scholarly journals Evaluation of the electrochemical performance of Ag containing AAO layers after extended exposure to a model corrosive medium

2020 ◽  
Vol 10 (4) ◽  
pp. 317-334
Author(s):  
Stephan V. Kozhukharov ◽  
Christian Girginov ◽  
Denitsa Kiradzhiyska ◽  
Aleksander Tsanev ◽  
Georgy Avdeev
Keyword(s):  
Corrosive Medium ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Barrier Properties ◽  
Anodized Aluminum ◽  
Anodized Aluminum Oxide ◽  
X Ray ◽  
Protective Layers ◽  
Research Activities

The coating procedure appears to be an indispensable finishing stage in the production of Al based industrial products, engineering facilities and equipment. For this reason, there is an ever-increasing interest towards the elaboration of reliable corrosion protective layers with apparent coverage, adhesion, and barrier properties. In this sense, both the for­ma­ti­on of anodized aluminum oxide (AAO) layer and its further modification with silver enable the elaboration of advanced (Al-O-Ag) films with extended beneficial charac­te­ris­tics. The present research activities are aimed at the determination of the corrosion pro­tective properties of electrochemically synthesized Al-O-Ag layers on the technically pure AA1050 alloy. The structures and compositions of the obtained Al-O-Ag layers were characterized by X-ray diffractometry (XRD) and X-ray photoelectron spectroscopy (XPS). The research activities were accomplished by means of two independent electrochemical characteri­za­tion methods: electrochemical impedance spectroscopy (EIS) and potentio­dynamic scan­ning (PDS). The electrochemical measurements were performed after 24, 168 and 672 hours of exposure to 3.5 % NaCl solution used as a model corrosive medium (MCM), in order to determine the barrier properties and durability of the elaborated Al-O-Ag layers. The analysis of the obtained results has undoubtedly shown that the proposed electro­chemical Al-O-Ag layer formation can successfully be used for the creation of self-standing layers with apparent corrosion protective properties. Besides, Al-O-Ag system can be used as a basis for development of efficient protective layers suitable for application in biologically contami­nated media.

scholarly journals Disposable and Low-Cost Electrode Based on Graphene Paper-Nafion-Bi Nanostructures for Ultra-Trace Determination of Pb(II) and Cd(II)

Nanomaterials ◽  
2020 ◽  
Vol 10 (8) ◽  
pp. 1620
Author(s):  
Antonino Scandurra ◽  
Francesco Ruffino ◽  
Mario Urso ◽  
Maria Grazia Grimaldi ◽  
Salvo Mirabella
Keyword(s):  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Low Cost ◽  
Anodic Stripping Voltammetry ◽  
Analytical Performance ◽  
X Ray ◽  
Bismuth Nanoparticles ◽  
Graphene Paper ◽  
Ultra Trace

There is a huge demand for rapid, reliable and low-cost methods for the analysis of heavy metals in drinking water, particularly in the range of sub-part per billion (ppb). In the present work, we describe the preparation, characterization and analytical performance of the disposable sensor to be employed in Square Wave Anodic Stripping Voltammetry (SWASV) for ultra-trace simultaneous determination of cadmium and lead. The electrode consists of graphene paper-perfluorosulfonic ionomer-bismuth nano-composite material. The electrode preparation implies a key step aimed to enhance the Bi3+ adsorption into nafion film, prior to the bismuth electro-deposition. Finely dispersed bismuth nanoparticles embedded in the ionomer film are obtained. The electrode was characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Atomic Force Microscopy (AFM), X-ray Photoelectron Spectroscopy (XPS) and Electrochemical Impedance Spectroscopy (EIS). The electrode shows a linear response in the 5–100 ppb range, a time-stability tested up to almost three months, and detection limits up to 0.1 ppb for both Pb2+ and Cd2+. The electrode preparation method is simple and low in cost and the obtained analytical performance is very competitive with the state of art for the SWASV determination of Pb2+ and Cd2+ in solution.

scholarly journals Synergistic Effects of Fe2O3 Nanotube/Polyaniline Composites for an Electrochemical Supercapacitor with Enhanced Capacitance

Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1557
Author(s):  
Farkhod Azimov ◽  
Jihee Kim ◽  
Seong Min Choi ◽  
Hyun Min Jung
Keyword(s):  
Electrode Materials ◽  
High Efficiency ◽  
Electrochemical Impedance ◽  
Synergistic Effects ◽  
Structural Development ◽  
Anodized Aluminum ◽  
Anodized Aluminum Oxide ◽  
Inner Diameter ◽  
Polyaniline Composites ◽  
Fe2o3 Nanotubes

