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Electrochemical Deposition: Properties and Applications

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A special issue of Coatings (ISSN 2079-6412). This special issue belongs to the section "Surface Characterization, Deposition and Modification".

Deadline for manuscript submissions: closed (15 January 2024) | Viewed by 17495

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Dr. Gergana Alexieva

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Faculty of Physics, Sofia University "St. Kliment Ohridski”, 1164 Sofia, Bulgaria
Interests: research of gas sensing properties of electrochemically deposited ZrO₂ and ZnO films; research on the properties of sensors based on organic compounds
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Special Issue Information

Dear Colleagues,

This Special Issue is related to the properties and applications of the electrochemical deposition method. This method is a universal technique in which a coating of the desired material can be obtained on the surface of a conductive substrate by electrolysis of an aqueous solution containing the metal ion to be deposited or a complex thereof. Electrochemical deposition is a method of producing the desired coatings by chemical reduction of the metal ions or their complexes in the solution in a controlled manner. In electrochemical deposition, the ion reduction processes in the solution are under the action of an external feed, the anode and cathode reactions being separate, while at chemical deposition, the electrons required for the reaction are delivered from the reducing agent and the anode/cathode reaction is inseparable. Furthermore, chemical reactions are only performed on catalytically active surfaces, i.e., the surfaces must be sufficiently catalytically active for oxidation-reduction reactions.

Electrochemical deposition is an inexpensive and relatively fast deposition method that can be applied on an industrial scale to apply large-area coatings. It is one of the few methods in which high-melting metals such as platinum and rhodium can be deposited in low temperatures. The layers deposited by this method have a fine structure and physical properties such as high hardness and reflection.

The purpose of this Special Issue is to enrich the knowledge of the method of electrochemical deposition by publishing articles related to new developments, computer models and new applications related to this method.

Potential topics in this summary:

Advanced electrochemical nanostructure and technologies;
Electrochemical characterization of metallic surfaces and thin films;
Theory in electrochemistry and measurements;
Green electrochemical technologies;
Computer modeling in electrochemistry;
Multilayers in electrochemical deposition;
Applications of electrochemical deposition in semiconductor technologies.

Dr. Gergana Alexieva
Guest Editor

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Keywords

electrochemical deposition
thin films
nanostructure
modeling

Published Papers (11 papers)

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Research

Jump to: Review

12 pages, 5375 KiB

Open AccessArticle

Electrochemically Obtained Poly(3,4-ethylenedioxythiophene) Layers for Electroanalytical Determination of Lipoic Acid

by Vasilena Karabozhikova and Vessela Tsakova

Coatings 2023, 13(12), 2014; https://doi.org/10.3390/coatings13122014 - 28 Nov 2023

Viewed by 575

Abstract

Poly(3,4-ethylenedioxythiophene) (PEDOT) is a conducting polymer with intrinsic redox activity often used to facilitate electrooxidation reactions. PEDOT coatings with different thicknesses are obtained via electrochemical polymerization in the presence of either polysterensulfonate (PSS) or dodecylsulfate (SDS) anions. The electrooxidation of alfa lipoic acid (ALA) is studied depending on the thickness of the polymer coatings and the counterions used for their synthesis. The kinetics of ALA oxidation is found to differ for thin and thick PEDOT coatings with diffusion limitations observed for thin layers. For thick coatings, the rate-determining step varies from adsorption to diffusion depending on the ALA concentration. The type of counterion affects both the ALA oxidation peak currents and the peak potential. SDS-doped PEDOT coatings show a shift in the oxidation peak to positive potentials and higher ALA oxidation currents. The effect is commented in terms of a larger electroactive surface area and possible specific hydrophobic polymer/analyte interactions. For thin PEDOT coatings, the concentration dependence of the voltammetric peaks is linear in a wide concentration range (40 to 1000 µM), whereas the use of differential pulse voltammetry results in a linear response in a lower concentration range (8–200 µM) suitable for practical applications. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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19 pages, 8512 KiB

Open AccessArticle

The Contribution of the Pore Size of Titanium DC (Direct Current) Sputtered Condensation Polymer Materials to Electromagnetic Interruption and Thermal Properties

by Hye-Ree Han

Coatings 2023, 13(10), 1756; https://doi.org/10.3390/coatings13101756 - 11 Oct 2023

