scholarly journals Green Preparation of High Surface Area Cu-Au Bimetallic Nanostructured Materials by Co-Electrodeposition in a Deep Eutectic Solvent

2021 ◽  
Author(s):  
Elena Plaza Mayoral ◽  
Paula Sebastián Pascual ◽  
Kim Nicole Dalby ◽  
Kim Degn Jensen ◽  
Ib Chorkendorff ◽  
...  
Keyword(s):  
Surface Area ◽  
Nanostructured Materials ◽  
Photoelectron Spectroscopy ◽  
Choline Chloride ◽  
High Surface ◽  
High Surface Area ◽  
Deep Eutectic Solvent ◽  
Fold Increase ◽  
Active Surface Area ◽  
X Ray

In this work we present an electrodeposition method in a deep eutectic solvent (DES) to prepare bimetallic high surface area nanostructures of Cu and Au with tunable structure and composition. The metal electrodeposition performed in green choline chloride within a urea deep eutectic solvent allows us to tailor the size, morphology and elemental composition of the deposits. We combine electrochemical methods with scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS) to characterize the electrodeposited nanostructured materials. We assess the increase of the electroactive surface area through the analysis of the lead underpotential deposition (UPD) on the prepared films. We observe a 5 to 15-fold increase of the active surface area compared to flat surfaces of polycrystalline Cu or Au. Our work reports, for the first time, a green route for the electrodeposition of Cu-Au bimetallic nanostructures in a deep eutectic solvent.

scholarly journals Green Preparation of High Surface Area Cu-Au Bimetallic Nanostructured Materials by Co-Electrodeposition in a Deep Eutectic Solvent

2021 ◽  
Author(s):  
Elena Plaza Mayoral ◽  
Paula Sebastián Pascual ◽  
Kim Nicole Dalby ◽  
Kim Degn Jensen ◽  
Ib Chorkendorff ◽  
...  
Keyword(s):  
Surface Area ◽  
Nanostructured Materials ◽  
Photoelectron Spectroscopy ◽  
Choline Chloride ◽  
High Surface ◽  
High Surface Area ◽  
Deep Eutectic Solvent ◽  
Fold Increase ◽  
Active Surface Area ◽  
X Ray

In this work we present an electrodeposition method in a deep eutectic solvent (DES) to prepare bimetallic high surface area nanostructures of Cu and Au with tunable structure and composition. The metal electrodeposition performed in green choline chloride within a urea deep eutectic solvent allows us to tailor the size, morphology and elemental composition of the deposits. We combine electrochemical methods with scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS) to characterize the electrodeposited nanostructured materials. We assess the increase of the electroactive surface area through the analysis of the lead underpotential deposition (UPD) on the prepared films. We observe a 5 to 15-fold increase of the active surface area compared to flat surfaces of polycrystalline Cu or Au. Our work reports, for the first time, a green route for the electrodeposition of Cu-Au bimetallic nanostructures in a deep eutectic solvent.

scholarly journals Characteristics of High Surface Area Molybdenum Nitride and Its Activity for the Catalytic Decomposition of Ammonia

Catalysts ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 192
Author(s):  
Seo-Hyeon Baek ◽  
Kyunghee Yun ◽  
Dong-Chang Kang ◽  
Hyejin An ◽  
Min Bum Park ◽  
...  
Keyword(s):  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
High Surface ◽  
High Surface Area ◽  
Catalytic Decomposition ◽  
Molybdenum Nitride ◽  
X Ray ◽  
Temperature Programmed Oxidation ◽  
Oxidation Reduction ◽  
Temperature Programmed

High surface area (>170 m2 g−1) molybdenum nitride was prepared by the temperature-programmed nitridation of α-MoO3 with pure ammonia. The process was optimized by adjusting the experimental variables: the reaction temperature, heating rate, and molar flow rate of ammonia. The physicochemical properties of the as-formed molybdenum nitride were characterized by X-ray diffraction, N2 sorption, transmission electron microscopy, temperature-programmed oxidation/reduction, and X-ray photoelectron spectroscopy. Of the experimental variables, the nitridation temperature was found to be the most critical parameter determining the surface area of the molybdenum nitride. When the prepared molybdenum nitride was exposed to air, the specific surface area rapidly decreased because of the partial oxidation of molybdenum nitride to molybdenum oxynitride. However, the surface area recovered to 90% the initial value after H2 treatment. The catalyst with the highest degree of nitridation showed the best catalytic activity, superior to that of unmodified α-MoO3, for the decomposition of ammonia because of its high surface area.

