Electrochemical Deposition and Nucleation of Aluminum on Tungsten in Aluminum Chloride-Sodium Chloride Melts

Electrochemical deposition and nucleation of aluminum on tungsten electrode from AlCl3-NaCl melts were studied by cyclic voltammetry, chronopotentiometry and chronoamperometry. Cyclic voltammetry and chronopotentiometry analyses showed that Al （Ⅲ） was reduced at 200℃ in two consecutive steps in an electrolyte of molten AlCl3-NaCl system with a composition 52：48 molar ratio. The current-time characteristics of nucleation aluminum on tungsten showed a strong dependence on overpotentials. Chronoamperometry showed that the deposition process of aluminum on tungsten was controlled by an instantaneous nucleation with a hemispherical diffusion-controlled growth mechanism. The results could lead to a better understanding of the AlCl3-NaCl melt system that has technological importance in electrodeposition of metals as well as in rechargeable batteries.

Synthesis of Biomimetic Superhydrophobic Surface through Electrochemical Deposition on Porous Alumina

The superhydrophobicity of plant leaves is a benefit of the hierarchical structures of their surfaces. These structures have been imitated in the creation of synthetic surfaces. In this paper, a novel process for fabrication of biomimetic hierarchical structures by electrochemical deposition of a metal on porous alumina is described. An aluminum specimen was anodically oxidized to obtain a porous alumina template, which was used as an electrode to fabricate a surface with micro structures through electrochemical deposition of a metal such as nickel and copper after the enlargement of pores. Astonishingly, a hier- archical structure with nanometer pillars and micrometer clusters was synthesized in the pores of the template. The nanometer pillars were determined by the nanometer pores. The lbrmation of micrometer clusters was related to the thin walls of the pores and the crystallization of the metal on a flat surface. From the as-prepared biomimetic surfaces, lotus-leaf-like superhydrophobic surfaces with nickel and copper deposition were achieved.

Synthesis of Zinc Oxide Nanostructures on Graphene/Glass Substrate via Electrochemical Deposition: Effects of Potassium Chloride and Hexamethylenetetramine as Supporting Reagents

The effects of the supporting reagents hexamethylenetetramine(HMTA)and potassium chloride(KCl)mixed in zinc nitrate hexahydrate(Zn(NO3)2 6H2O)on the morphological,structural,and optical properties of the resulting Zn O nanostructures electrodeposited on graphene/glass substrates were investigated.The supporting reagent HMTA does not increase the density of nanorods,but it does remarkably improve the smoothness of the top edge surfaces and the hexagonal shape of the nanorods even at a low temperature of 75°C.Hydroxyl(OH-)ions from the HMTA suppress the sidewall growth of non-polar planes and promote the growth of Zn O on the polar plane to produce vertically aligned nanorods along the c axis.By contrast,the highly electronegative chlorine(Cl-)ions from the supporting reagent KCl suppress the growth of Zn O on the polar plane and promote the growth on non-polar planes to produce vertical stacking nanowall structures.HMTA was found to be able to significantly improve the crystallinity of the grown Zn O structures,as indicated by the observation of much lower FWHM values and a higher intensity ratio of the emission in the UV region to the emission in the visible region.Equimolar mixtures of Zn(NO3)2 6H2O and the supporting reagents HMTA and KCl seem to provide the optimum ratio of concentrations for the growth of high-density,uniform Zn O nanostructures.The corresponding transmittances for such molar ranges are approximately 55–58%(HMTA)and 63–70%(KCl),which are acceptable for solar cell and optoelectronic devices.

Additive-aided electrochemical deposition of bismuth telluride in a basic electrolyte

A new basic electrolyte with two cationic plating additives, polydiaminourea and polyaminosulfone, was investigated for the electrochemical deposition of the bismuth telluride film on a nickel-plated copper foil. Tellurium starts to deposit at a higher potential （-0.35 V） than bismuth （-0.5 V） in this electrolyte. The tellurium-to-bismuth ratio increases while the deposition potential declines from -1 to -1.25 V, indicating a kinetically quicker bismuth deposition at higher potentials. The as-deposited film features good adhesion to the substrate and smooth morphology, and has a nearly amorphous crystal structure disclosed by X-ray diffraction patterns.

