scholarly journals In situ spectroscopic monitoring of CO2 reduction at copper oxide electrode

2017 ◽  
Vol 197 ◽  
pp. 517-532 ◽  
Author(s):  
Liying Wang ◽  
Kalyani Gupta ◽  
Josephine B. M. Goodall ◽  
Jawwad A. Darr ◽  
Katherine B. Holt
Keyword(s):  
Infrared Spectroscopy ◽  
Copper Oxide ◽  
Photoelectron Spectroscopy ◽  
Co2 Reduction ◽  
Modified Electrodes ◽  
Starting Material ◽  
Ex Situ ◽  
Spectroscopic Monitoring ◽  
Carbonate Species

Copper oxide modified electrodes were investigated as a function of applied electrode potential using in situ infrared spectroscopy and ex situ Raman and X-ray photoelectron spectroscopy. In deoxygenated KHCO3 electrolyte bicarbonate and carbonate species were found to adsorb to the electrode during reduction and the CuO was reduced to Cu(i) or Cu(0) species. Carbonate was incorporated into the structure and the CuO starting material was not regenerated on cycling to positive potentials. In contrast, in CO2 saturated KHCO3 solution, surface adsorption of bicarbonate and carbonate was not observed and adsorption of a carbonato-species was observed with in situ infrared spectroscopy. This species is believed to be activated, bent CO2. On cycling to negative potentials, larger reduction currents were observed in the presence of CO2; however, less of the charge could be attributed to the reduction of CuO. In the presence of CO2 CuO underwent reduction to Cu2O and potentially Cu, with no incorporation of carbonate. Under these conditions the CuO starting material could be regenerated by cycling to positive potentials.

CO2 Reduction to Propanol by Copper Foams: A Pre- and Post-Catalysis Study

2020 ◽  
Author(s):  
Jennifer A. Rudd ◽  
Ewa Kazimierska ◽  
Louise B. Hamdy ◽  
Odin Bain ◽  
Sunyhik Ahn ◽  
...  
Keyword(s):  
Carbon Dioxide ◽  
Photoelectron Spectroscopy ◽  
Carbon Capture ◽  
Surface Composition ◽  
Co2 Reduction ◽  
Structural Rearrangement ◽  
Copper Electrode ◽  
Ex Situ ◽  
X Ray ◽  
Copper Electrodes

The utilization of carbon dioxide is a major incentive for the growing field of carbon capture. Carbon dioxide could be an abundant building block to generate higher value products. Herein, we describe the use of porous copper electrodes to catalyze the reduction of carbon dioxide into higher value products such as ethylene, ethanol and, notably, propanol. For <i>n</i>-propanol production, faradaic efficiencies reach 4.93% at -0.83 V <i>vs</i> RHE, with a geometric partial current density of -1.85 mA/cm<sup>2</sup>. We have documented the performance of the catalyst in both pristine and urea-modified foams pre- and post-electrolysis. Before electrolysis, the copper electrode consisted of a mixture of cuboctahedra and dendrites. After 35-minute electrolysis, the cuboctahedra and dendrites have undergone structural rearrangement. Changes in the interaction of urea with the catalyst surface have also been observed. These transformations were characterized <i>ex-situ</i> using scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. We found that alterations in the morphology, crystallinity, and surface composition of the catalyst led to the deactivation of the copper foams.

Dependence of the intrinsic phase structure of Bi2O3 catalysts on photocatalytic CO2 reduction

2021 ◽  
Vol 11 (6) ◽  
pp. 2021-2025
Author(s):  
Liujin Wei ◽  
Guan Huang ◽  
Yajun Zhang
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Fourier Transform Infrared Spectroscopy ◽  
Phase Structure ◽  
Co2 Reduction ◽  
Fourier Transform Infrared ◽  
Time Resolved ◽  
Dependent Activity

The combination of time-resolved transient photoluminescence with in-situ Fourier transform infrared spectroscopy has been conducted to investigate the intrinsic phase structure-dependent activity of Bi2O3 catalyst for CO2 reduction.

