Characterization of Electrochemical Materials

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Electronic Materials electronicmat	-	-	2020	17 Days	CHF 1000
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Materials materials	3.4	5.2	2008	13.9 Days	CHF 2600

13 pages, 10002 KiB

Open AccessArticle

On the Electrochemically Active Surface Area Determination of Electrodeposited Porous Cu 3D Nanostructures

by Birutė Serapinienė, Laima Gudavičiūtė, Skirmantė Tutlienė, Asta Grigucevičienė, Algirdas Selskis, Jurga Juodkazytė and Rimantas Ramanauskas

Coatings 2023, 13(8), 1335; https://doi.org/10.3390/coatings13081335 - 29 Jul 2023

Cited by 3 | Viewed by 1260

Abstract

Porous 3D Cu layers with the following average parameters: thickness ~35 µm, pore density ~4.0 × 10⁶ cm⁻², and pore sizes ~25 µm were electrodeposited from an acidic sulphate electrolyte, and the suitability of different electrochemically active surface area determination [...] Read more.

Porous 3D Cu layers with the following average parameters: thickness ~35 µm, pore density ~4.0 × 10⁶ cm⁻², and pore sizes ~25 µm were electrodeposited from an acidic sulphate electrolyte, and the suitability of different electrochemically active surface area determination methods for characterising these electrodes was assessed. Structural characterisation of the samples was conducted using SEM and an optical profiler, while electrochemical measurements were performed using cyclic voltammetry and electrochemical impedance spectroscopy. The evaluation of electrochemically active surface area involved the underpotential deposition of Tl and Pb monolayers as well as double-layer capacitance measurements. The results obtained indicate that both methods yield similar results for non-porous Cu electrodes. However, for Cu 3D nanostructures, the evaluation mode significantly influences the results. Double-layer capacitance measurements show significantly higher values for the electrochemically active surface area compared to the underpotential deposition (UPD) technique. The complex spatial structure of the Cu 3D layer hinders the formation of a continuous monolayer during the UPD process, which is the principal reason for the observed differences. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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12 pages, 4288 KiB

Open AccessArticle

Influence of DETA on Thermal and Corrosion Protection Properties of GPTMS-TEOS Hybrid Coatings on Q215 Steel

by Shuanqiang Yang, Zhenzhen Jia, Jinjia Xu and Ruoyu Hong

Coatings 2023, 13(7), 1145; https://doi.org/10.3390/coatings13071145 - 24 Jun 2023

Viewed by 1153

Abstract

High-performance coating could be used to protect steels in engineering. The GPTMS-TEOS hybrid coatings were successfully prepared using (3-glycidoxypropyl) trimethoxysilane (GPTMS) and tetraethylorthosilicate (TEOS) as reaction raw materials and diethylenetriamine (DETA) as both a curing agent and catalyst at room temperature. The hybrid [...] Read more.

High-performance coating could be used to protect steels in engineering. The GPTMS-TEOS hybrid coatings were successfully prepared using (3-glycidoxypropyl) trimethoxysilane (GPTMS) and tetraethylorthosilicate (TEOS) as reaction raw materials and diethylenetriamine (DETA) as both a curing agent and catalyst at room temperature. The hybrid coating contained amorphous SiO₂ and was characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The DETA content of the hybrid coating has a significant impact on the performance of the coating. As the DETA content increases, the thermal stability of the hybrid coating increases at 400–600 °C due to the production of more SiO₂ in the amine-rich state. However, the gelation time decreases dramatically, preventing the hybrid coating from better infiltrating the surface of the steel substrate. In addition, there are not enough silicon hydroxyl groups to bond with the hydroxyl groups on the surface of carbon steel and adhesion is significantly reduced. Therefore, hybrid coatings with a moderate DETA content (NH:epoxy ratio equivalent to 1:1) show the best corrosion resistance, with a third-order magnitude increase in corrosion resistance compared to that of carbon steel. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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20 pages, 6388 KiB

Open AccessArticle

Mixing, Fast and Slow: Assessing the Efficiency of Electronically Conductive Networks in Hard Carbon Anodes

by Manisha Anne Sawhney and Jenny Baker

Coatings 2023, 13(4), 689; https://doi.org/10.3390/coatings13040689 - 28 Mar 2023

Viewed by 2140

Abstract

This work aimed to answer fundamental questions about the optimal processing and formulation of hard carbon electrodes typical of those anticipated in commercial sodium-ion cells. Procedurally simple tests were proposed to compare the effects of slurry mixing energy and conductive additives on the [...] Read more.

