Electrochemical studies on Zn/nano-CeO 2 electrodeposited composite coatings

The Zn-CeO 2 composite coatings through electrodeposition technique were successfully fabricated on mild steel substrate. As a comparison pure zinc coating was also prepared. The concentration of CeO 2 nanoparticles was varied in the electrolytic bath and the composites were electrodeposited both in the presence and absence of cetyltriammonium bromide (CTAB). The performance of the CeO 2 nanoparticles towards the deposition, crystal structure, texture, surface morphology and electrochemical corrosion behavior was studied. For characterizations of the electrodeposits, the techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM) were used. Both the additives ceria and surfactant polarize the reduction processes and thus influence the deposition process, surface nature and the electrochemical properties. The electrochemical experiments like potentiodynamic polarization and electrochemical impedance spectroscopic (EIS) studies carried out in 3.5 wt. NaCl solution explicit higher corrosion resistance by CeO 2 incorporated coating in the presence of surfactant. © 2012 Elsevier B.V. All rights reserved.

Morphology and electrochemical performance of graphene nanosheet array for Li-ion thin film battery

Highly branched and porous graphene nanosheet synthesized over different substrates as anode for Lithium ion thin film battery. These films synthesized by microwave plasma enhanced chemical vapor deposition at temperature 700 degrees C. Scanning electron microscopy and X-ray photo electron spectroscopy are used to characterize the film surface. It is found that the graphene sheets possess a curled and flower like morphology. Electrochemical performances were evaluated in swezelock type cells versus metallic lithium. A reversible capacity of 520 mAh/g, 450 mAh/g and 637 mAh/g was obtained after 50 cycles when current rate at 23 mu A cm(2) for CuGNS, NiGNS and PtGNS electrodes, respectively. Electrochemical properties of thin film anode were measured at different current rate and gave better cycle life and rate capability. These results indicate that the prepared high quality graphene sheets possess excellent electrochemical performances for lithium storage. (C) 2013 Elsevier Ltd. All rights reserved.

Effect of radio frequency power and thickness on the electrochemical properties of Li2-x MnO3-y thin films

In the present work, Li2-x MnO3-y (LMO) thin films have been deposited by radio frequency (RF) reactive magnetron sputtering using acid-treated Li2MnO3 powder target. Systematic investigations have been carried out to study the effect of RF power on the physicochemical properties of LMO thin films deposited on platinized silicon substrates. X-ray diffraction, electron microscopy, surface chemical analysis and electrochemical studies were carried out for the LMO films after post deposition annealing treatment at 500 A degrees C for 1 h in air ambience. Galvanostatic charge discharge studies carried out using the LMO thin film electrodes, delivered a highest discharge capacity of 139 mu Ah mu m(-1) cm(-2) in the potential window 2.0-3.5 V vs. Li/Li+ at 100 W RF power and lowest discharge capacity of 80 mu Ah mu m(-1) cm(-2) at 75 W RF power. Thereafter, the physicochemical properties of LMO films deposited using optimized RF power 100 W on stainless steel substrates has been studied in the thickness range of 70 to 300 nm as a case study. From the galvanostatic charge discharge experiments, a stable discharge capacity of 68 mu Ah mu m(-1) cm(-2) was achieved in the potential window 2.0-4.2 V vs. Li/Li+ tested up to 30 cycles. As the thickness increased, the specific discharge capacity started reducing with higher magnitude of capacity fading.

Photochemical Deposition of Co-Ac Catalyst on ZnO Nanorods for Solar Water Oxidation

The preparation of ZnO nanorod films decorated with cobalt-acetate (CoAc) electrocatalyst and its activity for photoelectrolysis of water have been demonstrated. The photochemically prepared CoAc catalyst is chemically and morphologically similar to the electrochemically prepared CoAc catalyst. The on-set potential of oxygen evolution reaction is lower on CoAc-ZnO photoanode in relation to bare ZnO photoanode. There is a three to four fold increase in photooxidation current of OER due to the presence of CoAc co-catalyst on ZnO. Thus, the photochemically prepared CoAc on ZnO is an alternative and efficient co-catalyst for photoelectrochemical oxygen evolution reaction. The enhancement in photocatalytic activity of ZnO by the CoAc catalyst photochemically deposited from acetate buffer solution is significantly greater than the cobalt-phosphate (CoPi) co-catalyst deposited from phosphate buffer solution. (C) The Author(s) 2015. Published by ECS. All rights reserved.