α-Fe2O3, which is an attractive material for supercapacitor electrodes, has been studied to address the issue of low capacitance through structural development and complexation to maximize the use of surface pseudocapacitance. In this study, the limited performance of α-Fe2O3 was greatly improved by optimizing the nanotube structure of α-Fe2O3 and its combination with polyaniline (PANI). α-Fe2O3 nanotubes (α-NT) were fabricated in a form in which the thickness and inner diameter of the tube were controlled by Fe(CO)5 vapor deposition using anodized aluminum oxide as a template. PANI was combined with the prepared α-NT in two forms: PANI@α-NT-a enclosed inside and outside with PANI and PANI@α-NT-b containing PANI only on the inside. In contrast to α-NT, which showed a very low specific capacitance, these two composites showed significantly improved capacitances of 185 Fg−1 for PANI@α-NT-a and 62 Fg−1 for PANI@α-NT-b. In the electrochemical impedance spectroscopy analysis, it was observed that the resistance of charge transfer was minimized in PANI@α-NT-a, and the pseudocapacitance on the entire surface of the α-Fe2O3 nanotubes was utilized with high efficiency through binding and conductivity improvements by PANI. PANI@α-NT-a exhibited a capacitance retention of 36% even when the current density was increased 10-fold, and showed excellent stability of 90.1% over 3000 charge–discharge cycles. This approach of incorporating conducting polymers through well-controlled nanostructures suggests a solution to overcome the limitations of α-Fe2O3 electrode materials and improve performance.

scholarly journals An Insight into Chemistry and Structure of Colloidal 2D-WS2 Nanoflakes: Combined XPS and XRD Study

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Xrd Analysis ◽  
Crystal Habit ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Morphological Evaluation ◽  
Rational Understanding ◽  
Structural Inspection

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.

Ternary Composite of Molybdenum Disulfide-Graphene Oxide-Polyaniline for Supercapacitor

2021 ◽  
Author(s):  
Ke Qu ◽  
Yuqi Bai ◽  
Miao Deng
Keyword(s):  
Graphene Oxide ◽  
Molybdenum Disulfide ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Light Emitting Diode ◽  
Rate Capability ◽  
Energy Storage And Conversion ◽  
Carbon Paper ◽  
Power Sources ◽  
X Ray

Abstract The ever-increasing need for small and lightweight power sources for use in portable or wearable electronic devices has spurred the development of supercapacitors as a promising energy storage and conversion system. In this work, a simple, facile and easy-to-practice method has been developed to employ carbon paper (CP) as the support to coat molybdenum disulfide (MoS2) and graphene oxide (GO), followed by electrodeposition of polyaniline (PANI) to render CP/MoS2-GO-PANI. The preparation parameters, such as amounts of MoS2, GO and number of aniline electropolymerization cycles, have been optimized to render CP/MoS2-GO-PANI the best capacitive performance. The as-prepared optimal CP/MoS2-GO-PANI is characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and X-ray photoelectron spectroscopy. The supercapacitive properties of CP/MoS2-GO-PANI as an electrode have been evaluated electrochemically via cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy testing. CP/MoS2-GO-PANI delivers a specific capacitance of 255.1 F/g at 1.0 A/g and exhibits excellent rate capability under larger current densities. Moreover, a symmetrical supercapacitor is assembled and three are connected in series to power a light-emitting diode for ~15 minutes, demonstrating the promising application potential of CP/MoS2-GO-PANI-based supercapacitor.

A Two-step Electrodeposition of Pd-Cu/Cu2O Nanocomposite on FTO Substrate for Non-enzymatic Hydrogen Peroxide Sensor

2021 ◽  
Vol 17 ◽  
Author(s):  
Ke Huan ◽  
Li Tang ◽  
Dongmei Deng ◽  
Huan Wang ◽  
Xiaojing Si ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Cyclic Voltammetry ◽  
Photoelectron Spectroscopy ◽  
Chemical Structure ◽  
Pd Nanoparticles ◽  
Optimal Conditions ◽  
Potential Oscillation ◽  
X Ray Diffraction ◽  
X Ray

Background: Hydrogen peroxide (H2O2) is a common reagent in the production and living, but excessive H2O2 may enhance the danger to the human body. Consequently, it is very important to develop economical, fast and accurate techniques for detecting H2O2. Methods: A simple two-step electrodeposition process was applied to synthesize Pd-Cu/Cu2O nanocomposite for non-enzymatic H2O2 sensor. Cu/Cu2O nanomaterial was firstly electrodeposited on FTO by potential oscillation technique, and then Pd nanoparticles were electrodeposited on Cu/Cu2O nanomaterial by cyclic voltammetry. The chemical structure, component, and morphology of the synthesized Pd-Cu/Cu2O nanocomposite were characterized by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The electrochemical properties of Pd-Cu/Cu2O nanocomposite were studied by cyclic voltammetry and amperometry. Results: Under optimal conditions, the as-fabricated sensor displayed a broad linear range (5-4000 µM) and low detection limit (1.8 µM) for the determination of H2O2. The proposed sensor showed good selectivity and reproducibility. Meanwhile, the proposed sensor has been successfully applied to detect H2O2 in milk. Conclusion: The Pd-Cu/Cu2O/FTO biosensor exhibits excellent electrochemical activity for H2O2 reduction, which has great potential application in the field of food safety.