Characterization of High Surface Area Silicon Oxynitrides

1992 ◽  
Vol 271 ◽  
Author(s):  
Peter W. Lednor ◽  
Rene De Ruiter ◽  
Kees A. Emeis
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
High Surface ◽  
High Surface Area ◽  
X Ray ◽  
Silicon Oxynitrides

ABSTRACTHigh surface area silicon oxynitrides have been prepared by nitrida- tion of silica with ammonia. Characterization by Fourier-transform infrared spectroscopy has allowed quantitative determination of hydroxyl, amido and imido groups. Data obtained by X-ray photoelectron spectroscopy show that the nitrogen is well distributed in the surface of the materials.

scholarly journals Preparation of high surface area Cu-Au bimetallic nanostructured materials by co-electrodeposition in a deep eutectic solvent

2021 ◽  
pp. 139309
Author(s):  
Elena Plaza-Mayoral ◽  
Paula Sebastián-Pascual ◽  
Kim Nicole Dalby ◽  
Kim Degn Jensen ◽  
Ib Chorkendorff ◽  
...  
Keyword(s):  
Surface Area ◽  
Nanostructured Materials ◽  
High Surface ◽  
High Surface Area ◽  
Deep Eutectic Solvent

Facile preparation of CeO2 microspheres with high surface area by ultrasonic spray pyrolysis

2018 ◽  
Vol 7 (3) ◽  
pp. 241-247 ◽  
Author(s):  
Shou-Feng Xue ◽  
Wen-Yuan Wu ◽  
Xue Bian ◽  
Zhen-Feng Wang ◽  
Yong-Fu Wu
Keyword(s):  
Electron Microscopy ◽  
Spray Pyrolysis ◽  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
High Surface ◽  
High Surface Area ◽  
Ultrasonic Spray Pyrolysis ◽  
Relative Sensitivity ◽  
X Ray ◽  
Ultrasonic Spray

Abstract CeCl3 solution was used as a precursor to prepare CeO2 microspheres by ultrasonic spray pyrolysis (USP). This is a green process that allows the transformation from CeCl3 to CeO2 without consuming any precipitant. The prepared material was investigated through various analysis technologies, such as X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high resolution TEM (HRTEM), energy dispersive X-ray spectroscopy (EDS), N2 adsorption-desorption and X-ray photoelectron spectroscopy (XPS). The prepared sample was confirmed as high purity CeO2 microspheres, and two different microstructures were observed. The microsphere surface area was 86.5 m2/g according to the Brunauer-Emmett-Teller method. The microsphere diameter ranged from 0.09 μm to 3.86 μm and the microsphere surface was covered by numerous nanoparticles. The observed nanoparticles ranged in size from 19 nm to 200 nm as determined from FESEM and HRTEM images. The concentrations of Ce4+, Ce3+, residual chloride and oxygen vacancy in CeO2 were studied by relative sensitivity factors based on the XPS results. Finally, the data suggested the possible formation mechanism of the CeO2 microsphere structure.

Tenacious Mass Transfer Limitations Drive Catalytic Selectivity during Electrochemical Carbon Dioxide Reduction

2019 ◽  
Author(s):  
Kailun Yang ◽  
Recep Kas ◽  
Wilson A. Smith
Keyword(s):  
Surface Area ◽  
High Surface ◽  
High Surface Area ◽  
Catalyst Layer ◽  
Active Surface ◽  
Active Surface Area ◽  
High Concentration ◽  
Copper Electrodes ◽  
Surface Enhanced ◽  
Local Current