Viewed by 736

Abstract

Using special materials has been in the spotlight, along with their multifunctional demands, research on electromagnetic interruption, thermal characteristics, biosignal sensors, secondary batteries, etc. In this study, titanium was sputtered into a condensation polymer material and considered in depth in terms of electromagnetic interruption, thermal properties, infrared blocking, etc. As a result of observing the electromagnetic wave shielding effect, the electromagnetic wavelength value decreased from 168.0 to 42.7 to 64.0 when titanium DC sputtered film samples were placed in front of the electromagnetic wave source. The titanium DC sputtered samples significantly reduced electrical resistance compared to the untreated samples. In addition, the IR transmittances of the titanium sputtered specimens were decreased compared to the untreated specimens. When only the cross-section was treated with titanium sputtering and the titanium surface was directed toward the infrared irradiator, the infrared permeability was 64.3 to 0.0%. After taking an infrared thermal image, ΔH, ΔV, ΔS, ΔY, ΔCr, and ΔCb values were calculated. It is believed that the titanium DC sputtered polyamide materials produced in this study can be used for high-functional protective clothing, sensors by applying electromagnetic interruption, IR blocking, and stealth functions. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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23 pages, 7442 KiB

Open AccessArticle

Medium and High Phosphorous Ni-P Coatings Obtained via an Electroless Approach: Optimization of Solution Formulation and Characterization of Coatings

by Virgilio Genova, Laura Paglia, Giovanni Pulci, Giulia Pedrizzetti, Alice Pranzetti, Marco Romanelli and Francesco Marra

Coatings 2023, 13(9), 1490; https://doi.org/10.3390/coatings13091490 - 24 Aug 2023

Cited by 1 | Viewed by 1216

Abstract

A new lead-free electroless Ni-P plating solution was developed for the deposition of coatings with medium phosphorus content (MP, 6–9 wt%), and its composition was optimized to obtain deposits with high phosphorus (HP, 10–14 wt%). Cleaning and activation treatments were studied in terms of effectiveness and influence on the deposition rate. The concentration of reagents (nickel salt, complexing agent, reducing agent and stabilizer) was studied, and their combined effect on P content and plating rate was investigated. The obtained coatings were analyzed by SEM and XRD and thermally treated at 400 °C and 600 °C to study microstructural evolution. Vickers hardness was measured on as-deposited and annealed coatings to relate hardness evolution to microstructural changes after thermal treatments. Optimal deposition conditions were determined, enabling the production of MP coatings (6.5 wt% P) with a plating rate of 40 µm/h and HP coatings (10.9 wt% P) with a plating rate of 25 µm/h at 90 °C. Samples heat-treated at 400 °C showed improved hardness thanks to crystallization and microprecipitation of Ni₃P hard phases, whereas hardness decrease was observed after treatment at 600 °C due to the combined effect of grain growth and coarsening of Ni₃P precipitates. No through-the-thickness cracks were detected by the Ferroxyl reagent after heat treatments. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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14 pages, 12280 KiB

Open AccessFeature PaperArticle

Rapid Thermal Processing of Kesterite Thin Films

by Maxim Ganchev, Stanka Spasova, Taavi Raadik, Arvo Mere, Mare Altosaar and Enn Mellikov

Coatings 2023, 13(8), 1449; https://doi.org/10.3390/coatings13081449 - 17 Aug 2023

