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At least 217 records · Page 12

Combined Rotating Disk Slurry Electrodeposition–Spontaneous Galvanic Displacement for Pt-M (M = Co, Ni, and Cu) Catalyst Synthesis for the Oxygen Reduction Reaction in Alkaline Media

Here, platinum-modified first-row transition-metal catalyst (M = Ni, Co, and Cu) nanoparticles on a carbon black Vulcan XC-72R (CBV) support were synthesized using rotating disk slurry electrodeposition (RoDSE) followed by spontaneous galvanic displacement (SGD) reactions. These RoDSE–SGD catalysts were evaluated for the oxygen reduction reaction (ORR) in 0.1 M KOH using rotating disk electrode techniques. The Ni and Co RoDSEs were done by using an electrochemical applied potential of -0.75 V versus the RHE and for Cu, -0.80 V versus the RHE using a CBV slurry solution containing 0.1 M KClO 4 . These metal nanoparticles on CBV (M/CBV) catalysts were modified with a Pt precursor via a spontaneous galvanic displacement (SGD) reaction, producing a Pt-M/CBV material to catalyze the ORR in an alkaline medium. High-resolution scanning transmission electron microscopy (HR-STEM) analysis indicates that the PtM/CBV samples include M clusters and Pt single atoms. The ORR characterization measurements were done under a controlled temperature (25.0 °C) and with a mass loading of 100 μg/cm 2 on a glassy carbon (GC) rotating disk electrode at 1600 rpm. The PtCo/CBV showed the highest ORR mass activity of 0.741 A/mgPt at 0.90 V versus the reversible hydrogen electrode (RHE) compared with commercial Pt/CBV. The M/CBV RoDSE catalysts were also tested for the oxygen evolution reaction (OER), and Ni/CBV provided the lowest overpotential of 450 mV at 10 mA/cm 2 disk in 0.1 M KOH.

30 DIRECT ENERGY CONVERSION↗

Electrodeposition of Au/Ag bimetallic dendrites assisted by Faradaic AC-electroosmosis flow

Au/Ag bimetallic dendrites were synthesized successfully from the corresponding aqueous solution via the AC electrodeposition method. Both of the morphologies and compositions could be tuned by the electrolyte concentration and AC frequency. The prepared bimetallic dendrites were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and UV–vis spectroscopy. The underlying dendrite growth mechanism was then proposed in the context of the Directed Electrochemical Nanowires Assembly (DENA) models. Owing to the unscreened voltage dropping in the electrolyte bulk, electromigration dominates the species flux process, and cations tend to accumulate in areas with strong electric field intensity, such as electrode edges. Moreover, Faradaic AC-electro-osmosis (ACEO) flow could increase the effective diffusion layer thickness in these areas during the electrochemical reaction, and leads to dendrite growth. Further Micro-Raman observations illustrated that the Au/Ag bimetallic dendrites exhibited pronounced surface-enhanced Raman scattering (SERS) activity, using 4-mercaptopyridine (4-MP) as model molecules.

36 MATERIALS SCIENCE↗

Magnetic signature of granular superconductivity in electrodeposited Pb nanowires

Nanocrystalline freestanding Pb nanowires ∼200 nm in diameter were fabricated by electrodeposition into track etched polycarbonate membranes in order to study their superconducting properties. Their superconducting critical temperature, as determined by measuring the Meissner effect, was the same as for bulk Pb, but their critical field was greatly enhanced up to ∼3000 Oe. By assuming the wires consisted of spherical superconducting grains, an estimated grain size r = 60 ± 25 nm was obtained from the magnetization measured as a function of the applied magnetic field at a fixed temperature. An independent estimate for r = 47 ± 12 nm, in good agreement with the previous one, was obtained from the magnetization measured as a function of temperature at a fixed applied magnetic field. Transmission electron microscopy was used to characterize grain size at the wire edges, where a grain size in agreement with the magnetic studies was observed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Experimental studies and micromagnetic simulations of electrodeposited Co nanotube arrays