This work aimed to answer fundamental questions about the optimal processing and formulation of hard carbon electrodes typical of those anticipated in commercial sodium-ion cells. Procedurally simple tests were proposed to compare the effects of slurry mixing energy and conductive additives on the morphology of and conductive networks in electrodes made with hard carbons from two different manufacturers. Long-range and short-range electronic conductivity was quantified with high repeatability for samples of each hard carbon electrode produced on different days. The most significant changes induced by mixing energy were observed in the electrodes produced without conductive additives, which was found to relate to post-processing particle size. Hard carbon from one source was pulverized by high energy mixing, replacing the electronic effect of conductive additives while increasing pore tortuosity and impedance. These findings recommend evaluating the dry electrode through-resistance as a complement to quantifying pre-cycling impedance to validate mixing protocol and the application of conductive additives in hard carbon electrodes. These procedures can also serve as reliable low-cost methods for quality control at early stages of sodium-ion anode manufacturing. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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14 pages, 6064 KiB

Open AccessArticle

Study of Electronic Bands of Diatomic Molecules for the Evaluation of Toxicity of Green Crackers Using LIBS Coupled with Chemometric Method

by Darpan Dubey, Rohit Kumar, Abhishek Dwivedi and Awadhesh Kumar Rai

Electron. Mater. 2023, 4(1), 1-14; https://doi.org/10.3390/electronicmat4010001 - 27 Dec 2022

Cited by 1 | Viewed by 1639

Abstract

Laser-induced Breakdown Spectroscopy (LIBS) is primarily an atomic emission spectroscopic method based on analyzing the spectral lines of elements in the laser-induced plasma. However, when the plasma cools down after its ignition, i.e., when one collects the emissions from the plasma after a [...] Read more.

Laser-induced Breakdown Spectroscopy (LIBS) is primarily an atomic emission spectroscopic method based on analyzing the spectral lines of elements in the laser-induced plasma. However, when the plasma cools down after its ignition, i.e., when one collects the emissions from the plasma after a certain interval of time/gate delay (~1 micro-second), the signature of the electronic bands of diatomic molecules is also observed along with ionic/atomic emission lines. The present manuscript reports the evaluation of toxicity/pollutants in green crackers based on the intensity of the electronic bands of the Aluminum Oxide (AlO), calcium oxide (CaO), and strontium oxide (SrO) molecules observed in the laser-induced plasma of the firecrackers. LIBS spectra of the green crackers show the presence of spectral lines of the heavy/toxic elements such as Al, Ca, Sr, Cr, Cu, and Ba, along with the electronic bands of the AlO, CaO, and SrO. Fourier Transform Infra-Red Spectroscopy (FTIR) has been used to validate the LIBS results and confirm the molecules in these crackers. The concentration of toxic elements in green crackers such as Aluminum (Al), Copper (Cu), and Chromium (Cr) has also been estimated using the Partial Least Square Regression method (PLSR) to evaluate and compare the extent of the toxicity of green crackers. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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16 pages, 4287 KiB

Open AccessArticle

Adsorption of 2,4-D and MCPA Herbicides on Carbon Black Modified with Hydrogen Peroxide and Aminopropyltriethoxysilane

by Izabella Legocka, Krzysztof Kuśmierek, Andrzej Świątkowski and Ewa Wierzbicka

Materials 2022, 15(23), 8433; https://doi.org/10.3390/ma15238433 - 26 Nov 2022

Cited by 4 | Viewed by 1282

Abstract

The carbon black N-220 surface was subjected to modification through H₂O₂ oxidation and deposition of aminopropyltriethoxysilane. The pristine (CB-NM) and modified materials (CB-Ox and CB-APTES) were characterized by N₂ adsorption–desorption isotherms, scanning electron microscopy, energy-dispersive X-ray spectroscopy (SEM-EDS), thermogravimetry, [...] Read more.

The carbon black N-220 surface was subjected to modification through H₂O₂ oxidation and deposition of aminopropyltriethoxysilane. The pristine (CB-NM) and modified materials (CB-Ox and CB-APTES) were characterized by N₂ adsorption–desorption isotherms, scanning electron microscopy, energy-dispersive X-ray spectroscopy (SEM-EDS), thermogravimetry, and FTIR spectroscopy. Carbon black samples were applied as adsorbents for the removal of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) herbicides from aqueous solutions. The influence of their surface properties on adsorption efficiency was analyzed and discussed. The results showed that the adsorption of the herbicides was pH-dependent, and the most favorable adsorption was observed in an acidic environment. The experimental data best fit pseudo-second-order and Langmuir models for kinetic and equilibrium data, respectively. The adsorption rate of both the herbicides increased in the order of CB-APTES < CB-Ox < CB-NM and was closely correlated with the mesopore volume of the carbon blacks. The monolayer adsorption capacities were found to be 0.138, 0.340, and 0.124 mmol/g for the adsorption of 2,4-D and 0.181, 0.348, and 0.139 mmol/g for the adsorption of MCPA on CB-NM, CB-APTES, and CB-Ox, respectively. The results showed that the surface chemistry of the adsorbent plays a more important role than its porous structure. Both herbicides were preferably adsorbed on APTES-modified carbon black and were adsorbed the worst on oxidized carbon black (CB-APTES > CB-NM > CB-Ox). Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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7 pages, 7535 KiB