On The Optimized Nucleation of Near-Single-Crystal Cvd Diamond Film

1995 ◽  
Vol 416 ◽  
Author(s):  
L. C. Chen ◽  
C. C. Juan ◽  
J. Y. Wu ◽  
K. H. Chen ◽  
J. W. Teng
Keyword(s):  
Single Crystal ◽  
Photoelectron Spectroscopy ◽  
Morphological Evolution ◽  
Present Report ◽  
Ex Situ ◽  
Nucleation Density ◽  
Induced Current ◽  
Current Time ◽  
Single Crystal Diamond

ABSTRACTNear-single-crystal diamond films have been obtained in a number of laboratories recently. The optimization of nucleation density by using a bias-enhanced nucleation (BEN) method is believed to be a critical step. However, the condition of optimized nucleation has never been clearly delineated. In the present report, a novel quantitative technique was established to monitor the nucleation of diamond in-situ. Specifically, the induced current was measured as a function of nucleation time during BEN. The timedependence of induced current was studied under various methane concentrations as well as substrate temperatures. The optimized nucleation condition can be unambiguously determined from the current-time plot. Besides the in-situ current probe, ex-situ x-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) were also used to investigate the chemical and morphological evolution. Characteristic XPS and AFM features of optimized nucleation is discussed.

scholarly journals Hydrogen isotopic anomalies in extraterrestrial organic matter: role of cosmic ray irradiation and implications for UCAMMs

2019 ◽  
Vol 627 ◽  
pp. A122 ◽  
Author(s):  
B. Augé ◽  
E. Dartois ◽  
J. Duprat ◽  
C. Engrand ◽  
G. Slodzian ◽  
...  
Keyword(s):  
Organic Matter ◽  
Infrared Spectroscopy ◽  
Spatial Scale ◽  
Secondary Ion Mass Spectrometry ◽  
Isotopic Fractionation ◽  
Cosmic Ray ◽  
High Energy ◽  
Galactic Cosmic Rays ◽  
Ex Situ

Context. Micrometeorites represent, at timescales shorter than a few million years, the dominant source of extraterrestrial matter at the surface of the Earth. Analyses of ultracarbonaceous micrometeorites recovered from Antarctica, known as UCAMMs reveal an exceptionally N-rich organic matter associated with spatially extended high D enrichments. Experiments show that this specific organic matter might have been formed in the outer solar system by energetic irradiation of N-rich icy surfaces. Aims. We experimentally investigate the hydrogen isotopic fractionation resulting from irradiation of normal and D-rich N2-CH4 ices by high energy ions, simulating the exposition to Galactic cosmic rays of icy bodies surfaces orbiting at large heliocentric distances. Methods. Films of N2-CH4 ices and a N2-CH4/CD4/N2-CH4 “sandwich” ice were exposed to 129Xe13+ ion beams at 92 and 88 MeV. The chemical evolution of the samples was monitored using in situ Fourier transform infrared spectroscopy. After irradiation, targets were annealed to room temperature. The solid residues of the whole process left after ice sublimation were characterized in situ by infrared spectroscopy, and the hydrogen isotopic composition measured ex situ by imaging secondary ion mass spectrometry at the sub-micron scale (NanoSIMS). Results. Irradiation leads to the formation of new molecules and radicals. After annealing, the resulting poly-HCN-like macro-molecular residue exhibits an infrared spectrum close to that of UCAMMs. The residue resulting from irradiation of N2-CH4 ices does not exhibit a significant deuterium enrichment comparable to that found in extraterrestrial organic matter. The residue formed by irradiation of D-rich ices shows the formation of isotopic heterogeneities with localised hotspots and an extended contribution likely due to the diffusion of the radiolytic products from the D-rich layer. Conclusions. These results show that high-energy cosmic ray irradiation does not induce the large hydrogen isotopic fractionation observed at small spatial scale in interplanetary organics. By contrast, large D/H ratio heterogeneities at the sub-micron spatial scale in extraterrestrial organic matter can result from isotopically heterogeneous ices mixtures (i.e. condensed with different D/H ratios), which were transformed into refractory organic matter upon irradiation.

Ion Beam Study of Early Stages of Growth of GaN films on Sapphire

2002 ◽  
Vol 743 ◽  
Author(s):  
Eugen M. Trifan ◽  
David C. Ingram
Keyword(s):  
Photoelectron Spectroscopy ◽  
Ion Beam ◽  
Ex Situ ◽  
Crystallographic Axis ◽  
In Situ Characterization ◽  
X Ray ◽  
Ion Channeling ◽  
Stages Of Growth ◽  
Early Stages