Magnetic hollow nanotubes of cobalt forming close-packed arrays are synthesized by controlling the growth during electrodeposition in AAO template. Superconducting quantum interference device (SQUID) magnetometry is used to experimentally measure the static magnetization of the array of nanotubes. Excellent qualitative agreements of SQUID and micromagnetic simulations for static measurements are observed. This motivates us to evaluate dynamic response measurements via micromagnetic simulations. The coercivity simulated along the longitudinal axis of the nanotube is found increase with the length of isolated as well as for array of nanotubes. The effect of interactions is also clearly observed both in static as well as in dynamic evaluations. The interactions cause reduction in coercivity along with the switching which depends upon the length of the nanotubes. The calculation for FMR modes also indicates that propagation of the spin waves are greatly influenced by the hollow centre of nanotube as compare to nanowire and support to maintain the stable vortex configuration. For array of nanotubes, multiple peaks are found over larger number of frequencies which is anticipated due the interactions between nanotubes. Simulation for bias field and angular dependence of spin wave modes also yields a significant influenced by the presence of neighbouring nanotubes.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Preparation and characterization of electrodeposited cobalt nanowires

Electrochemical deposition technique has been used to deposit cobalt nanowires into the nano sized channels of Anodized Aluminium Oxide (AAO) templates. CoCl{sub 2}М‡6H2O salt solution was used, which was buffered with H{sub 3}BO{sub 3} and acidified by dilute H{sub 2}SO{sub 4} to increase the plating life and control pH of the solution. Thin film of copper around 150 nm thick on one side of AAO template coated by e-beam evaporation system served as cathode to create electrical contact. FESEM analysis shows that the as-deposited nanowires are highly aligned, parallel to one another and have high aspect ratio with a reasonably high pore-filing factor. The TEM results show that electrodeposited cobalt nanowires are crystalline in nature. The Hysteresis loop shows the magnetization properties for in and out of plane configuration. The in plane saturation magnetization (Ms) is lower than out of plane configuration because of the easy axis of magnetization is perpendicular to nanowire axis. These magnetic nanowires could be utilized for applications such as spintronic devices, high density magnetic storage, and magnetic sensor applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effect of pulse frequency on microstructural, nanomechanical, and wear properties of electrodeposited Ni–TiN composite coatings

The current paper reports successful syntheses of Ni–TiN composite coatings by pulse electrodeposition. The effect of pulse frequency on the microstructures, nanomechanical, and wear properties of the coatings was investigated using transmission electron microscopy, X–ray diffraction, nanoindenter, scanning electron microscopy, and wear test instrument. The results showed that the Ni–TiN composite coating prepared at the pulse frequency of 100 Hz showed the presence of a less number of TiN particles and some degrees of aggregation in micro-regions. By contrast, in the Ni–TiN coating deposited at the pulse frequency of 500 Hz, the TiN particles were large in number and dispersed homogeneously, thereby, offering the coating a uniform and fine structure. The average grain diameters of Ni and TiN in the coating prepared at 100 Hz were 154.7 and 44.8 nm, respectively, whereas those for the coating prepared at 500 Hz were 67.3 and 25.9 nm, respectively. The maximum TiN content in the Ni-TiN coating deposited at 800 Hz was approximately 10.5 wt. %. The maximum microhardness and the Young's modulus values for the Ni–TiN composite coatings deposited at 800 Hz were 35.7 GPa and 167.4 GPa, respectively. Furthermore, the Ni–TiN composite coating prepared at 100 Hz had more severe damages, whereas the morphologies of worn surface of the coatings deposited at 500 Hz and 800 Hz were smooth and only a few small pits appeared on the surface.