Open AccessArticle

Development of Carbon Nanotube/Silicone Pad for Improved Performance of Electromyostimulation Training

by Myeongcheol Kim, Jaegyun Im, Junsul Park, Kyung-Bum Kim and Jaegeun Lee

Energies 2022, 15(18), 6681; https://doi.org/10.3390/en15186681 - 13 Sep 2022

Viewed by 1421

Abstract

We have developed a carbon nanotube (CNT) pad to replace carbon black, which is essential for electric muscle stimulation (EMS) suits that can provide efficient exercise effects in a short time. The optimized CNT pad had 10 times lower concentration but showed 20 [...] Read more.

We have developed a carbon nanotube (CNT) pad to replace carbon black, which is essential for electric muscle stimulation (EMS) suits that can provide efficient exercise effects in a short time. The optimized CNT pad had 10 times lower concentration but showed 20 times lower resistance than the carbon black pad. In the case of the peak voltage indicating the EMS performance, it was confirmed that the CNT (4.0 wt%) was 25.9 V and the carbon black (40 wt%) was 6.5 V, which was about 4 times better. CNT added increased from 4.0 wt% to 10.0 wt%, and the peak voltage increased from 25.9 V to 26.8 V, but the output voltage was not significantly improved compared to the amount of CNT added. These experimental results are expected to show higher EMS properties than carbon black because carbon nanotubes and silicon are agglomerated to form a particle-like shape. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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17 pages, 3826 KiB

Open AccessArticle

Operando Analysis of Losses in Commercial-Sized Solid Oxide Cells: Methodology Development and Validation

by Antunes Staffolani, Arianna Baldinelli, Gianni Bidini, Francesco Nobili and Linda Barelli

Energies 2022, 15(14), 4978; https://doi.org/10.3390/en15144978 - 7 Jul 2022

Cited by 4 | Viewed by 1747

Abstract

The development of decarbonised systems is being fostered by the increasing demand for technological solutions for the energy transition. Solid Oxide Cells are high-efficiency energy conversion systems that are foreseen for commercial development. They exhibit potential power generation and power-to-gas applications, including a [...] Read more.

The development of decarbonised systems is being fostered by the increasing demand for technological solutions for the energy transition. Solid Oxide Cells are high-efficiency energy conversion systems that are foreseen for commercial development. They exhibit potential power generation and power-to-gas applications, including a reversible operation mode. Long-lasting high performance is essential for guaranteeing the success of the technology; therefore, it is fundamental to provide diagnosis tools at this early stage of development. In this context, operando analysis techniques help detect and identify incipient degradation phenomena to either counteract damage at its origin or correct operando protocols. Frequent switches from the fuel cell to the electrolyser mode add more challenges with respect to durable performance, and deep knowledge of reverse-operation-induced damage is lacking in the scientific and technical literature. Following on from preliminary experience with button cells, in this paper, the authors aim to transfer the methodology to commercial-sized Solid Oxide Cells. On the basis of the experimental evidence collected on planar square cells under dry and wet reactant feed gases, the main contributions to impedance are identified as being charge transfer (f = 10³–10⁴ Hz), oxygen surface exchanged and diffusion in bulk LSCF (f = 10²–10³ Hz), and gas diffusion in the fuel electrode (two peaks, f = 1–100 Hz). The results are validated using the ECM methodology, implementing an LRel(RctQ)GWFLW circuit. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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9 pages, 2436 KiB

Open AccessArticle

Performance of Insoluble IrO₂ Anode for Sewage Sludge Cake Electrodehydration Application with Respect to Operation Conditions

by Nam-Young Lee, Mi-Young You, Jaemyung Lee, Seohan Kim and Pung Keun Song

Coatings 2022, 12(6), 724; https://doi.org/10.3390/coatings12060724 - 25 May 2022

Cited by 2 | Viewed by 1725

Abstract

The efficient management of wastewater and sewage sludge treatment are becoming crucial with industrialization and increasing anthropological effects. Dehydration of sewage sludge cakes (SSCs) is typically carried out using mechanical and electrochemical processes. Using the mechanical dehydration process, only a limited amount of [...] Read more.

