The electrochemical behaviour of protic quaternary amine based room-temperature ionic liquid N2210(OTf) at negatively and positively polarized micro-mesoporous carbon electrode investigated by in situ X-ray photoelectron spectroscopy, in situ mass-spectroscopy, cyclic voltammetry and electrochemical impedance spectroscopy methods

2021 ◽  
pp. 115561
Author(s):  
Jaanus Kruusma ◽  
Arvo Tõnisoo ◽  
Rainer Pärna ◽  
Thomas Thomberg ◽  
Mati Kook ◽  
...  
Keyword(s):  
Cyclic Voltammetry ◽  
Photoelectron Spectroscopy ◽  
Mesoporous Carbon ◽  
Room Temperature ◽  
Electrochemical Impedance ◽  
Electrochemical Behaviour ◽  
Carbon Electrode ◽  
Quaternary Amine ◽  
X Ray

scholarly journals in Situ X-ray Photoelectron Spectroscopic and Electrochemical Studies of the Bromide Anions Dissolved in 1-Ethyl-3-Methyl Imidazolium Tetrafluoroborate

Nanomaterials ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 304 ◽  
Author(s):  
Jaanus Kruusma ◽  
Arvo Tõnisoo ◽  
Rainer Pärna ◽  
Ergo Nõmmiste ◽  
Enn Lust
Keyword(s):  
Photoelectron Spectroscopy ◽  
Mesoporous Carbon ◽  
Residual Water ◽  
Carbon Electrode ◽  
Xps Spectra ◽  
X Ray ◽  
In Situ Xps ◽  
Vacuum Interface ◽  
Photoelectron Peak

Influence of electrode potential on the electrochemical behavior of a 1-ethyl-3-methylimidazolium tetrafluoroborate (EMImBF4) solution containing 5 wt % 1-ethyl-3-methylimidazolium bromide (EMImBr) has been investigated using electrochemical and synchrotron-initiated high-resolution in situ X-ray photoelectron spectroscopy (XPS) methods. Observation of the Br 3d5/2 in situ XPS signal, collected in a 5 wt % EMImBr solution at an EMImBF4–vacuum interface, enabled the detection of the start of the electrooxidation process of the Br- anion to Br3- anion and thereafter to the Br2 at the micro-mesoporous carbon electrode, polarized continuously at the high fixed positive potentials. A new photoelectron peak, corresponding to B–O bond formation in the B 1s in situ XPS spectra at E ≤ –1.17 V, parallel to the start of the electroreduction of the residual water at the micro-mesoporous carbon electrode, was observed and is discussed. The electroreduction of the residual water caused a reduction in the absolute value of binding energy vs. potential plot slope twice to ca. dBE dE-1 = –0.5 eV V-1 at E ≤ –1.17 V for C 1s, N 1s, B 1s, F 1s, and Br 3d5/2 photoelectrons.

scholarly journals The Electrochemical Behaviour of Quaternary Amine-Based Room-Temperature Ionic Liquid N4111(TFSI)

Catalysts ◽  
2021 ◽  
Vol 11 (11) ◽  
pp. 1315
Author(s):  
Jaanus Kruusma ◽  
Arvo Tõnisoo ◽  
Rainer Pärna ◽  
Thomas Thomberg ◽  
Mati Kook ◽  
...  
Keyword(s):  
Ionic Liquid ◽  
Room Temperature ◽  
Electrochemical Impedance ◽  
Electrochemical Behaviour ◽  
Room Temperature Ionic Liquid ◽  
Potential Range ◽  
Quaternary Amine ◽  
Xps Spectra ◽  
Strong Adsorption

