X-Ray Photoelectron Spectroscopy (XPS) and Electrochemical Analysis of the Irradiation Effects on Passive Film of Stainless Steels

1992 ◽  
Vol 111-112 ◽  
pp. 621-628
Author(s):  
G. Capobianco ◽  
A. Glisenti ◽  
G. Granozzi ◽  
G. Palma
2016 ◽  
Vol 6 (6) ◽  
pp. 20160056 ◽  
Author(s):  
R. Pruna ◽  
F. Palacio ◽  
M. Martínez ◽  
O. Blázquez ◽  
S. Hernández ◽  
...  

Fabrication and organosilane-functionalization and characterization of nanostructured ITO electrodes are reported. Nanostructured ITO electrodes were obtained by electron beam evaporation, and a subsequent annealing treatment was selectively performed to modify their crystalline state. An increase in geometrical surface area in comparison with thin-film electrodes area was observed by atomic force microscopy, implying higher electroactive surface area for nanostructured ITO electrodes and thus higher detection levels. To investigate the increase in detectability, chemical organosilane-functionalization of nanostructured ITO electrodes was performed. The formation of 3-glycidoxypropyltrimethoxysilane (GOPTS) layers was detected by X-ray photoelectron spectroscopy. As an indirect method to confirm the presence of organosilane molecules on the ITO substrates, cyclic voltammetry and electrochemical impedance spectroscopy (EIS) were also carried out. Cyclic voltammograms of functionalized ITO electrodes presented lower reduction-oxidation peak currents compared with non-functionalized ITO electrodes. These results demonstrate the presence of the epoxysilane coating on the ITO surface. EIS showed that organosilane-functionalized electrodes present higher polarization resistance, acting as an electronic barrier for the electron transfer between the conductive solution and the ITO electrode. The results of these electrochemical measurements, together with the significant difference in the X-ray spectra between bare ITO and organosilane-functionalized ITO substrates, may point to a new exploitable oxide-based nanostructured material for biosensing applications. As a first step towards sensing, rapid functionalization of such substrates and their application to electrochemical analysis is tested in this work. Interestingly, oxide-based materials are highly integrable with the silicon chip technology, which would permit the easy adaptation of such sensors into lab-on-a-chip configurations, providing benefits such as reduced size and weight to facilitate on-chip integration, and leading to low-cost mass production of microanalysis systems.


Author(s):  
César Zúñiga-Loyola ◽  
Gabriel Abarca ◽  
Maria Soledad Ureta-Zanartu ◽  
Carolina Aliaga ◽  
Jose Zagal ◽  
...  

Fe phthalocyanine was coordinated to pyridine-modified carbon nanotubes and studied as a catalyst for the oxygen reduction (ORR) and oxygen evolution reactions (OER). X-ray Photoelectron Spectroscopy (XPS), Mössbauer, and Electron...


Author(s):  
Wei Han ◽  
Fengzhou Fang

Abstract The study is to investigate the electropolishing characteristics of 316L stainless steel in a sulfuric acid-free electrolyte of phosphoric acid and glycerol and to explore the possibility of using this eco-friendly electrolyte instead of the widely used sulfuric acid-based electrolyte. The influences of process parameters on polishing effects and the corrosion resistance of electropolished samples are investigated. The experimental results show that the electropolishing temperature and acid concentration are directly related to the mass transport mechanism in the limiting current plateau region. The grain boundaries of workpiece were electrochemically dissolved faster than the grain themselves at the beginning of the electropolishing process because they are more reactive than grains. Moreover, the conventional sulfuric—phosphoric acid electrolyte was also used to electropolish the 316L stainless steel, and the electropolished surfaces were compared with the sulfuric acid-free electrolyte proposed in this study. When the sulfuric acid-free electrolyte was used to electropolish the 316L stainless steel, the X-ray photoelectron spectroscopy (XPS) analysis shows that atomic Cr/Fe ratio of 316L stainless steel was increased from 0.802 to 1.909 after electropolishing process in the sulfuric acid-free electrolyte of phosphoric acid and glycerol. The corrosion resistance of the electropolished 316L stainless steel is studied using electrochemical analysis, and the results are verified experimentally.


