One-step Cathodic Electrodeposition Research Articles

Smart gradient coating suitable for bone growth prepared on plasma-electrolytically oxidised Mg and its sequential degradation behaviour

A gradient coating containing collagen and inorganic strontium/calcium phosphate (Sr/CaP) was fabricated on plasma-electrolytically oxidised magnesium via one-step cathodic electrodeposition. First, Sr-doped dicalcium phosphate dihydrate and hydroxyapatite (DCPD and HA) was deposited, followed by a collagen/CaP layer. The morphological evolution, sequential degradation behaviour, and in vitro bio-properties of the coatings were investigated. The incorporation of collagen remarkably refined the morphology of the CaP, and a more aggregated nano-spherical morphology was observed with increasing collagen concentration. Sr could partially replace Ca in the CaP crystals. Collagen combined with CaP formed a relatively stable skeletal frame, which provided sufficient barrier properties and more sites for the re-precipitation of bone tissue, as well as a more promising proliferation and differentiation ability of osteoblasts. A gradient coating that matches the requirements of bone growth at various periods is suggested for implantation.

Labeled free electrochemiluminescence aptamer platform based on one-step cathodic electrochemical growth of 2D/3D Ru-BTC-MOFs nanoparticles to detect carcinoembryonic antigen

[Ru(dcbpy)3]2+ functionalized 2D/3D hybrid metal–organic frameworks (Ru-BTC-MOFs), which performed good ECL performance, were synthesized by on one-step cathodic electrodeposition with Zn(NO3)2 as metal ion source, Ru(dcbpy)3Cl2) (tri(4,4-dicarboxybipyridine) ruthenium chloride) and H3BTC (1,3,5-phenyl tricarboxylic acid) as organic ligand. The effect of electrodeposition voltage, electrodeposition time, H3BTC and [Ru(dcbpy)3]Cl2 concentration on the morphology and ECL performance of Ru-BTC-MOFs were investigated in detail. An ECL biosensor platform for sensitive detection of carcinoembryonic antigen (CEA) was constructed by further modified AuNPs and aptamer on the Ru-BTC-MOFs/GCE. The specifically recognition and adsorption of CEA would hinder the electron transfer between Ru-BTC-MOFs and trinpropylamine (TPA) as the co-reactive agent, resulting in decreasing the ECL intensity. Under the optimal experimental conditions, the ECL intensity and logarithm of CEA concentration showed a good linear relationship in the concentration range of 10.0 fg/mL to 10.0 ng/mL, and the detection limit was 5.56 fg/mL. The proposed sensor performed acceptable reproducibility, repeatability, anti-interference ability and stability, and it would be expected to have broad application prospects in clinical trials.

One-step cathodic electrodeposition of a cobalt hydroxide-graphene nanocomposite and its use as a high performance supercapacitor electrode material.

In this study, Co(OH)2-reduced graphene oxide has been synthesized using a simple and rapid one-step cathodic electrodeposition method in a two electrode system at a constant current density on a stainless steel plate, and then characterized as a supercapacitive material on Ni foam. The composites were characterized by FT-IR, X-ray diffraction, scanning electron microscopy, and cyclic voltammetry using a galvanostatic charge/discharge test. The feeding ratios of the initial components for electrodeposition had a significant effect on the structure and electrochemical performance of the Co(OH)2-reduced graphene oxide composite. The results show that the 1 : 4 (w/w) ratio of GO : CoCl2·6H2O was optimum and produced an intertwined composite structure with impressive supercapacitive behavior. The specific capacitance of the composite was measured to be 734 F g−1 at a current density of 1 A g−1. Its rate capability was ∼78% at 20 A g−1 and its capacitance retention was 95% after 1000 cycles of charge–discharge. Moreover, its average energy density and power density were calculated to be 60.6 W h kg−1 and 3208 W kg−1, respectively. This green synthesis method enables a rapid and low-cost route for the large scale production of Co(OH)2-reduced graphene oxide nanocomposite as an efficient supercapacitor material.