ABSTRACTAn innovative approach for in-situ characterization has been used in this work to investigate the composition, growth mode, morphology and crystalline ordering of the early stages of growth of GaN films grown on sapphire by MOCVD for substrate temperatures in the range of 450°C to 1050°C. We have performed in-situ characterization by Rutherford Backscattering Spectroscopy (RBS), Ion Channeling, X-ray Photoelectron Spectroscopy (XPS), and Low Energy Electron Diffraction. Ex-situ the films have been characterized by Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and thickness profilometry. The films have been grown in an in-house designed and build MOCVD reactor that is attached by UHV lines to the analysis facilities. RBS analysis indicated that the films have the correct stoichiometry, have variable thickness and for low substrate temperature completely cover the substrate while for temperatures 850°C and higher islands are formed that may cover as few as 5 percent of the substrate. From Ion Channeling and LEED we have determined the crystallographic phase to be wurtzite. The crystalline quality increases with higher deposition temperature and with thickness. The films are epitaxialy grown with the <0001> crystallographic axis and planes of the GaN films aligned with the sapphire within 0.2 degrees.

The pyrolysis of precursors for GaAs MOCVD studied by in-situ and ex-situ Fourier transform infrared spectroscopy

1992 ◽  
Vol 124 (1-4) ◽  
pp. 10-15 ◽  
Author(s):  
S.R. Armstrong ◽  
R.D. Hoare ◽  
M.E. Pemble ◽  
I.M. Povey ◽  
A. Stafford ◽  
...  
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Fourier Transform Infrared Spectroscopy ◽  
Fourier Transform Infrared ◽  
Ex Situ

Excimer laser cleaning, annealing, and ablation of β–SiC

1989 ◽  
Vol 4 (6) ◽  
pp. 1480-1490 ◽  
Author(s):  
Pehr E. Pehrsson ◽  
Ray Kaplan
Keyword(s):  
Excimer Laser ◽  
Photoelectron Spectroscopy ◽  
Ex Situ ◽  
Carbon Surface ◽  
Laser Exposure ◽  
Electron Loss ◽  
Bulk Heating ◽  
Surface Contaminants ◽  
Excimer Laser Irradiation

The effects of ArF excimer laser irradiation on β–SiC in UHV were examined for a variety of laser intensities and pulse densities. The samples were analyzed in situ with Auger and electron loss spectroscopies, and ex situ with x-ray photoelectron spectroscopy. With progressively higher laser intensities, the SiC surface was initially cleaned of carbon and oxygen surface contaminants, and the Si–LVV Auger lineshape changed from the oxide to the carbide. Still higher laser intensities then partially reordered the surface. A carbon surface layer developed, and the C-KLL lineshape transformed from carbidic to graphitic. Finally, the surface segregated into an almost pure Si layer and an underlying carbon-rich layer, followed by ablation and pitting. Bulk heating during laser exposure may enhance reordering of sputtered or implanted material.

scholarly journals CO2 Reduction to Propanol by Copper Foams: A Pre- and Post-Catalysis Study

2020 ◽  
Author(s):  
Jennifer A. Rudd ◽  
Ewa Kazimierska ◽  
Louise B. Hamdy ◽  
Odin Bain ◽  
Sunyhik Ahn ◽  
...  
Keyword(s):  
Carbon Dioxide ◽  
Photoelectron Spectroscopy ◽  
Carbon Capture ◽  
Surface Composition ◽  
Co2 Reduction ◽  
Structural Rearrangement ◽  
Copper Electrode ◽  
Ex Situ ◽  
X Ray ◽  
Copper Electrodes

The utilization of carbon dioxide is a major incentive for the growing field of carbon capture. Carbon dioxide could be an abundant building block to generate higher value products. Herein, we describe the use of porous copper electrodes to catalyze the reduction of carbon dioxide into higher value products such as ethylene, ethanol and, notably, propanol. For <i>n</i>-propanol production, faradaic efficiencies reach 4.93% at -0.83 V <i>vs</i> RHE, with a geometric partial current density of -1.85 mA/cm<sup>2</sup>. We have documented the performance of the catalyst in both pristine and urea-modified foams pre- and post-electrolysis. Before electrolysis, the copper electrode consisted of a mixture of cuboctahedra and dendrites. After 35-minute electrolysis, the cuboctahedra and dendrites have undergone structural rearrangement. Changes in the interaction of urea with the catalyst surface have also been observed. These transformations were characterized <i>ex-situ</i> using scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. We found that alterations in the morphology, crystallinity, and surface composition of the catalyst led to the deactivation of the copper foams.

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