36 MATERIALS SCIENCE↗

Electrodeposition of Zn based nanostructure thin films for photovoltaic applications

We present here a systematic study on the synthesis thin films of various ZnO, CdO, Zn{sub x}Cd{sub 1-x} (O) and ZnTe nanostructures by electrodeposition technique with ZnCl{sub 2,} CdCl{sub 2} and ZnSO{sub 4} solution as starting reactant. Several reaction parameters were examined to develop an optimal procedure for controlling the size, shape, and surface morphology of the nanostructure. The results showed that the morphology of the products can be carefully controlled through adjusting the concentration of the electrolyte. The products present well shaped Nanorods arrays at specific concentration and temperature. UV-VIS spectroscopy and X-ray diffraction results show that the product presents good crystallinity. A possible formation process has been proposed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Electrodeposited nanostructured MnO{sub 2} for non-enzymatic hydrogen peroxide sensing

Electrodeposited MnO{sub 2} nanostructure was synthesized on indium tin oxide coated glass electrode by cyclic voltammetry. The as obtained samples were subsequently characterized by atomic force microscopy and their electro-catalytic response towards hydrogen peroxide in alkaline medium of 0.1M NaOH was studied using cyclic voltammetry and amperometry.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Structural characterization of InSb thin films grown by electrodeposition

In the present work we have grown InSb thin films on brass substrates, using the electrodeposition technique. The electrochemical baths used in the growth were made up of aqueous solutions of InCl{sub 3} and SbCl{sub 3} mixed together in various proportions. The films grown were characterized by X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Energy Dispersive Analysis of X-rays (EDAX). Compositional studies show that stoichiometric InSb films can be prepared from a bath containing 0.05M InCl{sub 3} and 0.04M SbCl{sub 3}. XRD studies reveal that the films grown are polycrystalline having the zinc blende structure with (111) orientation. Crystallite size, dislocation density and strain were calculated using the XRD results. Optical transmission spectra were recorded using an FTIR spectrophotometer. The value of direct band gap was found to be around 0.20 eV for the thin films having the best stoichiometry.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Temperature dependent barrier height and ideality factor of electrodeposited n-CdSe/Cu Schottky barrier diode

This article reports the measurement of temperature-dependent barrier height and ideality factor of n-CdSe/Cu Schottky barrier diode. The Cadmium Selenide (CdSe) thin films have been deposited by simple electrodeposition technique. The XRD measurements ravels the deposited single phase CdSe films are highly oriented on (002) plane and the average particle size has been calculated to be ~18 nm. From SEM characterization, it is clear that the surface of CdSe thin films are continuous, homogeneous and the film is well adhered to the substrate and consists of fine grains which are irregular in shape and size. Current-Voltage characteristics have been measured at different temperatures in the range (298 K – 353 K). The barrier height and ideality factor are found to be strongly temperature dependent. The inhomogenious barrier height increases and ideality factor decreases with increase in temperature. The expectation value has been calculated and its value is 0.30 eV.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Electrodeposited Co{sub 93.2}P{sub 6.8} nanowire arrays with core-shell microstructure and perpendicular magnetic anisotropy

We demonstrate the formation of an unusual core-shell microstructure in Co{sub 93.2}P{sub 6.8} nanowires electrodeposited by alternating current (ac) in an alumina template. By means of transmission electron microscopy, it is shown that the coaxial-like nanowires contain amorphous and crystalline phases. Analysis of the magnetization data for Co-P alloy nanowires indicates that a ferromagnetic core is surrounded by a weakly ferromagnetic or non-magnetic phase, depending on the phosphor content. The nanowire arrays exhibit an easy axis of magnetization parallel to the wire axis. For this peculiar composition and structure, the coercivity values are 2380 ± 50 and 1260 ± 35 Oe, parallel and perpendicular to the plane directions of magnetization, respectively. This effect is attributed to the core-shell structure making the properties and applications of these nanowires similar to pure cobalt nanowires with an improved perpendicular anisotropy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enhanced room temperature ferromagnetism in electrodeposited Co-doped ZnO nanostructured thin films by controlling the oxygen vacancy defects