A Comparative Study on Electrochemical Behaviour of Co3O4 and Co3O4-MWCNTs for Supercapacitors

Co3O4 and Co3O4/MWCNTs were prepared by hydrothermal process under autogenous pressure in Teflon lined autoclave and calcined at 250 degrees C. Both samples were characterized by PXRD, FT-IR, SEM-EDS, TEM & FT-Raman to evaluate their surface and bulk properties. The PXRD pattern of the materials indicated the formation of cubic phase of Co3O4. FT-IR results showed the presence of metal oxygen bond in the samples. The SEM and TEM images of the Co3O4 / MWCNTs indicated spherical and cubic aggregates of metal oxide particles (10-30 nm) decorated both on the surface and inside the tubes of carbon nanotubes. The characteristic Ig and Id (graphitic and defects) Raman bands indicated the retention of tubular structure of MWCNTs even after the deposition of Co3O4. The calcined Co3O4-MWCNTs composites and Co3O4 exhibited specific capacitance of 284 & 205 F/g at a sweep rate of 2mVs(-1) in 6M KOH by cyclic voltammetry. The psuedocapacitance performances of calcined Co3O4-MWCNTs were found to be better than Co3O4. Chronopotentiometric studies made for the materials at a current density of 500mA/g indicated 100% columbic efficiency at 2000th cycle for Co3O4/ MWCNTs which is a better electrode material than Co3O4.

FexSi grown with mass-analyzed low-energy dual ion beam deposition

Heavily iron-implanted silicon was prepared by mass-analyzed low-energy dual ion beam deposition technique. Auger electron spectroscopy depth profiles indicate that iron ions are shallowly implanted into the single-crystal silicon substrate and formed 35 nm thick FexSi films. X-ray diffraction measurements show that as-implanted sample is amorphous and the structure of crystal is partially restored after as-implanted sample was annealed at 400degreesC. There are no new phases formed. Carrier concentration depth profile of annealed sample was measured by Electrochemical C-V method and indicated that FexSi film shows n-type conductivity while silicon substrate is p-type. The p-n junction is formed between FexSi film and silicon substrate showing rectifying effect. (C) 2003 Elsevier B.V. All rights reserved.

Electrical, electrochemical, and optical characterization of ceria films

Acceptor-doped ceria has been recognized as a promising intermediate temperature solid oxide fuel cell electrode/electrolyte material. For practical implementation of ceria as a fuel cell electrolyte and for designing model experiments for electrochemical activity, it is necessary to fabricate thin films of ceria. Here, metal-organic chemical vapor deposition was carried out in a homemade reactor to grow ceria films for further electrical, electrochemical, and optical characterization. Doped/undoped ceria films are grown on single crystalline oxide wafers with/without Pt line pattern or Pt solid layer. Deposition conditions were varied to see the effect on the resultant film property. Recently, proton conduction in nanograined polycrystalline pellets of ceria drew much interest. Thickness-mode (through-plane, z-direction) electrical measurements were made to confirm the existence of proton conductivity and investigate the nature of the conduction pathway: exposed grain surfaces and parallel grain boundaries. Columnar structure presumably favors proton conduction, and we have found measurable proton conductivity enhancement. Electrochemical property of gas-columnar ceria interface on the hydrogen electrooxidation is studied by AC impedance spectroscopy. Isothermal gas composition dependence of the electrode resistance was studied to elucidate Sm doping level effect and microstructure effect. Significantly, preferred orientation is shown to affect the gas dependence and performance of the fuel cell anode. A hypothesis is proposed to explain the origin of this behavior. Lastly, an optical transmittance based methodology was developed to obtain reference refractive index and microstructural parameters (thickness, roughness, porosity) of ceria films via subsequent fitting procedure.

Chemical and Electrochemical Behavior of Graphene-Covered Silicon Photoanodes

This dissertation describes efforts over the last five years to develop protective layers for semiconductor photoelectrodes based on monolayer or few-layer graphene sheets. Graphene is an attractive candidate for a protective layer because of its known chemical inertness, transparency, ease of deposition, and limited number of electronic states. Monolayer graphene was found to effectively inhibit loss of photocurrent over 1000 seconds at n-Si/aqueous electrolyte interfaces that exhibit total loss over photocurrent over 100 seconds. Further, the presence of graphene was found to effect only partial Fermi level pinning at the Si/graphene interface with respect to a range of nonaqueous electrolytes. Fluorination of graphene was found to extend the stability imparted on n-Si by the monolayer sheet in aqueous Fe(CN)₆^3-/4- electrolyte to over 100,000 seconds. It was demonstrated that the stability of the photocurrent of n-Si/fluorinated graphene/aqueous electrolyte interfaces relative to n-Si/aqueous electrolyte interfaces is likely attributable to the inhibition of oxidation of the silicon surface.

This dissertation also relates efforts to describe and define terminology relevant to the field of photoelectrochemistry and solar fuels production. Terminology describing varying interfaces employed in electrochemical solar fuels devices are defined, and the research challenges associated with each are discussed. Methods for determining the efficiency of varying photoelectrochemical and solar-fuel-producing cells from the current-voltage behavior of the individual components of such a device without requiring the device be constructed are described, and a range of commonly employed performance metrics are explored.

Deposition of low stress amorphous zinc tin oxide at ambient temperature using a remote plasma sputtering process suitable for delicate substrates

ZnxSnyOz thin films (<100nm thickness), deposited by remote sputtering from a metal target using a confined argon plasma and oxygen gas jet near the sample, were investigated for their material properties. No visible deformation or curl was observed when deposited on plastic. Materials were confirmed to be amorphous and range between 5 and 10 at.% Sn concentration by x-ray diffraction, x-ray photoemission spectroscopy and energydispersive x-ray spectroscopy. Factors affecting the material composition over time are discussed. Depletion of the Sn as the target ages is suspected. © The Electrochemical Society.