Mechanistic Study of One-Step Cathodic Electrodeposition of Mixed Cu-In-Ga Oxide/Hydroxide Films with Hydrogen Peroxide Oxygen Precursor

Electrodeposition of multicomponent oxide films with semiconducting properties for use in various applications like photovoltaics is of great interest. This paper deals with mixed copper, indium, gallium oxides which can be used as precursors for copper indium gallium diselenide layer in thin film solar cells and potentially p-type transparent oxide layers, in the delafossite family. One-step cathodic electrodeposition of Cu-In-Ga mixed oxide/hydroxide is investigated using hydrogen peroxide as the oxygen source. The deposition mechanism of the Cu-In-Ga oxide layers is studied by cyclic voltammetry and in situ using an electrochemical quartz crystal microbalance. A marked influence of hydrogen peroxide on the Cu(II), In(III) and Ga(III) electrochemical system is evidenced. Hydrogen peroxide enables the incorporation of indium and gallium as oxides/hydroxides at much less negative potentials than the In and Ga metals. A reaction path is proposed which accounts for the main experimental results. The reduction process starts with the reduction of cupric species, which is followed by the reduction of hydrogen peroxide. For peroxide concentrations higher than 20 mM, the precipitation of Ga and In oxides/hydroxides takes place. At more negative potentials the reactions become controlled by mass transfer allowing to control the composition of the films.

Effect of Electrodeposition Potential on Composition of CuIn1−xGaxSe2Absorber Layer for Solar Cell by One-Step Electrodeposition

CIGS polycrystalline thin films were successfully fabricated by one-step cathodic electrodeposition on Mo-coated glass. In this study, we applied a galvanometry mode with three-electrode potentiostatic systems to produce a constant concentration electroplating solution, which were composed of CuCl2, InCl3, GaCl3, and SeO2. Then these as-electrodeposited films were annealed in argon atmosphere and characterized by X-ray diffraction. The results revealed that annealing treatment significantly improved the crystallinity of electrodeposited films and formed CIGS chalcopyrite structure, but at low applied deposition voltage (−950 mV versus SCE) there appeared second phase. The cross-section morphology revealed that applied voltage at −1350 mV versus SCE has uniform deposition, and higher applied voltage made grain more unobvious. The deposition rate and current density are proportional to deposition potential, and hydrogen was generated apparently when applying potential beyond −1750 mV versus SCE. It was found that the CIGS compound did not match exact stoichiometry ofCu : In : Ga : Se =1 : x : 1-x : 2. This result suggests the possibility of controlling the property of thin films by varying the applied potential during electrodeposition.

Synthesis of MnO2–chitosan nanocomposite by one-step electrodeposition for electrochemical energy storage application

MnO2–chitosan hybrid nanocomposite films with low and high chitosan's molecular weights are synthesized by one-step cathodic electrodeposition on nickel foam substrate for electrochemical capacitors (ECs) application. The films have been characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), fourier transform infrared (FTIR) spectroscopy, cyclic voltammetry, galvanostatic charge–discharge, and electrochemical impedance spectroscopy. The MnO2–chitosan hybrid nanocomposite films show better specific capacitance and rate capability than chitosan-free MnO2 film. For the MnO2–chitosan composite films, the highest specific capacitance is 424 F g−1 obtained at a current density of 1 mA cm−2. The deposited film retains a very stable capacitance over 400 cycles by charging and discharging at 3 mA cm−2, and only 3% capacity loss is observed. The presence of chitosan promotes both ion and electron transport in the matrix of MnO2. Besides, it allows the formation of porous and crack-free deposited films. A deposition mechanism for MnO2–chitosan hybrid nanocomposite films is proposed.

Characterization of Single Bath Electrodeposited Cu2ZnSnSe4 Thin Films

Cu2ZnSnSe4 (CZTSe), a chalcopyrite-like semiconductor, which has high optical absorption and p-type electrical conductivity, provide a low-cost mass production solution with abundant and cheap materials, Zn and Sn. In previous researches, CZTSe was produced from co-evaporated or sputtered precursors. In this study, electrodeposition, a non-vacuum and low-cost process, was used to grow CZTSe films. The films were grown by one-step cathodic electrodeposition in single electrolyte bath, which contained CuCl2, ZnCl2, SnCl2, and were deposited onto Mo coated glass substrates at room temperature. The CZTSe thin films have been obtained after annealing the as-deposited thin CZT films with powder of Se. The reduction potentials of each element in the electrolyte were determined by linear scan voltammetry (LSV) method. The film properties were characterized by field-emission scanning electron microscopy (FE-SEM) amd EDS.