Fabrication of ZnO nanoparticles-embedded hydrogenated diamond-like carbon films by electrochemical deposition technique

ZnO nanoparticles-embedded hydrogenated diamond-like carbon （ZnO-DLC） films have been prepared by electro- chemical deposition in ambient conditions. The morphology, composition, and microstructure of the films have been investigated. The results show that the resultant films are hydrogenated diamond-like carbon films embedded with ZnO nanoparticles in wurtzite structure, and the content and size of the ZnO nanoparticles increase with increasing deposition voltage, which are confirmed by X-ray photoelectron spectroscopy （XPS）, Raman, and transmission electron microscope （TEM）. Furthermore, a possible mechanism used to describe the growth process of ZnO-DLC films by electrochemical deposition is also discussed.

High performance Cu2O film/ZnO nanowires self-powered photodetector by electrochemical deposition

Self-powered photodetectors based on nanomaterials have attracted lots of attention for several years due to their various advantages.In this paper,we report a high performance Cu2O/ZnO self-powered photodetector fabricated by using electrochemical deposition.ZnO nanowires arrays grown on indium-tin-oxide glass are immersed in Cu2O film to construct type-Ⅱband structure.The Cu2O/ZnO photodetector exhibits a responsivity of 0.288 mA/W at 596 nm without bias.Compared with Cu2O photoconductive detector,the responsivity of the Cu2O/ZnO self-powered photodetector is enhanced by about two times at 2 V bias.It is attributed to the high power conversion efficiency and the efficient separation of the photogenerated electron-hole pairs,which are provided by the heterojunction.The outstanding comprehensive performances make the Cu2O film/ZnO nanowires self-powered photodetector have great potential applications.

Formation and Characterization of Europium Bisphthalocyanine Organic Nanowires by Electrochemical Deposition

Europium bisphthalocyanine (EuPc2) nanowires were prepared by electrochemical deposition method. Scanning electron microscopy (SEM) images show the evolution of the morphologies of nanowires obtained under different deposition time (Td). The optical properties of europium bisphthalocyanine films were studied by UV-Vis absorption spectra. The morphology of EuPc2 nanowires could be controlled by changing deposition conditions, which provides a useful method to make organic nanowires.

Thermoelectric properties of Indium doped skutterudite thick film synthesized by a facile technique of electrochemical deposition

Doped/filled skutterudites are much studied materials due to their excellent thermoelectric performance.However,their synthesis and preparation is complicated.This work synthesized indium(In)doped cobalt triantimonide(CoSb_(3))skutterudite thick films using a facile electrochemical deposition technique through chronoamperometric steps for 2 h.The nominal composition of In element is found in the range of 0.55e0.23 for a stoichiometric condition of In doped CoSb_(3)thick films.The early crystal growth of In doped films shows instantaneous nucleation and is controlled by the charge transfer process with diffusion coefficient,D of 10^(-5)cm^(2)/s.The incorporation of In into the interstitial sites of CoSb_(3)cages is evident from the lattice constant(a)expansion as observed in XRD.The optimum Seeback coefficient(S)of the 0.5 mmol In doped CoSb_(3)thick film is89.84 mV/K at 282 K,due to an increase in the carrier concentration(n~10^(20)cm^(-3)).The negative S is due to the electron donor behaviour of the In.Meanwhile,high electrical conductivity,s value(14.26 kS/m)contributes to a power factor(S2s)increment of 115.11 mW/(m$K2).The result shows a promising thermoelectric property of doped skutterudite synthesized by electrochemical deposition technique.

Effect of Amino-,Methyl- and Epoxy-Silane Coupling as a Molecular Bridge for Formatting a Biomimetic Hydroxyapatite Coating on Titanium by Electrochemical Deposition