FexSi grown with mass-analyzed low-energy dual ion beam deposition

Heavily iron-implanted silicon was prepared by mass-analyzed low-energy dual ion beam deposition technique. Auger electron spectroscopy depth profiles indicate that iron ions are shallowly implanted into the single-crystal silicon substrate and formed 35 nm thick FexSi films. X-ray diffraction measurements show that as-implanted sample is amorphous and the structure of crystal is partially restored after as-implanted sample was annealed at 400degreesC. There are no new phases formed. Carrier concentration depth profile of annealed sample was measured by Electrochemical C-V method and indicated that FexSi film shows n-type conductivity while silicon substrate is p-type. The p-n junction is formed between FexSi film and silicon substrate showing rectifying effect. (C) 2003 Elsevier B.V. All rights reserved.

Ultrathin platinum-group metal coated hierarchical flowerlike gold microstructure: Electrochemical design and characterization

The deliberate tailoring of hierarchical flowerlike gold microstructure (HFGMs) at the ultrathin level is an ongoing challenge and could introduce opportunities for new fabrication and application in many fields. In this paper. a templateless, surfactantless, electrochemical strategy for fabrication of ultrathin platinum-group metal coated HFGMs is proposed. HFGMs were prepared by simple electrodeposition on an indium tin oxide (ITO) substrate.

Dendrimer films as matrices for electrochemical fabrication of novel gold/palladium bimetallic nanostructures

Electrodeposition of novel Au/Pd bimetallic nanostructures with dendrimer films as matrices has been reported. The dendrimers exhibited highly open structures arising from protonation of amines and this made them have good penetrability for solvent molecules. The unique properties of dendrimers obviously affected the morphologies and compositions of deposited bimetallic nanostructures compared with those from unmodified surfaces. Field-emitted scanning electron microscopy, energy dispersive spectroscopy, X-ray photoelectron spectroscopy and UV-vis spectroscopy were used to characterize these nanostructures.

Electrolytic Deposition and Diffusion of Lithium onto Magnesium-9 Wt Pct Yttrium Bulk Alloy in Low-Temperature Molten Salt of Lithium Chloride and Potassium Chloride

The electrolytic deposition and diffusion of lithium onto bulk magnesium-9 wt pct yttrium alloy cathode in molten salt of 47 wt pct lithium chloride and 53 wt pct potassium chloride at 693 K were investigated. Results show that magnesium-yttrium-lithium ternary alloys are formed on the surface of the cathodes, and a penetration depth of 642 mu m is acquired after 2 hours of electrolysis at the cathodic current density of 0.06 A center dot cm(-2). The diffusion of lithium results in a great amount of precipitates in the lithium containing layer. These precipitates are the compound of Mg41Y5, which arrange along the grain boundaries and hinder the diffusion of lithium, and solid solution of yttrium in magnesium. The grain boundaries and the twins of the magnesium-9 wt pct yttrium substrate also have negative effects on the diffusion of lithium.

Charge Transport Processes of Immobilized Heteropolyanions at Self-assembled Monolayer Modified Gold Electrode by Electrochemical Quartz Crystal Microbalance Measurement

The in situ electrochemical quartz crystal microbalance(EQCM) technique was used to investigate the ion transport of immobilized heteropolyanions at a self-assembled monolayer(SAM) modified gold electrode during electrochemical redox process. A mixed transfer method was presented to analyse the abnormal change of resonant frequency based on the simultaneous insertion/extraction of different ions. The results indicate that the migration of HSO4- anions was indispensable in the redox process of the heteropolyan ions in a I mol/L H2SO4 solution and played a key role in the abnormal change of the resonant frequency. Such a change was attributed to different packing densities derived by means of differently immobilized methods.

Combining chemical reduction with an electrochemical technique for the simultaneous detection of Cr(VI), Pb(II) and Cd(II)

This work herein reports the approach for the simultaneous determination of heavy metal ions including cadmium (Cd(II)), lead (Pb(II)), and chromium (Cr(VI)) using a bismuth film electrode (BFE) by anodic stripping voltammertry (ASV). The BFE used was plated in situ. Due to the reduction of Cr(VI) with H2O2 in the acid medium, on one hand, the Cr(III) was produced and Cr(VI) was indirectly detected by monitoring the content of Cr(III) using square-wave ASV. On the other hand, Pb(II) was also released from the complex between Pb(II) and Cr(VI). Furthermore, the coexistence of the Cd(II) was also simultaneously detected with Pb(II) and Cr(VI) in this system as a result of the formation of an alloy with Bi. The detection limits of this method were 1.39 ppb for Cd(II), 2.47 ppb for Pb(II) and 5.27 ppb for Cr(VI) with a preconcentration time of 120 s under optimal conditions (S/N = 3), respectively. Furthermore, the sensitivity of this method can be improved by controlling the deposition time or by using a cation-exchange polymer (such as Nafion) modified electrode.