Electrodeposition of zinc oxide/tetrasulfonated copper phthalocyanine hybrid thin film for dye-sensitized solar cell application

Hybrid film of zinc oxide (ZnO) and tetrasulfonated copper phthalocyanine (TSPcCu) was grown on an indium tin oxide (ITO) glass by one-step cathodic electrodeposition from aqueous mixtures of Zn(NO 3) 2, TSPcCu and KCl. The addition of TSPcCu strongly influences the morphology and crystallographic orientation of the ZnO. The nanosheets stack of ZnO leads to a porous surface structure which is advantageous to further adsorb organic dyes. The photovoltaic properties were investigated by assembling the DSSC device based on both the only ZnO film and the ZnO/TSPcCu hybrid films. Photoelectrochemical analysis revealed that the optimized DSSC device with TSPcCu represented a more than three-fold improvement in power conversion efficiency than the device without TSPcCu. The DSSC based on ZnO/TSPcCu hybrid films demonstrates an open circuit voltage of 0.308 V, a short circuit current of 90 μA cm −2, a fill factor of 0.26, and a power conversion efficiency of 0.14%.

The preparation of SnO2 film by electrodeposition

Abstract SnO2 is an interesting material for a wide array of applications. In this report, pure SnO2 films were deposited on Cu substrates by one-step cathodic electrodeposition without any pretreatment of the electrolyte or post-treatment of the deposit. It was found that the concentration of HNO3 in the electrolyte, ageing of the electrolyte, the electrodeposition temperature, and the electrodeposition voltage are critical to obtain SnO2 films and avoid co-deposition of Sn. By carefully controlling those processing parameters, pure SnO2 films composed of fine particles with good adherence to the Cu substrate have been successfully prepared.

STUDY OF THE STOICHIOMETRIC RATIO OF ONE-STEP ELECTRODEPOSITED CuInSe2 FILMS ON ITO/SODA-LIME GLASS

Copper indium diselenide ( CuInSe 2) thin films were grown on indium–tin oxide (ITO)/soda-lime glass using a one-step cathodic electrodeposition process at potentials lower than -0.6 V vs SCE, and in the presence of a large excess of In 3+. The source solution contained CuCl 2, InCl 3, and H 2 SeO 3 complexed by citric acid. The concentration of InCl 3 in the electrochemical bath affected the structure, composition, stoichiometric ratio, and morphological properties of electrodeposited films. CuInSe 2 films with a chalcopyrite structure and quite good stoichiometry were directly electrodeposited from a solution of 20 mM InCl 3, 5 mM CuCl 2, and 8 mM H 2 SeO 3. Annealing of these CuInSe 2 films in the temperature range from 300°C to 500°C improves their crystallinity and increases their grain size. Good chalcopyrite CuInSe 2 films with a (112) preferential orientation suitable for the production of efficient solar cells are obtained after annealing at 500°C. The formation mechanism of the ternary CuInSe 2 compound during the electrodeposition process was discussed.

Electrochemically Deposited 2D Nanowalls of Calcium Phosphate−PDDA on a Glassy Carbon Electrode and Their Applications in Biosensing

A novel calcium phosphate (CaP)−poly[diallyldimethylammonium chloride] (PDDA) composite film with two-dimensional (2D) nanostructure was first constructed on glassy carbon electrode (GCE) via a simply one-step cathodic electrodeposition method at room temperature. X-ray photoelectron spectroscopy, X-ray powder diffraction, scanning electronic microscopy, and electrochemical impedance spectroscopy were used to characterize the composite film. The experimental results demonstrated that PDDA plays an important role in the formation of nanowall-like morphologies. The effects of the percentage of PDDA and the deposition time on the film growth were investigated. The composite film is favorable for protein immobilization with many specific properties, such as nontoxicity, high specific surface area, large specific cell-volume, and sufficiently functional groups for attaching protein. Hemoglobin (Hb) immobilized on such a film showed a pair of stable and well-defined peaks at −0.403 and −0.303 V at the scan rate...

