carbon monoxide formation by a factor of about four. This result suggests that electrolyte mass transport limitations and an increase of the local pH in the tight folds of the catalyst outweigh the effects of alterations in grain characteristics. Together, our studies demonstrate that nano-folded geometries can significantly alter grain characteristics, mass transport, and catalytic selectivity. </p>

2019 ◽  
Author(s):  
Kam Sang Kwok ◽  
Yuxuan Wang ◽  
Michael Cao ◽  
Hao Shen ◽  
Weinan Xu ◽  
...  

<p>The local structure and geometry of catalytic interfaces can influence the selectivity of chemical reactions. Here, using a pre-strained polymer, we uniaxially compress a thin gold film to form a nano-folded catalyst. We observe two kinds of folds and can tune the ratio of loose to tight folds by varying the extent of pre-strain in the polymer. We characterize the nano-folded catalysts using x-ray diffraction, scanning, and transmission electron microscopy. We observe grain reorientation and coarsening in the nano-folded gold catalysts. Electroreduction of carbon dioxide with these nano-folded catalysts reveals an enhancement of Faradaic efficiency for carbon monoxide formation by a factor of about four. This result suggests that electrolyte mass transport limitations and an increase of the local pH in the tight folds of the catalyst outweigh the effects of alterations in grain characteristics. Together, our studies demonstrate that nano-folded geometries can significantly alter grain characteristics, mass transport, and catalytic selectivity. </p>


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):  
R. Gronsky

The phenomenon of clustering in Al-Ag alloys has been extensively studied since the early work of Guinierl, wherein the pre-precipitation state was characterized as an assembly of spherical, ordered, silver-rich G.P. zones. Subsequent x-ray and TEM investigations yielded results in general agreement with this model. However, serious discrepancies were later revealed by the detailed x-ray diffraction - based computer simulations of Gragg and Cohen, i.e., the silver-rich clusters were instead octahedral in shape and fully disordered, atleast below 170°C. The object of the present investigation is to examine directly the structural characteristics of G.P. zones in Al-Ag by high resolution transmission electron microscopy.


Author(s):  
Vicki L. Baliga ◽  
Mary Ellen Counts

Calcium is an important element in the growth and development of plants and one form of calcium is calcium oxalate. Calcium oxalate has been found in leaf seed, stem material plant tissue culture, fungi and lichen using one or more of the following methods—polarized light microscopy (PLM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction.Two methods are presented here for qualitatively estimating calcium oxalate in dried or fixed tobacco (Nicotiana) leaf from different stalk positions using PLM. SEM, coupled with energy dispersive x-ray spectrometry (EDS), and powder x-ray diffraction were used to verify that the crystals observed in the dried leaf with PLM were calcium oxalate.


Author(s):  
A. Zangvil ◽  
L.J. Gauckler ◽  
G. Schneider ◽  
M. Rühle

The use of high temperature special ceramics which are usually complex materials based on oxides, nitrides, carbides and borides of silicon and aluminum, is critically dependent on their thermomechanical and other physical properties. The investigations of the phase diagrams, crystal structures and microstructural features are essential for better understanding of the macro-properties. Phase diagrams and crystal structures have been studied mainly by X-ray diffraction (XRD). Transmission electron microscopy (TEM) has contributed to this field to a very limited extent; it has been used more extensively in the study of microstructure, phase transformations and lattice defects. Often only TEM can give solutions to numerous problems in the above fields, since the various phases exist in extremely fine grains and subgrain structures; single crystals of appreciable size are often not available. Examples with some of our experimental results from two multicomponent systems are presented here. The standard ion thinning technique was used for the preparation of thin foil samples, which were then investigated with JEOL 200A and Siemens ELMISKOP 102 (for the lattice resolution work) electron microscopes.


Author(s):  
John A. Sutliff

Near-eutectic Pb-Sn alloys are important solders used by the electronics industry. In these solders, the eutectic mixture, which solidifies last, is the important microstructural consituent. The orientation relation (OR) between the eutectic phases has previously been determined for directionally solidified (DS) eutectic alloys using x-ray diffraction or electron chanelling techniques. In the present investigation the microstructure of a conventionally cast, hyper-eutectic Pb-Sn alloy was examined by transmission electron microscopy (TEM) and the OR between the eutectic phases was determined by electron diffraction. Precipitates of Sn in Pb were also observed and the OR determined. The same OR was found in both the eutectic and precipitation reacted materials. While the precipitation of Sn in Pb was previously shown to occur by a discontinuous precipitation reaction,3 the present work confirms a recent finding that volume diffusion controlled precipitation can also occur.Samples that are representative of the solder's cast microstructure are difficult to prepare for TEM because the alloy is multiphase and the phases are soft.


2002 ◽  
Vol 716 ◽  
Author(s):  
Seok Woo Hong ◽  
Yong Sun Lee ◽  
Ki-Chul Park ◽  
Jong-Wan Park

AbstractThe effect of microstructure of dc magnetron sputtered TiN and TaN diffusion barriers on the palladium activation for autocatalytic electroless copper deposition has been investigated by using X-ray diffraction, sheet resistance measurement, field emission scanning electron microscopy (FE-SEM) and plan view transmission electron microscopy (TEM). The density of palladium nuclei on TaN diffusion barrier increases as the grain size of TaN films decreases, which was caused by increasing nitrogen content in TaN films. Plan view TEM results of TiN and TaN diffusiton barriers showed that palladium nuclei formed mainly on the grain boundaries of the diffusion barriers.


2003 ◽  
Vol 775 ◽  
Author(s):  
Donghai Wang ◽  
David T. Johnson ◽  
Byron F. McCaughey ◽  
J. Eric Hampsey ◽  
Jibao He ◽  
...  

AbstractPalladium nanowires have been electrodeposited into mesoporous silica thin film templates. Palladium continually grows and fills silica mesopores starting from a bottom conductive substrate, providing a ready and efficient route to fabricate a macroscopic palladium nanowire thin films for potentially use in fuel cells, electrodes, sensors, and other applications. X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicate it is possible to create different nanowire morphology such as bundles and swirling mesostructure based on the template pore structure.


2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Claudia Maria Simonescu ◽  
Valentin Serban Teodorescu ◽  
Camelia Capatina

This paper presents the obtaining of copper sulfide CuS (covelite) from Cu(CH3COO)2.H2O and thioacetamide (TAA) system. The reaction was conducted in presence or absence of sodium-bis(2-ethylhexyl) sulfosuccinate (Na-AOT). The effects of various reaction parameters on the size and on the shape of nanoparticles have been examined. CuS obtained was characterized by X ray diffraction, IR spectroscopy, TEM � transmission electron microscopy and SAED selected area electron diffraction. The influence of surfactant to the shape and size of CuS (covellite) nanocrystals was established. The size of the nanocrystals varied from 10-60 nm depending on the reaction conditions such as quantity of surfactant.


Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.


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