<p>This study evaluated the performance of the commonly used strong buffer electrolytes, i.e. phosphate buffers, during CO<sub>2</sub> electroreduction in neutral pH conditions by using in-situ surface enhanced infrared absorption spectroscopy (SEIRAS). Unfortunately, the buffers break down a lot faster than anticipated which has serious implications on many studies in the literature such as selectivity and kinetic analysis of the electrocatalysts. Increasing electrolyte concentration, surprisingly, did not extend the potential window of the phosphate buffers due to dramatic increase in hydrogen evolution reaction. Even high concentration phosphate buffers (1 M) break down within the potentials (-1 V vs RHE) where hydrocarbons are formed on copper electrodes. We have extended the discussion to high surface area electrodes by evaluating electrodes composed of copper nanowires. We would like highlight that it is not possible to cope with high local current densities on these high surface area electrodes by using high buffer capacity solutions and the CO<sub>2</sub> electrocatalysts are needed to be evaluated by casting thin nanoparticle films onto inert substrates as commonly employed in fuel cell reactions and up to now scarcely employed in CO<sub>2</sub> electroreduction. In addition, we underscore that normalization of the electrocatalytic activity to the electrochemical active surface area is not the ultimate solution due to concentration gradient along the catalyst layer.This will “underestimate” the activity of high surface electrocatalyst and the degree of underestimation will depend on the thickness, porosity and morphology of the catalyst layer. </p> <p> </p>

scholarly journals Non-Thermal Plasma-Modified Ru-Sn-Ti Catalyst for Chlorinated Volatile Organic Compound Degradation

Catalysts ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 1456
Author(s):  
Yujie Fu ◽  
You Zhang ◽  
Qi Xin ◽  
Zhong Zheng ◽  
Yu Zhang ◽  
...  
Keyword(s):  
Plasma Treatment ◽  
Photoelectron Spectroscopy ◽  
High Surface ◽  
High Surface Area ◽  
Surface Oxidation ◽  
Treatment Method ◽  
X Ray ◽  
Chlorinated Volatile Organic Compounds ◽  
Volatile Organic ◽  
Doped Titania

Chlorinated volatile organic compounds (CVOCs) are vital environmental concerns due to their low biodegradability and long-term persistence. Catalytic combustion technology is one of the more commonly used technologies for the treatment of CVOCs. Catalysts with high low-temperature activity, superior selectivity of non-toxic products, and resistance to chlorine poisoning are desirable. Here we adopted a plasma treatment method to synthesize a tin-doped titania loaded with ruthenium dioxide (RuO2) catalyst, possessing enhanced activity (T90%, the temperature at which 90% of dichloromethane (DCM) is decomposed, is 262 °C) compared to the catalyst prepared by the conventional calcination method. As revealed by transmission electron microscopy, X-ray diffraction, N2 adsorption, X-ray photoelectron spectroscopy, and hydrogen temperature-programmed reduction, the high surface area of the tin-doped titania catalyst and the enhanced dispersion and surface oxidation of RuO2 induced by plasma treatment were found to be the main factors determining excellent catalytic activities.

scholarly journals Organomineral nanocomposite carbon burial during Oceanic Anoxic Event 2

2014 ◽  
Vol 11 (5) ◽  
pp. 6815-6844
Author(s):  
S. C. Löhr ◽  
M. J. Kennedy
Keyword(s):  
Surface Area ◽  
High Surface ◽  
High Surface Area ◽  
Mineral Surfaces ◽  
Mineral Surface ◽  
X Ray ◽  
Oceanic Anoxic Event ◽  
Carbon Burial ◽  
Anoxic Events ◽  
Mineral Surface Area

Abstract. Organic carbon (OC) enrichment in sediments deposited during Oceanic Anoxic Events (OAEs) is commonly attributed to elevated productivity and marine anoxia. We find that OC enrichment in the late Cenomanian aged OAE2 at Demerara Rise was controlled by co-occurrence of anoxic bottom-water, sufficient productivity to saturate available mineral surfaces and variable deposition of high surface area detrital smectite clay. Redox indicators show consistently oxygen-depleted conditions, while a strong correlation between OC concentration and sediment mineral surface area (R2=0.92) occurs across a range of TOC values from 9–33%. X-ray diffraction data indicates intercalation of OC in smectite interlayers while electron, synchrotron infrared and X-ray microscopy show an intimate association between clay minerals and OC, consistent with preservation of OC as organomineral nanocomposites and aggregates rather than discrete, μm-scale pelagic detritus. Since the consistent ratio between TOC and mineral surface area suggests that excess OC relative to surface area is lost, we propose that it is the varying supply of smectite that best explains variable organic enrichment against a backdrop of continuous anoxia, which is conducive to generally high TOC during OAE2 at Demerara Rise. Smectitic clays are unique in their ability to form stable organomineral nanocomposites and aggregates that preserve organic matter, and are common weathering products of continental volcanic deposits. An increased flux of smectite coinciding with high carbon burial is consistent with evidence for widespread volcanism during OAE2, so that organomineral carbon burial may represent a potential feedback to volcanic degassing of CO2.