We report the growth of un-doped and cobalt doped ZnO nanostructures fabricated on FTO coated glass substrates using electrodeposition method. A detailed study on the effects of dopant concentration on morphology, structural, optical, and magnetic properties of the ZnO nanostructures has been carried out systematically by varying the Co concentration (c.{sub Co}) from 0.01 to 1 mM. For c.{sub Co }≤ 0.2 mM, h-wurtzite phase with no secondary phases of Co were present in the ZnO nanostructures. For c.{sub Co} ≤ 0.2 mM, the photoluminescence spectra exhibited a decrease in the intensity of ultraviolet emission as well as band-gap narrowing with an increase in dopant concentration. All the doped samples displayed a broad emission in the visible range and its intensity increased with an increase in Co concentration. It was found that the defect centers such as oxygen vacancies and zinc interstitials were the source of the visible emission. The X-ray photoelectron spectroscopy studies revealed, Co was primarily in the divalent state, replacing the Zn ion inside the tetrahedral crystal site of ZnO without forming any cluster or secondary phases of Co. The un-doped ZnO nanorods exhibited diamagnetic behavior and it remained up to a c.{sub Co} of 0.05 mM, while for c.{sub Co }> 0.05 mM, the ZnO nanostructures exhibited ferromagnetic behavior at room temperature. The coercivity increased to 695 G for 0.2 mM Co-doped sample and then it decreased for c.{sub Co }> 0.2 mM. Our results illustrate that up to a threshold concentration of 0.2 mM, the strong ferromagnetism is due to the oxygen vacancy defects centers, which exist in the Co-doped ZnO nanostructures. The origin of strong ferromagnetism at room temperature in Co-doped ZnO nanostructures is attributed to the s-d exchange interaction between the localized spin moments resulting from the oxygen vacancies and d electrons of Co{sup 2+} ions. Our findings provide a new insight for tuning the defect density by precisely controlling the dopant concentration in order to get the desired magnetic behavior at room temperature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Fabrication of single phase p-CuInSe{sub 2} nanowire arrays by electrodeposited into anodic alumina templates

Single-phase CuInSe{sub 2} nanowire (NW) arrays were prepared at various pH values in a heated electrolyte by using pulse electrodeposition techniques and an anodized aluminum oxide template. X-ray diffraction showed that the CuInSe{sub 2} NW nucleation mechanism received H{sup +} constraints when the NWs were deposited at pH 1.7 with a (112) orientation and annealed at 550 °C. The CuInSe{sub 2} NW band gap was determined to be approximately 1 eV through optical measurements. Transmission electron microscopy showed that at the pH value of 1.7, small particles of the single-phase CuInSe{sub 2} NWs aligned along the crystallographic direction are nucleated to form large particles. Scanning electron microscopy revealed that the NW diameter and the length were 80 nm and 2.3 μm, respectively. From Mott–Schottky and Ohmic contact plots, the CuInSe{sub 2} NWs were found to be p-type semiconductors, and their work function was estimated to be approximately 4.69 eV.

36 MATERIALS SCIENCE↗

Effect of different nickel precursors on capacitive behavior of electrodeposited NiO thin films

In the present study, the effect of nickel precursors containing different anions like nitrate, chloride and sulphate on the morphology and pseudocapacitance behavior of NiO is investigated. The NiO samples were prepared by using a potentiondynamic electrodeposition technique in the three electrode cell. Cyclic voltammetry technique was exploited for potentiodynamic deposition of the films. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), etc. The XRD reveals the cubic crystal structure for all samples. The SEM micrograph shows nanoflakelike, up grown nanoflakes and honeycomb like nanostructured morphologies for nitrate, chloride and sulphate precursors respectively. The capacitive behavior of these samples was recorded using cyclic voltammetry (CV), charge-discharge and electrochemical impedance spectroscopy (EIS) in 1 M KOH electrolyte. The specific capacitance values of NiO samples obtained using CV for nitrate, chloride and sulphate precursors were 136, 214 and 893 Fg{sup −1} respectively, at the scan rate of 5 mVs{sup −1}. The charge discharge study shows high specific energy for the sample obtained from sulphate (23.98 Whkg{sup −1}) as compared to chloride (9.67 Whkg{sup −1}) and nitrate (4.9 Whkg{sup −1}), whereas samples of cholride (13.9 kWkg{sup −1} and nitrate (10.5 kWkg{sup −1}) shows comparatively more specific power than samples obtained from sulphate (7.6 kWkg{sup −1}). The equivalent series resistance of NiO samples observed from EIS study are 1.34, 1.29 and 1.27 Ω respectively for nitrate, chloride and sulphate precursors. These results emphasizes that the samples obtained from sulphate precursors provides very low impedance through honeycomb like nanostructured morphology which supports good capacitive behavior of NiO.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electrodeposition of Fe{sub 2}O{sub 3} nanoparticles and its supercapacitive properties