The objective of this study was to determine the role of functional groups of silane coupling on bioactive titanium （Ti） surface by electrochemical deposition, and calcium phosphate （CAP） coating, as well as bone cell adhesion and proliferation. Methyl group （-CH3）, amino group （-NH2）, and epoxy group （-glyph name--C（O）C） were introduced onto the bioactive Ti surface using self-assembled monolayers （SAMs） with different silane coupling agents as molecular bridges. The effect of the surface functional groups on the growth features of the CaP crystals was analyzed （including chemical compositions, element content, minerals morphology and crystal structure etc.）. CH3-terminated SAMs showed a hydrophobic surface and others were hydrophilic by contact angle measurement; NH2-terminated SAMs showed a positive charge and others were negatively charged using zeta-potential measurement. Scanning electron microscopy results confirmed that flower-like structure coatings consisting of various pinpoint-like crystals were formatted by different functional groups of silane coupling, and the CaP coatings were multicrystalline consisting of hydroxyapatite （HA） and precursors. CaP coating of CH3-terminated SAMs exhibited more excellent crystallization property as compared to coatings of --NH2 and -C（O）C groups. In vitro MC3T3- El cells adhesion and proliferation were performed. The results showed that CaP coatings on silane coupling functionalized surfaces supported cell adhesion and proliferation. Thus, these functional groups of silane coupling on Ti can form homogeneous and oriented nano-CaP coatings and provide a more biocompatible surface for bone regeneration and biomedical applications.

Intrinsic thermal stability of inverted perovskite solar cells based on electrochemical deposited PEDOT

Thermal stability of perovskite materials is an issue impairing the long-term operation of inverted perovskite solar cells(PSCs). Herein, the thermal attenuation mechanism of the MAPb I3films that deposited on two different hole transport layers(HTL), poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate)(PEDOT:PSS) and poly(3,4-ethylenedioxythiophene)(PEDOT), is comprehensively studied by applying a heat treatment at 85℃. The thermal stress causes the mutual ions migration of I, Pb and Ag through the device, which leads to the thermal decomposition of perovskite to form Pb I2. Interestingly, we find that I ions tend to migrate more towards electron transport layer(ETL) during heating, which is different with the observation of I ions migration towards HTL when bias pressure is applied. Moreover, the use of electrochemical deposited PEDOT as HTL significantly decreases the defect density of MAPb I3films as compared to PEDOT:PSS supported one. The electrochemical deposition PEDOT has good carrier mobility and low acidity, which avoids the drawbacks of aqueous PEDOT:PSS. Accordingly, the inverted PSCs based on PEDOT show superior durability than that with PEDOT:PSS. Our results reveal detailed degradation routes of a new kind of inverted PSCs which can contribute to the understanding of the failure of thermal-aged inverted PSCs.

Electrochemical deposition of uranium oxide with an electrocatalytically active electrode using double potential step technique

The development of effective uranium-removal techniques is of great significance to the environment and human health.In this work,a double potential step technique(DPST)was applied to remove U(VI)from uranium-containing wastewater using a carbon felt electrode modified by graphene oxide/phytic acid composite(GO-PA@CF).The application of DPST can inhibit water splitting and prevent GO-PA from adsorbing other interfering ions in wastewater.The GO-PA composite can effectively accelerate the electrochemical reduction rate of U(VI),which significantly improved the electrochemical deposition rate of uranium oxide.As a result,the maximum removal efficiency and maximum removal capacity of GOPA@CF electrode reached 98.7%and 1149.3 mg/g,respectively.The removal efficiency remained 97.2%after five cycles of reuse.Moreover,the removal efficiency of GO-PA@CF electrode can reach more than 70%in simulated wastewater.

H_2S Gas Sensor Based on Nanocrystalline ZnO Synthesized by Electrochemical-Deposition

ZnO nanocrystals were prepared by a direct current electrochemical deposition process under 3.0V working voltage and 30A/m^2 current density using zinc sulfate as raw materials.The nanocrystals were characterized by X-ray diffraction (XRD)and transmission electron microscopy(TEM).The results indicated that the nanocrystals are hexagonal wurtzite ZnO with particle size range of 25nm～40nm without any treating.Gas sensing properties of the sensors were tested by mixing a gas in air at static state;the tested results showed that the sensors based on nanocrystalline ZnO had satisfied gas sensing properties to H_2S gas at rather low temperature.