In this study, we used the in situ X-ray photoelectron spectroscopy (XPS), in situ mass spectroscopy, cyclic voltammetry and electrochemical impedance spectroscopy methods, for the first time, in a detailed exploration of the electrochemical behaviour of a quaternary amine cation-based room-temperature ionic liquid, butyl-trimethyl-ammonium bis(trifluoromethylsulfonyl)imide (N4111(TFSI)), at the negatively and positively polarised molybdenum carbide-derived micro-mesoporous carbon (mmp-C(Mo2C)) electrodes that can be used as high surface area supporting material for electrocatalysts. The shapes of the C 1s, N 1s, O 1s, F 1s and S 2p XPS spectra were stable for N4111(TFSI) within a very wide potential range. The XPS data indicated the non-specific adsorption character of the cations and anions in the potential range from −2.00 V to 0.00 V. Thus, this region can be used for the detailed analysis of catalytic reaction mechanisms. We observed strong adsorption from 0.00 V to 1.80 V, and at E > 1.80 V, very strong adsorption of the N4111(TFSI) at the mmp-C(Mo2C) took place. At more negative potentials than −2.00 V, the formation of a surface layer containing both N4111+ cations and TFSI− anions was established with the formation of various gaseous compounds. Collected data indicated the electrochemical instability of the N4111+ cation at E < −2.00 V.

scholarly journals Characterization of Ti/SnO2 Interface by X-ray Photoelectron Spectroscopy

Nanomaterials ◽  
2022 ◽  
Vol 12 (2) ◽  
pp. 202
Author(s):  
Miranda Martinez ◽  
Anil R. Chourasia
Keyword(s):  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Chemical Interaction ◽  
Photoelectron Spectra ◽  
X Ray ◽  
Increasing Trend ◽  
Substrate Temperatures ◽  
Beam Technique

The Ti/SnO2 interface has been investigated in situ via the technique of x-ray photoelectron spectroscopy. Thin films (in the range from 0.3 to 1.1 nm) of titanium were deposited on SnO2 substrates via the e-beam technique. The deposition was carried out at two different substrate temperatures, namely room temperature and 200 °C. The photoelectron spectra of tin and titanium in the samples were found to exhibit significant differences upon comparison with the corresponding elemental and the oxide spectra. These changes result from chemical interaction between SnO2 and the titanium overlayer at the interface. The SnO2 was observed to be reduced to elemental tin while the titanium overlayer was observed to become oxidized. Complete reduction of SnO2 to elemental tin did not occur even for the lowest thickness of the titanium overlayer. The interfaces in both the types of the samples were observed to consist of elemental Sn, SnO2, elemental titanium, TiO2, and Ti-suboxide. The relative percentages of the constituents at the interface have been estimated by curve fitting the spectral data with the corresponding elemental and the oxide spectra. In the 200 °C samples, thermal diffusion of the titanium overlayer was observed. This resulted in the complete oxidation of the titanium overlayer to TiO2 upto a thickness of 0.9 nm of the overlayer. Elemental titanium resulting from the unreacted overlayer was observed to be more in the room temperature samples. The room temperature samples showed variation around 20% for the Ti-suboxide while an increasing trend was observed in the 200 °C samples.

scholarly journals Investigation of Electrochemical Behaviour of Quercetin on the Modified Electrode Surfaces with Procaine and Aminophenyl in Non-Aquous Medium

2008 ◽  
Vol 5 (3) ◽  
pp. 539-550 ◽  
Author(s):  
Ibrahim Ender Mulazimoglu ◽  
Erdal Ozkan
Keyword(s):  
Cyclic Voltammetry ◽  
Electrochemical Impedance Spectroscopy ◽  
Impedance Spectroscopy ◽  
Glassy Carbon ◽  
Electrode Surface ◽  
Electrochemical Impedance ◽  
Electrochemical Behaviour ◽  
Carbon Electrode ◽  
Amine Group ◽  
Tetrabutylammonium Tetrafluoroborate