Minerals ◽  
2019 ◽  
Vol 9 (3) ◽  
pp. 159 ◽  
Author(s):  
Maoxin Hong ◽  
Xingxing Wang ◽  
Lingbo Wu ◽  
Chaojun Fang ◽  
Xiaotao Huang ◽  
...  

Bioleaching experiments, electrochemical tests, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were conducted to investigate the intermediates transformation of bornite by Leptospirillum ferriphilum and Acidithiobacillus caldus. The bioleaching experimental results showed that the presence of L. ferriphilum and A. caldus significantly accelerated the bornite bioleaching. In addition, the intermediate species of bornite bioleaching with these two kinds of bacteria were similar. Electrochemical analysis indicated that the dissolution of bornite was an acid-consuming process. The results of XRD showed that intermediate species, namely covellite (CuS), mooihoekit (Cu9Fe9S16) and isocubanite (CuFe2S3), were formed during bornite bioleaching, and a mass of elemental sulfur was formed in the late stage of bioleaching. The Cu 2p photoelectron spectrum revealed that Cu was present in the form of Cu (I) during the bornite bioleaching. Additionally, the S 2p3/2 photoelectron spectrum suggested that S2− and S22− were gradually converted to Sn2−/S0, and the formation of elemental sulfur hindered the further dissolution of the bornite.


2015 ◽  
Vol 658 ◽  
pp. 190-194 ◽  
Author(s):  
Siriporn Meeying ◽  
Pinsuda Viravathana ◽  
Atchana Wongchaisuwat ◽  
Siree Tangbunsuk

PdCoNi nanocomposites supported on graphene (PdCoNi/G) have been obtained from chemical reduction of metal catalysts and graphite oxide (GO) with a strong reducing agent, followed by calcination at high temperature under N2 condition, and used for electrooxidation of methanol in direct methanol fuel cell. The morphologies and structural properties of electrocatalysts were examined by scanning electron microscopy (SEM) and X-ray diffraction (XRD). X-ray spectroscopy techniques (X-ray photoelectron spectroscopy XPS) was used to investigate the chemical state of the synthesized catalysts. The results of Pd XPS spectra showed the metallic Pd and PdO phases for precalcined and calcined PdCoNi/G nanocomposite, respectively. The X-ray measurement of Co and Ni displayed the various metallic oxides in synthesized electrocatalysts. For electrochemical analysis, cyclic voltammetry (CV) and chronoamperometry (CA) indicated that the PdCoNi/G nanocomposites enhanced the methanol oxidation, compared to the lower activity in the calcined electrocatalysts.


2014 ◽  
Vol 93 ◽  
pp. 41-49 ◽  
Author(s):  
M.J. Lázaro ◽  
C. Alegre ◽  
M.J. Nieto-Monge ◽  
D. Sebastián ◽  
M.E. Gálvez ◽  
...  

The objective of this work is to study the behavior of Nitrogen-doped carbons as supports of catalysts for the electro-oxidation of methanol. Two carbon materials have been considered: a) carbon xerogels (CXG), highly mesoporous, whose porosity and pore size distribution are easily performed during the synthesis method; b) carbon nanofibers (CNF), which have a high electrical conductivity, good behavior in high temperature conditions and resistance to acid/basic media. Meanwhile, a commercial carbon black (Vulcan XC72R) which is commonly used in manufacturing of electrocatalysts fuel cells was used for comparison. Nitrogen was introduced into the CXG during the synthesis process, what is commonly referred as doping, by including melamine as a reactant. In contrast, N-groups were created over CNF by post-treatment with: ammonia (25%), urea (98%), melamine (99%) and ethylenediamine (99.5%), with a carbon: nitrogen molar ratio 1:0.6. N-containing carbon materials were characterized by elemental analysis, nitrogen adsorption, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), SEM-EDX and TEM to determinate the amount and forms of nitrogen introduced. Pt-catalysts were prepared by the microemulsion method. The influence of the nitrogen doping and functionalization on the catalytic behavior in the electrochemical oxidation of methanol was evaluated by different physicochemical and electrochemical analysis.


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