Characterization of electrodeposited CuInSe 2 (CIS) film

CuInSe 2 thin film was grown by one-step cathodic electrodeposition on Pt-coated glass using amperometry mode (fixed potential), in a three-electrode potentiostatic system containing the precursor solutions, 10 mM CuSO 4, 50 mM InSO 4, 30 mM SeO 2, and 0.1 M K 2SO 4 as a supporting electrolyte, at a pH of 1.5 (±0.1) adjusted with 0.1 M H 2SO 4. The structure, chemical composition, morphology, optical properties, and uniformity of the electrodeposited CuInSe 2 film were characterized by X-ray diffraction (XRD), electron probe micro analysis (EPMA), UV–vis–NIR spectrophotometry, field-emission scanning electron microscopy (FE-SEM), and Auger electron spectroscopy (AES), respectively. Several experiments were conducted in which the deposition voltage and post-annealing conditions were varied. As the applied deposition voltage was increased from −0.6 V to −0.7 V versus Ag/AgCl, a CuInSe 2 thin film with a chalcopyrite structure came to be predominantly formed, in accordance with the chemical composition, while the formation of the binary compounds (CuO and Cu x Se) which influence the degradation of the performance in the application of CIS-based solar cells, rapidly decreased. The optimum conditions consisted of an annealing temperature of about 350 °C for 30 min under nitrogen ambient. At this temperature, a CuInSe 2 thin film, in the form of ternary compound, is formed with the required conditions, namely good crystallinity, good stoichiometry, a suitable bandgap, and depth uniformity.

Electrochemical Self-Assembly of ZnO / SO 3EtPTCDI Hybrid Photoelectrodes

Self-assembled growth of ZnO films modified with -bis(ethylenesulfate)-3,4,9,10-perylene tetracarboxylic acid diimide has been realized by a one-step cathodic electrodeposition. Scanning electron microscopy and X-ray diffraction examination of the hybrid films has revealed morphological and structural changes with increasing dye concentration in the deposition bath. The photoelectrochemical action spectra demonstrate a significant enhancement of the anodic photocurrent for electrodes in comparison to that of pure ZnO electrodes, thus evidencing photosensitization of ZnO by the adsorbed dye molecules. A maximum incident photon-to-current conversion efficiency of 7.0% was obtained for such hybrid thin-film electrodes. Impedance measurements indicated a positive shift of the flatband potential of ZnO as a consequence of dye adsorption, enabling the injection of photogenerated electrons from the lowest unoccupied π-molecular orbital of into the conduction band of ZnO. © 2003 The Electrochemical Society. All rights reserved.

One-step electrochemical synthesis of ZnO/Ru(dcbpy) 2(NCS) 2 hybrid thin films and their photoelectrochemical properties

Hybrid thin films of crystalline zinc oxide (ZnO) and Ru(dcbpy) 2(NCS) 2 (dcbpy=4,4′-dicarboxy-2,2′-bipyridine) have been synthesized by one-step cathodic electrodeposition from oxygen-saturated aqueous solutions containing zinc chloride and the Ru complex. While the pure ZnO thin films are oriented with the c-axis perpendicular to the substrate, the ZnO crystallites in the hybrid thin films are oriented with the c-axis parallel to the substrate as a consequence of the adsorption of the Ru complex onto the growing surface of ZnO. Thin hybrid films (up to about 0.5 μm) consist of grains with approximately 300 nm diameter, which are composed of ZnO crystallites of approximately 20 nm. For thicker films, the formation of an overlayer in a totally different morphology has been observed. The hybrid thin films have a composition of ZnO:Ru(dcbpy) 2(NCS) 2=30:1 in molar ratio, corresponding to a volume ratio of ZnO:Ru(dcbpy) 2(NCS) 2=1:1.7, indicating a very high amount of the Ru complex in the film. The loaded Ru complex can be mostly extracted by dipping the film in a dilute alkaline solution, indicating the porous nature of the film and the presence of the dye mainly on the surface of ZnO. The hybrid thin film electrodes exhibit sensitized photoanodic currents upon white light illumination in organic electrolyte solutions containing iodide which are analyzed in terms of wavelength dependence, I–V characteristics and by time-resolved photocurrent measurements. The thinner films performed considerably better than the thicker films in which dye aggregation seemed to decrease the electron injection efficiency.

Improved performance of a dye-sensitized solar cell using a TiO2/ZnO/Eosin Y electrode

TiO2/ZnO/Eosin Y structure films were prepared by a one-step cathodic electrodeposition method and used as a photoanode in a dye-sensitized solar cell (DSSC). Using this TiO2/ZnO/Eosin Y electrode in DSSC, the degradation of the cell with time was reduced and ISC, VOC and fill factor values were increased. The use of a thin ZnO layer, permitted the formation of an energy barrier at the electrode/electrolyte interface, thus reducing recombination rate and improving cell performance. In addition, the adsorbed dye molecules prepared by one-step cathodic electrodeposition with ZnO were very stable compared with that prepared by conventional immersing method, as evidenced by UV/vis absorption spectroscopy measurements.