In this study, cyclic voltammetry and electrochemical ımpedance spectroscopy have been used to investigate the electrochemical behaviour of quercetin (3,3′,4′,5,7-pentahydroxyflavone) on the procaine and aminophenyl modified electrode. The modification of procaine and aminophenyl binded electrode surface with quercetin was performed in +0,3/+2,8 V (for procaine) and +0,4/+1,5 V (for aminophenyl) potential range using 100 mV s-1scanning rate having 10 cycle. A solution of 0.1 M tetrabutylammonium tetrafluoroborate in acetonitrile was used as a non-aquous solvent. For the modification process a solution of 1 mM quercetin in 0.1 M tetrabutylammonium tetrafluoroborate was used. In order to obtain these two surface, a solution of 1 mM procaine and 1 mM nitrophenyl diazonium salt in 0.1 M tetrabutylammonium tetrafluoroborate was used. By using these solutions bare glassy carbon electrode surface was modified. Nitrophenyl was reduced to amine group in 0.1 M HCl medium on the nitrophenyl modified glassy carbon elelctrode surface. Procaine modified glassy carbon electrode surface was quite electroactive. Although nitrophenyl modified glassy carbon elelctrode surface was electroinactive, it was activated by reducing nitro group into amine group. For the characterization of the modified surface 1 mM ferrocene in 0.1 M tetrabutylammonium tetrafluoroborate for cyclic voltammetry and 1 mM ferricyanide/ferrocyanide (1:1) mixture in 0,1 M KCl for electrochemical impedance spectroscopy were used.

Study of Ta as a Diffusion Barrier in Cu/SiO2 Structure

2000 ◽  
Vol 612 ◽  
Author(s):  
J. S. Pan ◽  
A. T. S. Wee ◽  
C. H. A. Huan ◽  
J. W. Chai ◽  
J. H. Zhang
Keyword(s):  
Photoelectron Spectroscopy ◽  
Electron Spectroscopy ◽  
Auger Electron ◽  
Room Temperature ◽  
Depth Profiling ◽  
Oxide Formation ◽  
X Ray ◽  
Chemical States ◽  
The Stability

AbstractTantalum (Ta) thin films of 35 nm thickness were investigated as diffusion barriers as well as adhesion-promoting layers between Cu and SiO2 using X-ray diffractometry (XRD), Scanning electron microscopy (SEM), Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). After annealing at 600°C for 1h in vacuum, no evidence of interdiffusion was observed. However, XPS depth profiling indicates that elemental Si appears at the Ta/SiO2 interface after annealing. In-situ XPS studies show that the Ta/SiO2 interface was stable until 500°C, but about 32% of the interfacial SiO2 was reduced to elemental Si at 600°C. Upon cooling to room temperature, some elemental Si recombined to form SiO2 again, leaving only 6.5% elemental Si. Comparative studies on the interface chemical states of Cu/SiO2 and Ta/SiO2 indicate that the stability of the Cu/Ta/SiO2/Si system may be ascribed to the strong bonding of Ta and SiO2, due to the reduction of SiO2 through Ta oxide formation.

CuWO4 Nanoparticles: Investigation of Dielectric, Electrochemical Behaviour and Photodegradation of Pharmaceutical Waste

2019 ◽  
Vol 19 (11) ◽  
pp. 7026-7034 ◽  
Author(s):  
M. Thiruppathi ◽  
M. Vahini ◽  
P. Devendran ◽  
M. Arunpandian ◽  
K. Selvakumar ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Room Temperature ◽  
Electrochemical Impedance ◽  
Electrochemical Behaviour ◽  
Diclofenac Sodium ◽  
X Ray Diffraction ◽  
Sem Images ◽  
X Ray ◽  
Transmission Electron ◽  
Pharmaceutical Waste

The hydrothermally synthesized CuWO4 nanoparticles (NPs) were characterized with different analysis such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM), Energy Dispersive X-ray Spectroscopy (EDX), Cyclic Voltammetry (CV), UV-Visible and Photoluminescence (PL) analysis. The prepared CuWO4 NPs were examined with Electrochemical Impedance Spectroscopy (EIS). SEM images show that CuWO4 NPs are highly spherical shaped morphology and porous in nature. The optical band gap of prepared CuWO4 NPs is found to be 2.12 eV. Photodegradation of diclofenac sodium (DFS) (medical waste) in the aqueous medium with CuWO4 NPs under visible light irradiation shows 98% degradation. The CuWO4 NPs was stable up to 5th cycle it can be used as a reusable photocatalyst for the DFS degradation. The electrical conductivity and dielectric properties of the CuWO4 NPs at room temperature is analyzed by EIS studies. The bulk conductivity value of the prepared nanoparticles is 1.477×10-5 S/cm at room temperature. The conductivity of CuWO4 NPs is found to be due to electrons movement. The CuWO4 NPs shows higher photocatalytic and electrocatalytic activity for decomposition of DFS and methanol electro-oxidation in alkaline medium respectively.