The efficient management of wastewater and sewage sludge treatment are becoming crucial with industrialization and increasing anthropological effects. Dehydration of sewage sludge cakes (SSCs) is typically carried out using mechanical and electrochemical processes. Using the mechanical dehydration process, only a limited amount of water can be removed, and the resultant SSCs have a water content of approximately 70–80 wt.%, which is significantly high for land dumping or recycling as solid fuel. Dumping high-moisture-content SSCs in land can lead to leakage of hazardous wastewater into the ground and cause economic loss. Therefore, dehydration of SSCs is crucial. Contemporary treatment methods focus on the development of anode materials for the electrochemical processes. IrO₂ is an insoluble anode material that is eco-friendly, less expensive, and exhibits high chemical stability, and it has been widely used and investigated in wastewater treatment and electrodehydration (ED) industries. Herein, we evaluated the performance of the ED system developed using IrO₂ anode material. The operating conditions of the anode such as reaction time, sludge thickness, and voltage on SSC were optimized. The performance of the ED system was evaluated based on the moisture content of SSCs after dehydration. The moisture content decreased proportionally with the reaction time, sludge thickness, and voltage. The moisture content of 40 wt.% was determined as the optimum quantity for land dumping or to be used as recycled solid fuel. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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11 pages, 2406 KiB

Open AccessArticle

Can Finite Element Method Obtain SVET Current Densities Closer to True Localized Corrosion Rates?

by Mohsen Saeedikhani, Sareh Vafakhah and Daniel J. Blackwood

Materials 2022, 15(11), 3764; https://doi.org/10.3390/ma15113764 - 24 May 2022

Cited by 1 | Viewed by 2835

Abstract

In this paper, the finite element method was used to simulate the response of the scanning vibrating electrode technique (SVET) across an iron–zinc cut-edge sample in order to provide a deeper understanding of the localized corrosion rates measured using SVET. It was found [...] Read more.

In this paper, the finite element method was used to simulate the response of the scanning vibrating electrode technique (SVET) across an iron–zinc cut-edge sample in order to provide a deeper understanding of the localized corrosion rates measured using SVET. It was found that, if the diffusion layer was neglected, the simulated current density using the Laplace equation fitted the experimental SVET current density perfectly. However, the electrolyte was not perturbed by a vibrating SVET probe in the field, so a diffusion layer existed. Therefore, the SVET current densities obtained from the local conductivity of the electrolyte would likely be more representative of the true corrosion rates than the SVET current densities obtained from the bulk conductivity. To help overcome this difference between natural conditions and those imposed by the SVET experiment, a local electrolyte corrected conductivity SVET (LECC-SVET) current density was introduced, which was obtained by replacing the bulk electrolyte conductivity measured experimentally by the local electrolyte conductivity simulated using the Nernst−Einstein equation. Although the LECC-SVET current density did not fit the experimental SVET current density as perfectly as that obtained from the Laplace equation, it likely represents current densities closer to the true, unperturbed corrosion conditions than the SVET data from the bulk conductivity. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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14 pages, 2315 KiB

Open AccessArticle

Electropolymerized Aniline-Based Stainless Steel Fiber Coatings Modified by Multi-Walled Carbon Nanotubes for Electroanalysis of 4-Chlorophenol

by Krzysztof Kuśmierek, Katarzyna Skrzypczyńska, Andrzej Świątkowski, Ewa Wierzbicka and Izabella Legocka

Materials 2022, 15(10), 3436; https://doi.org/10.3390/ma15103436 - 10 May 2022

Viewed by 1550

Abstract

In this paper, a stainless steel fiber coated electropolymerized aniline, without and with carbon nanotubes (SS/PANI and SS/PANI/CNT), along with CNTs modified carbon paste electrodes (CPEs), were prepared. The electrodes were characterized by differential pulse voltammetry (DPV) and applied for the detection of [...] Read more.

In this paper, a stainless steel fiber coated electropolymerized aniline, without and with carbon nanotubes (SS/PANI and SS/PANI/CNT), along with CNTs modified carbon paste electrodes (CPEs), were prepared. The electrodes were characterized by differential pulse voltammetry (DPV) and applied for the detection of 4-chlorophenol (4-CP). For all the electrodes, the oxidative peak current showed a linear dependence on the 4-CP concentration in the range of 0.05–0.5 mmol/L with R² ≥ 0.991. SS/PANI/CNT electrodes showed greater sensitivity for the detection of the 4-CP than the SS/PANI and CPEs. For all of the aniline-based stainless steel electrodes, both the LOD and LOQ decreased with the increase in the number of electropolymerization cycles. The lowest LOD (0.38 µmol/L) and LOQ (1.26 µmol/L) were observed for the SS/PANI/CNT electrode modified in aniline solution during 30 cycles. The methods were successfully applied to the analysis of 4-CP in real samples (tap water and river water). The results demonstrated the good agreement of the added and found concentrations of the 4-CP. The recovery and precision were from 95.12% to 102.24% and from 1.53% to 6.79%, respectively. The proposed electrodes exhibited acceptable reproducibility, admirable stability, and adequate repeatability and showed potential for the analysis of 4-CP in water. Full article

(This article belongs to the Topic Characterization of Electrochemical Materials)

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