Cited by 1 | Viewed by 1031

Abstract

Multinary chalcogenides with Kesterite structure Cu₂ZnSn(S,Se)₄ (CZTSSe) are a prospective material base for the enhancement of the photovoltaics industry with abundant and environmentally friendly constituents and appropriate electro-physical properties for building highly efficient devices at a low cost with a short energy pay-back time. The actual record efficiency of 13.6%, which was reached recently, is far below the current isostructural chalcopyrite’s solar cells efficiency of near 24%. The main problems for future improvements are the defects in and stability of the Kesterite absorber itself and recombination losses at interfaces at the buffer and back contacts. Here, we present an investigation into the rapid thermal annealing (RTA) of as-electrodeposited thin films of Cu₂ZnSnS₄ (CZTS). The treatment was carried out in a cold wall tubular reactor in dynamic conditions with variations in the temperature, speed and time of the specific elements of the process. The effect of annealing was investigated by X-ray diffractometry, Raman scattering and Scanning Electron Microscopy (SEM). The phase composition of the films depending on treatment conditions was analyzed, showing that, in a slow, prolonged, high-temperature process, the low-temperature binaries react completely and only Kesterite and ZnS are left. In addition, structural investigations by XRD have shown a gradual decrease in crystallite sizes when the temperature level and duration of the high-temperature segment increases, and respectively increase in the strain due to the formation of the phases in non-equilibrium conditions. However, when the speed of dynamic segments in the process decreases, both the crystallite size and strain of the Kesterite non-monotonically decrease. The grain sizes of Kesterite, presented by SEM investigations, have been shown to increase when the temperature and the duration increase, while the speed decreases, except at higher temperatures of near 750 °C. The set of experiments, following a scrupulous analysis of Raman data, were shown to have the potential to elucidate a way to ensure the fine manipulation of the substitutional Cu/Zn defects in the structure of CZTS thin films, considering the dependences of the ratios of Q = I₂₈₇/I₃₀₃ and Q′ = I₃₃₈/(I₃₆₆ + I₃₇₄) on the process variables. Qualitatively, it can be concluded that increases in the speed, duration and temperature of RTA lead to increases in the order of the structure, whereas, at higher temperatures of near 750 °C, these factors decrease. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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13 pages, 5648 KiB

Open AccessArticle

Transforming Chimney Soot via Stochastic Polymerization for Active Electrode Coating

by Miroslav Petrov, Lyubomir Slavov, Toma Stankulov, Boryana Karamanova, Teodor Milenov, Dimitar Dimov and Ivalina Avramova

Coatings 2023, 13(8), 1354; https://doi.org/10.3390/coatings13081354 - 02 Aug 2023

Cited by 1 | Viewed by 989

Abstract

A polymerization procedure is presented to increase the molecular weight of hydrocarbons in household chimney soot without thermal treatment at high temperatures. Pristine soot was subject to chlorination, with half of it treated with magnesium (Mg-plates) to create random-type Grignard reagents (R-Mg-Cl) in diethyl ether media. Mixing the Grignard reagent and the rest of the halogenated soot material created new C-C bonds, thus increasing the molecular weight of the final product. The obtained stochastically polymerized soot (SPS) was investigated using Raman spectroscopy, FTIR spectroscopy and XPS and was subjected to electrochemical testing as an assembled supercapacitor with a KOH electrolyte. Results show significant carbon structure differences due to the chemical procedures and newly created functional groups in the soot. Such functional groups could increase the capacity of supercapacitors, creating pseudo-capacitance by participating in redox reactions. The results also unveiled removing any random contaminations in the pristine soot and obtaining a more uniform final product containing hydrocarbons with longer chains, thus increasing the molecular weight. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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17 pages, 9616 KiB

Open AccessArticle

Electrophoretic Deposition and Characterization of Er-Doped Bi₂O₃ Cathode Barrier Coatings on Non-Conductive Ce_0.8Sm_0.2O_1.9 Electrolyte Substrates

by Elena Kalinina, Larisa Ermakova and Elena Pikalova

Coatings 2023, 13(6), 1053; https://doi.org/10.3390/coatings13061053 - 06 Jun 2023