Corrosion Study of Two-step Deposition Coatings on Copper Foil

To improve corrosion inhibition performance of copper foil with a novel two-step electrochemical modification processes,the surface of 35μm copper foils was coated with graphene oxide(GO)via electrochemical method at first step,then was further coated with 3-aminopropyltrimethoxysilane(APTS)at the second step.For the first step the copper foil acted as anode,and as cathode for the second one(we labeled it as E-GO).Optimum coating parameters for the preparation of E-GO coating are 5 V and 1 min with ratio of APTS/deionized water(DI)1.5/98.5(v/v).The physicochemical properties of modified coating were studied by X-ray diffraction(XRD),scanning electron microscopy(SEM)and hydrophilicity test.Electrochemical behavior of different samples were also investigated.The experimental results indicate that anti-corrosion performance is significantly improved with two-step modified coating.And E-GO coating shows more positive corrosion potential and the highest corrosion resistance rate than others according to the Tafel curve.It is also found that surface hydrophobicity of E-GO coating is significantly improved.

Electrochemical characterization of ion selectivity in electrodeposited nickel hexacyanoferrate thin films

The ion selectivity of electrodeposited nickel hexacyanoferrate （NiHCF） thin films was investigated using electrochemical impedance spectroscopy （EIS） and cyclic voltammetry （CV）. NiHCF thin films were prepared by cathodic deposition on Pt and Al substrates. EIS and CV curves were determined in 1 mol/L （KNO3＋C5NO3） and 1 mol/L （NaNO3＋CsNO3） mixture solutions, which were sensitive to the concentration of Cs^＋ in the electrolytes. Experimental results show that all Nyquist impedance plots show depressed semicircles in the high-frequency range changing over into straight lines at lower frequencies. With increasing amounts of Cs^＋, the redox potentials in CV curves shift toward more positive values and the redox peaks broaden; the semicircle radius in corresponding EIS curves and the charge transfer resistance also increase. EIS combining CV is able to provide valuable insights into the ion selectivity of NiHCF thin films. 2008 University of Science and Technology Beijing. All rights reserved.

Localized electrodeposition micro additive manufacturing of pure copper microstructures

The fabrication of pure copper microstructures with submicron resolution has found a host of applications,such as 5G communications and highly sensitive detection.The tiny and complex features of these structures can enhance device performance during high-frequency operation.However,manufacturing pure copper microstructures remain challenging.In this paper,we present localized electrochemical deposition micro additive manufacturing(LECD-μAM).This method combines localized electrochemical deposition(LECD)and closed-loop control of atomic force servo technology,which can effectively print helical springs and hollow tubes.We further demonstrate an overall model based on pulsed microfluidics from a hollow cantilever LECD process and closed-loop control of an atomic force servo.The printing state of the micro-helical springs can be assessed by simultaneously detecting the Z-axis displacement and the deflection of the atomic force probe cantilever.The results showed that it took 361 s to print a helical spring with a wire length of 320.11μm at a deposition rate of 0.887μm s^(-1),which can be changed on the fly by simply tuning the extrusion pressure and the applied voltage.Moreover,the in situ nanoindenter was used to measure the compressive mechanical properties of the helical spring.The shear modulus of the helical spring material was about 60.8 GPa,much higher than that of bulk copper(~44.2 GPa).Additionally,the microscopic morphology and chemical composition of the spring were characterized.These results delineate a new way of fabricating terahertz transmitter components and micro-helical antennas with LECD-μAM technology.

Cadmium selenide-sensitized upright-standing mesoporous zinc oxide nanosheets for efficient photoelectrochemical H_2 production

Cadmium selenide(Cd Se)-sensitized upright-standing mesoporous zinc oxide(ZnO) nanosheets were prepared via a chemical bath deposition followed by annealing and electrochemical deposition of Cd Se quantum dots(QDs). The Cd Se QDs absorb visible photons under sunlight illumination, promoting electrons from the valence band to the conduction band of Cd Se, which then quickly transfer to ZnO followed by the external load to the Pt counter electrode for water reduction. The as-prepared Cd Se/ZnO nanosheets show promising photoelectrochemical activities for hydrogen generation.