scholarly journals Enhancement of the cerium oxide primer layers deposited on AA2024-T3 aircraft alloy by preliminary Enhancement of the cerium oxide primer layers deposited on AA2024-T3 aircraft alloy by preliminary anodization

2018 ◽  
Author(s):  
Stephan V. Kozhukharov ◽  
Christian Girginov
Keyword(s):  
Cerium Oxide ◽  
Electrochemical Impedance ◽  
Protective Coatings ◽  
Salt Spray ◽  
Neutral Salt ◽  
Anodized Aluminum ◽  
Cross Sectional ◽  
Anodized Aluminum Oxide ◽  
Linear Voltammetry ◽  
And Performance

<p class="PaperAbstract"><span lang="EN-US">The possibility for combination between Anodized Aluminum Oxide (AAO) and Cerium Oxide Primer Layer (CeOPL) for elaboration of efficient protective coatings for AA2024-T3 aircraft alloy is proposed in the present research. The combined AAO/CeOPL coating characterizations include Electrochemical Impedance Spectroscopy (EIS) combined with Linear Voltammetry (LVA), for extended times (until 2520 hours) to a model corrosive medium (3.5% NaCl). Topographical and cross-sectional (SEM and EDX) observations were performed in order to determine the AAO/CeOPL film thickness and composition. The AAO/CeOPL layer durability tests were confirmed by standard Neutral Salt Spray (NSS). The data analysis from all the used measurement methods has undoubtedly shown that the presence of AAO film significantly improves the cerium oxide primer layer (CeOPL) protective properties and performance. </span></p>

scholarly journals Organosilane-functionalization of nanostructured indium tin oxide films

2016 ◽  
Vol 6 (6) ◽  
pp. 20160056 ◽  
Author(s):  
R. Pruna ◽  
F. Palacio ◽  
M. Martínez ◽  
O. Blázquez ◽  
S. Hernández ◽  
...  
Keyword(s):  
Surface Area ◽  
Indium Tin Oxide ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Annealing Treatment ◽  
Electrochemical Analysis ◽  
Cyclic Voltammograms ◽  
X Ray ◽  
Chip Technology ◽  
Significant Difference

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.

scholarly journals Graphitic Nitrogen in Carbon Catalysts Important for the Reduction of Nitrite Revealed by 15N NMR Spectroscopy at Natural Abundance

2020 ◽  
Author(s):  
Zheng Chen ◽  
Aleksander Jaworski ◽  
Jianhong Chen ◽  
Tetyana Budnyak ◽  
Ireneusz Szewczyk ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Reduction Reaction ◽  
Nitrite Reduction ◽  
15N Nmr ◽  
Carbon Catalyst ◽  
X Ray ◽  
Wide Range ◽  
Alkaline Conditions

Metal-free nitrogen-doped carbon is considered as a green functional material, but the structural determination of the atomic positions of nitrogen remains challenging. We recently demonstrated that directly-excited solid state <sup>15</sup>N NMR (ssNMR) spectroscopy is a powerful tool for the determination of such positions in an N-doped carbon at natural <sup>15</sup>N isotope abundance. Here we present a green chemistry approach to the synthesis of N-doped carbon using cellulose as precursor, and a study of the catalytic properties and atomic structures of the related catalyst. The N-doped carbon (NH<sub>3</sub>) was obtained by oxidation of cellulose with HNO<sub>3</sub> followed by ammonolysis at 800°C. It had a N content of 6.5 wt.% and a surface area of 557 m<sup>2 </sup>g<sup>–1</sup>, and <sup>15</sup>N ssNMR spectroscopy provided evidence for graphitic nitrogen besides of regular pyrrolic and pyridinic nitrogen. This structure determination enabled probing the role of graphitic nitrogen for electrocatalytic reactions, such as the hydrogen evolution reaction (HER), oxygen evolution reaction (OER), and nitrite reduction reaction. The N-doped carbon catalyst (NH<sub>3</sub>) had higher electrocatalytic activities in OER and HER under alkaline conditions and a higher activity for nitrite reduction, as compared with a catalyst prepared by carbonization of the HNO<sub>3</sub>-treated cellulose in N<sub>2</sub>. The electrocatalytic selectivity for nitrite reduction of the N-doped carbon catalyst (NH<sub>3</sub>) was directly related to the graphitic nitrogen functions. Complementary structural analysis by means of <sup>13</sup>C and <sup>1</sup>H ssNMR, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and low-temperature N<sub>2 </sub>adsorption were preformed and provided support to the findings. The results show that directly-excited <sup>15</sup>N ssNMR at natural <sup>15</sup>N abundance is generally capable to provide information on N-doped carbon materials, and it is expected that the approach can be applied to a wide range of solids with an intermediate amount of N atoms.

Sign in / Sign up

Export Citation Format

Share Document