Viewed by 809

Abstract

In this study, the formation of thin-film barrier coatings based on a highly conductive Bi_1.60Er_0.4O₃ (EDB) solid electrolyte on supporting Ce_0.8Sm_0.2O_1.9 (SDC) electrolyte substrates was implemented for the first time using electrophoretic deposition (EPD). The electrokinetic properties of EDB-based suspensions in a non-aqueous dispersion medium of isopropanol modified with small additions of polyethyleneimine (PEI, 0.26 g/L) and acetylacetone (0.15 g/L), as well as in a mixed isopropanol/acetylacetone (70/30 vol.%) medium, were studied. The dependences of the thickness of the EDB coatings on voltage and deposition time were obtained using deposition on a model Ni foil electrode. Preliminary synthesis of a conductive polypyrrole (PPy) polymer film was used to create surface conductivity on non-conductive SDC substrates. The efficiency of using a modified dispersion medium based on isopropanol to obtain a continuous EDB coating 12 μm thick, sintered at a temperature of 850 °C for 5 h, is shown. The microstructure and morphology of the surface of the EDB coating were studied. A Pt/SDC/EDB/Pt cell was used to characterize the coating’s conductivity. The EPD method is shown to be promising for the formation of barrier coatings based on doped bismuth oxide. The developed method can be used for creating cathode barrier layers in SOFC technology. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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10 pages, 4590 KiB

Open AccessCommunication

Electrodeposition of Soft Magnetic Fe-W-P Alloy Coatings from an Acidic Electrolyte

by Natalia Kovalska, Antonio Mulone, Jordi Sort, Uta Klement, Gurdial Blugan, Wolfgang Hansal and Wolfgang Kautek

Coatings 2023, 13(4), 801; https://doi.org/10.3390/coatings13040801 - 20 Apr 2023

Viewed by 1065

Abstract

Fe-W-P coatings were deposited from a newly developed electrolytic bath. The effect of plating parameters, such as electrolyte current density and pH has been studied. It was found that the pH has a very strong effect on the phosphorous content of the coatings. Metallic-like, non-powdery alloys of Fe-W-P deposits with no cracks (lowly stressed) can be obtained at a lower pH (<3), exhibiting high phosphorus (up to 13 at.%) and low tungsten (6 at.%) contents. At a higher pH (>3), the composition changes to low phosphorus and high tungsten content, showing a matte, greyish, and rough surface. The applied current density also influences the morphology and the amount of phosphorous content. The deposits showed an amorphous structure for all samples with soft ferromagnetic properties. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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10 pages, 16409 KiB

Open AccessArticle

Effect of Deposition Parameters on Morphological and Compositional Characteristics of Electrodeposited CuFeO₂ Film

by Min-Kyu Son

Coatings 2022, 12(12), 1820; https://doi.org/10.3390/coatings12121820 - 25 Nov 2022

Cited by 2 | Viewed by 1089

Abstract

Deposition parameters determine the characteristics of semiconductor films in electrodeposition. Thus, it is essential to understand the effect of deposition parameters on the electrodeposited film for fabricating suitable semiconductor film fitting for various applications. In this work, the morphological and compositional properties of electrodeposited delafossite CuFeO₂ film, according to the deposition parameters, were studied. The CuFeO₂ film was fabricated by the galvanostatic electrodeposition and post-annealing process under inert gas flow. The type of solvent, electrolyte condition, applied current density and deposition time were controlled as the variable deposition parameters. As a result, the typical CuFeO₂ film, without any impurities, was electrodeposited in the electrolyte-based DMSO solvent. Interestingly, the concentration of potassium perchlorate as a complexing agent caused morphological change in electrodeposited CuFeO₂ film, as well as compositional transition. On the other hand, the applied current density and deposition time only influenced the morphology of electrodeposited CuFeO₂ film. These observations would provide specific guidelines for the fabrication of electrodeposited CuFeO₂ film with suitable composition and morphology for various applications. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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11 pages, 4403 KiB

Open AccessArticle

Controlled Electroplating of Noble Metals on III-V Semiconductor Nanotemplates Fabricated by Anodic Etching of Bulk Substrates

by Elena I. Monaico, Eduard V. Monaico, Veaceslav V. Ursaki and Ion M. Tiginyanu

Coatings 2022, 12(10), 1521; https://doi.org/10.3390/coatings12101521 - 11 Oct 2022