Photoactive area modification in bulk heterojunction organic solar cells using optimization of electrochemically synthesized ZnO nanorods

In this work, ZnO nanorod arrays grown by an electrochemical deposition method are investigated. The crucial parameters of length, diameter, and density of the nanorods are optimized over the synthesize process and nanorods growth time. Crystalline structure, morphologies, and optical properties of ZnO nanorod arrays are studied by different techniques such as x-ray diffraction, scanning electron microscope, atomic force microscope, and UV-visible transmission spectra. The ZnO nanorod arrays are employed in an inverted bulk heterojunction organic solar cell of Poly （3-hexylthiophene）：[6- 6] Phenyl-（6） butyric acid methyl ester to introduce more surface contact between the electron transporter layer and the active layer. Our results show that the deposition time is a very important factor to achieve the aligned and uniform ZnO nanorods with suitable surface density which is required for effective infiltration of active area into the ZnO nanorod spacing and make a maximum interfacial surface contact for electron collection, as overgrowing causes nanorods to be too dense and thick and results in high resistance and lower visible light transmittance. By optimizing the thickness of the active layer on top of ZnO nanorods, an improved efficiency of 3.17% with a high FF beyond 60% was achieved.

High-performance magnesium ion asymmetric Ppy@FeOOH//Mn3O4 micro-supercapacitor

Micro-supercapacitors(MSCs)are attractive electrochemical energy storage devices owing to their high power density and extended cycling stability.However,relatively low areal energy density still hinders their practical applications.Here,an asymmetric Mg ion MSC with promising high energy density is fabricated.Firstly,indium tin oxide(ITO)NWs were synthesized by chemical vapor deposition as the excellent current collector.Subsequently,nanostructured Mn_(3)O_(4)and Ppy@FeOOH were deposited on the laser-engraved interdigital structure ITO NWs electrodes as the positive and negative electrodes,respectively.Beneficial from the hierarchical micro-nano structures of active materials,high conductive electron transport pathways,and charge-balanced asymmetric electrodes,the obtained MSC possesses a high potential window of 2.2 V and a high areal capacitance of 107.3 mF cm^(-2)at 0.2 mA cm^(-2).The insitu XRD,VSM,and ex-situ XPS results reveal that the primary energy storage mechanism of Mg ions in negative FeOOH electrode is Mg ions de-/intercalation and phase transition reaction of FeOOH.Furthermore,the MSC exhibits a high specific energy density of 71.18μWh cm^(-2)at a power density of 0.22 mWh cm^(-2)and capacitance retention of 85%after 5000 cycles with unvaried Coulombic efficiency.These results suggest promising applications of our MSC in miniaturized energy storage devices.

Oxidation Resistance of Fe-13Cr Alloy with Micro-Laminated (ZrO_2-Y_2O_3)/(Al_2O_3-Y_2O_3) Films

The micro-laminated （ZrO2-Y2O3）/（Al2O3-Y2O3） composite films were prepared on the surface of Fe-13Cr alloy by an electrochemical process and a sintering process alternately. High-resolution field emission scanning electron microscopy （FE-SEM） was used to characterize the laminated films, indicating that the micro-laminated （ZrO2-Y2O3）] （Al2O3-Y2O3） films have nano-structures. SEM, EDS and mass gain measurement were adopted to study the oxidation resistance of films on Fe-13Cr alloy. It is proved that such micro-laminated films are more effective than ZrO2-Y2O3 or Al2O3-Y2O3 films to resist the oxidation of the alloy, and the oxidation resistance is increased with increasing layers in micro-laminated films. These beneficial effects can be contributed to the mechanism, by which such micro-laminated （ZrOE- YEO3）/（Al2O3-Y2O3） composite film combines all the beneficial effects and overcomes all the disadvantages of both ZrOE- Y2O3 film and Al2O3-Y2O3 film during oxidation of alloy.

Preparation of Au NPs/ZnO NTs Hybrid Array and Its Photo Catalytic Performance for MO

X-ray diffraction, scanning electron microscopy and transmission electron microscopy were employed to investigate the microstructure and morphology of Au NPs/ZnO NTs, and their photo-catalytic capability was assessed to a nicety. The results demonstrated that the diameter and the wall thickness of ZnO nanotube were about 200 and 50 nm, respectively. The diameter of Au nanoparticle was about 30 nm. The characterization on the photo-catalytic capability of the Au-ZnO nanotube hybrid indicated that the degradation of methyl orange was 80% within 4 h. Controlled experiments have shown that Au-Zn O nanotube hybrid presents superior photo-catalytic capability to both bare ZnO nanorod and Au-ZnO nanorod hybrid indicated that the degradation procedure of methyl orange.