In situ investigation of M/CuO interface (M is Ti, V, Cr or Mn) by X-ray photoelectron spectroscopy

2015 ◽  
Vol 29 (04) ◽  
pp. 1530002 ◽  
Author(s):  
A. R. Chourasia ◽  
Jacob Stahl
Keyword(s):  
Metal Oxide ◽  
Copper Oxide ◽  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Chemical Reactivity ◽  
Spectral Features ◽  
Metallic Oxide ◽  
X Ray ◽  
Elemental Copper

The technique of X-ray photoelectron spectroscopy has been used to investigate the chemical reactivity at the metal/ CuO interfaces. Thin films of the metallic overlayer (0.5 nm, 1.0 nm and 2.0 nm thickness) were deposited on copper oxide substrates at room temperature. In situ characterization of the interfaces has been performed. The 2p core level regions of the metals have been investigated. The spectral features show considerable reactivity at the interfaces. The core level peaks of the metal are observed to be shifted to the high BE energy side with the appearance of satellites. The spectral data confirm the formation of the metallic oxide at the interface. The satellite structure in the copper region is observed to disappear and the spectral features are found to approach those of elemental copper. The room temperature deposition of the metal on copper oxide therefore results in the reduction of copper oxide to elemental copper followed by the oxidation of the metal. The interface is found to consist of a mixture of metal oxide and elemental copper. The 2.0 nm samples were annealed. These samples show the diffusion of copper oxide through the overlayer. The metal reacts with this diffusing oxide to form metallic oxide. The interface is found to consist of a mixture of unreacted metal, the metal oxide, and elemental copper. The amount of the unreacted metal varied between 0% and 40% and can be controlled by the processing conditions. The investigation shows room temperature chemical reactivity at the metal/ CuO interface and provides a new method of preparing sub-nano-oxide films.

scholarly journals Room-Temperature Reaction of Oxygen with Gold: An In situ Ambient-Pressure X-ray Photoelectron Spectroscopy Investigation

2010 ◽  
Vol 132 (9) ◽  
pp. 2858-2859 ◽  
Author(s):  
Peng Jiang ◽  
Soeren Porsgaard ◽  
Ferenc Borondics ◽  
Mariana Köber ◽  
Alfonso Caballero ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Ambient Pressure ◽  
Temperature Reaction ◽  
X Ray

Metal-Ceramic Interfacial Reactions: The Copper-Cordierite and Titanium-Cordierite Systems.

1988 ◽  
Vol 119 ◽  
Author(s):  
M. Bortz ◽  
F. S. Ohuchi
Keyword(s):  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Interfacial Reactions ◽  
Comprehensive Treatment ◽  
Interfacial Chemistry ◽  
Ceramic Substrates ◽  
Copper Diffusion ◽  
X Ray ◽  
Metal Ceramic

AbstractInterfacial reactions between either copper or titanium and cordierite-based (2MgO.2Al2O3.5SiO2) ceramic substrates are probed using X-ray Photoelectron Spectroscopy (XPS). Room temperature reactions are found to be strongly dependent on interfacial chemistry; while copper reacts weakly with the cordierite surface, titanium strongly reduces the Si-O and Al-O substrate bonds. Behavior during subsequent “in situ” annealing is dependent on substrate morphology. On amorphous cordierite films copper remains nonreactive while titanium dissociates remaining Si-O and Al-O bonds, forming a low valency Ti1+ oxide. On crystalline cordierite substrates copper diffuses rapidly upon annealing while titanium reduces substrate bonds forming a high valency Ti3+ oxide. Furthermore, thin 5Å Ti interlayers prevent copper diffusion at temperatures below 650°C. This study represents the first comprehensive treatment of the interfacial reactions in metal-multicomponent ceramic systems.

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