Cited by 6 | Viewed by 2218

Abstract

Porous templates are widely used for the preparation of various metallic nanostructures. Semiconductor templates have the advantage of controlled electrical conductivity. Site-selective deposition of noble metal formations, such as Pt and Au nanodots and nanotubes, was demonstrated in this paper for porous InP templates prepared by the anodization of InP wafers. Metal deposition was performed by pulsed electroplating. The produced hybrid nanomaterials were characterized by scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). It was shown that uniform deposition of the metal along the pore length could be obtained with optimized pulse parameters. The obtained results are discussed in terms of the optimum conditions for effective electrolyte refreshing and avoiding its depletion in pores during the electroplating process. It was demonstrated that the proposed technology could also be applied for the preparation of metal nanostructures on porous oxide templates, when it is combined with thermal treatment for the oxidation of the porous semiconductor skeleton. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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10 pages, 1649 KiB

Open AccessArticle

Structural, Morphological and Optical Properties of Nanostructured ZrO₂ Films Obtained by an Electrochemical Process at Different Deposition Temperatures

by Konstantin Lovchinov, Rositsa Gergova and Gergana Alexieva

Coatings 2022, 12(7), 972; https://doi.org/10.3390/coatings12070972 - 08 Jul 2022

Cited by 2 | Viewed by 1676

Abstract

This article focuses on the impact of the deposition temperature (in the range from 60 to 80 °C) in ZrO₂ films obtained by the electrochemical deposition process on SnO₂-covered glass substrates. The solution in which the deposition takes place is aqueous, containing ZrOCl₂ with a concentration of 3 × 10⁻⁵ M and KCl with a concentration of 0.1 M. By implementing X-ray diffraction (XRD), optical profilometry, scanning electron microscopy (SEM), and UV-VIS-NIR spectroscopy, the temperature dependence of ZrO₂ films properties was revealed. The X-ray Diffraction XRD spectra showed six different diffraction maxima ((−111)M, (101)T, (111)M, (112)M, (202)M, and (103)M) associated with the electrochemical ZrO₂ layers, and the polycrystalline structure of the films was confirmed at all deposition temperatures. The determination of the average roughness did not indicate significant temperature dependence in the deposited layers. SEM micrographs showed that the layers were composed of grains, most of them of a regular shape, although their size increased slightly with an increased deposition temperature. The coarsest-grained structure was observed for the layers deposited at 80 °C. It was demonstrated that the deposition temperature weakly impacts the reflectance and transmittance spectra of the ZrO₂ layers. Such layers with low values of specular and high values of diffuse transition, and reflection in the spectral range from 380 to 800 nm, can be applied to various optoelectronic devices such as thin-film solar cells. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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Review

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16 pages, 2505 KiB

Open AccessReview

A Review on Sustainable Manufacturing of Ceramic-Based Thin Films by Chemical Vapor Deposition (CVD): Reactions Kinetics and the Deposition Mechanisms

by M. Sabzi, S. H. Mousavi Anijdan, M. Shamsodin, M. Farzam, A. Hojjati-Najafabadi, P. Feng, N. Park and U. Lee

Coatings 2023, 13(1), 188; https://doi.org/10.3390/coatings13010188 - 14 Jan 2023

Cited by 15 | Viewed by 4646

Abstract

Chemical vapor deposition (CVD) is a process that a solid is formed on a substrate by the chemical reaction in the vapor phase. Employing this technology, a wide range of materials, including ceramic nanocomposite coatings, dielectrics, and single crystalline silicon materials, can be coated on a variety of substrates. Among the factors influencing the design of a CVD system are the dimensions or geometry of the substrate, substrate temperature, chemical composition of the substrate, type of the deposition process, the temperature within the chamber, purity of the target material, and the economics of the production. Three major phenomena of surface reaction (kinetic), diffusion or mass transfer reaction, and desorption reaction are involved during the CVD process. Thermodynamically, CVD technology requires high temperatures and low pressures in most systems. Under such conditions, the Gibbs free energy of the chemical system quickly reaches its lowest value, resulting in the production of solids. The kinetic control of the CVD technology should always be used at low temperatures, and the diffusion control should be done at high temperatures. The coating in the CVD technology is deposited in the temperature range of 900–1400 °C. Overall, it is shown here that by controlling the temperature of the chamber and the purity of the precursors, together with the control of the flow rate of the precursors into the chamber, it is possible to partially control the deposition rate and the microstructure of the ceramic coatings during the CVD process. Full article

(This article belongs to the Special Issue Electrochemical Deposition: Properties and Applications)

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