scholarly journals Enhanced Photocatalytic Activity of Titania by Co-Doping with Mo and W

Catalysts ◽  
2018 ◽  
Vol 8 (12) ◽  
pp. 631 ◽  
Author(s):  
Osmín Avilés-García ◽  
Jaime Espino-Valencia ◽  
Rubí Romero-Romero ◽  
José Rico-Cerda ◽  
Manuel Arroyo-Albiter ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Diffuse Reflectance Spectroscopy ◽  
High Surface ◽  
High Surface Area ◽  
Absorption Capacity ◽  
Radiation Absorption ◽  
Experimental Conditions ◽  
X Ray ◽  
Assembly Method ◽  
Co Doped

Various W and Mo co-doped titanium dioxide (TiO2) materials were obtained through the EISA (Evaporation-Induced Self-Assembly) method and then tested as photocatalysts in the degradation of 4-chlorophenol. The synthesized materials were characterized by thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Raman spectroscopy (RS), N2 physisorption, UV-vis diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The results showed that the W-Mo-TiO2 catalysts have a high surface area of about 191 m2/g, and the presence of an anatase crystalline phase. The co-doped materials exhibited smaller crystallite sizes than those with one dopant, since the crystallinity is inhibited by the presence of both species. In addition, tungsten and molybdenum dopants are distributed and are incorporated into the anatase structure of TiO2, due to changes in red parameters and lattice expansion. Under our experimental conditions, the co-doped TiO2 catalyst presented 46% more 4-chlorophenol degradation than Degussa P25. The incorporation of two dopant cations in titania improved its photocatalytic performance, which was attributed to a cooperative effect by decreasing the recombination of photogenerated charges, high radiation absorption capacity, high surface areas, and low crystallinity. When TiO2 is co-doped with the same amount of both cations (1 wt.%), the highest degradation and mineralization (97% and 74%, respectively) is achieved. Quinones were the main intermediates in the 4-chlorophenol oxidation by W-Mo-TiO2 and 1,2,4-benzenetriol was incompletely degraded.

Hydrothermal Synthesis and Characterization of Phosphor Doped Tetragonal Zirconia Nanocrystallites

2011 ◽  
Vol 197-198 ◽  
pp. 846-852
Author(s):  
Jian Jun Yin ◽  
Tao Wang ◽  
Wei Jing Xing
Keyword(s):  
Photoelectron Spectroscopy ◽  
Raw Materials ◽  
High Surface ◽  
High Surface Area ◽  
Tetragonal Zirconia ◽  
Zirconium Oxychloride ◽  
Dihydrogen Phosphate ◽  
Hydrothermal Conditions ◽  
Hydrothermal Temperature ◽  
X Ray

Using zirconium oxychloride hydrate ( ZrOCl2•8H2O) and ammonia water (NH3•H2O) as raw materials, and ammonium dihydrogen phosphate (NH4H2PO4) as additives, tetragonal zirconia (t-ZrO2) with size range of 8–12 nm were prepared by coprecipitation method under hydrothermal conditions. The influence factors on phase transformation and the particle size such as phosphor loading, hydrothermal temperature and calcination temperature were studied by X-ray diffraction (XRD), Fourier transform Roman spectra (FT-Roman), the Brunauer-Emmett-Teller (BET) method and X-ray photoelectron spectroscopy (XPS) techniques etc. Research results show that a small amount of phosphor has been incorporated into the framework of ZrO2 crystals, producing a certain amount of oxygen vacancies. Phosphor can effectively restrain crystal particles growth and improve the thermal stability of metastable t-ZrO2. The phosphor doped t-ZrO2 had a high surface area (244.2 m2/g). In contrast to the pure ZrO2 particles readily aggregating, the phosphor species deposited on the framework of ZrO2 crystals prevented the agglomeration of the primary particles during calcinations.

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