Fe{sub 2}O{sub 3} metal oxide nanoparticles are synthesized by electrodeposition method on stainless steel substrate. The crystal structure and surface morphological studies of the obtained metal oxide thin film are carried out by using X-ray diffraction (XRD) technique and Scanning Electron Microscopy (SEM) respectively. The electrochemical properties of Fe{sub 2}O{sub 3} thin film like Cyclic Voltammetry (CV), Galvonostatic Charge-Discharge (GCD) and Electrochemical Impedance Spectroscopy (EIS) are studied in a bath of 0.5 M Na{sub 2}SO{sub 4} as electrolyte. The observed specific capacitance shows improved values 135 Fg{sup −1} at 5 mVs{sup −1} scan rate. The electrochemical stability of Fe{sub 2}O{sub 3} electrode is investigated using cyclic voltammetry for 1000 cycles at a scan rate 50 mVs{sup −1}. The Fe{sub 2}O{sub 3} electrode exhibits superior cycling stability with only 4-5% capacitance loss after one thousand cycles. The values of specific power and specific energy of Fe{sub 2}O{sub 3} electrode obtained from Galvonostatic charge discharge studies are 2250 W.kg{sup −1} and 63.15 Wh.kg{sup −1} respectively at current density 1 A/g. From all the electrochemical properties of Fe{sub 2}O{sub 3} electrode, it indicates that it will be promising electrode material for supercapacitor application.

36 MATERIALS SCIENCE↗

Multiphysics simulation of microscale copper printing by confined electrodeposition using a nozzle array

3D printing of metals at the microscale and nanoscale is crucial to produce high-density interconnects and intricate structures in electronic devices. Conventional melting and sintering processes are not suitable for these scales due to a reliance on individual metal particles in the size range of tens of micrometers. Confined electrodeposition (CED) is an established alternative to conventional metal 3D printing processes in which an electrolyte is used to selectively induce deposition of the metal on the printing surface. However, commercialization and efficiency of this process have been limited due to a reliance on sub-micrometer nozzles to achieve desirable deposition rates and single nozzle to achieve uniformity of printed structures. Here, we address these challenges by computationally analyzing an array of microscale nozzles. We tailor the convection within the electrolyte to alter both deposition rate and geometric uniformity of the printed structures. The results show that for large nozzles the evaporation alone is not sufficient to obtain high deposition rates, yet an external pressure can be used to increase deposition and alter uniformity (thickness) of printed structures. Our results can be used to design and analyze new experiments toward parallel multi-nozzle deposition using CED toward high-throughput metal printing.

3D printing↗

Platinum Electrodeposition for Supported ALD Templated Foam Hohlraum Liners

Two commercially available platinum plating solutions (Platanex III and Platanex Luna) were evaluated for the electrodeposition of platinum layers on gold hohlraums and cylindrically shaped silver-gold ingots. The successful deposition of thin Pt layers on gold hohlraums as well as thick Pt layers on silver-gold alloys will allow for the integration of atomic layer deposition templated foam inside a hohlraum. We found that when the manufacturer’s recommendations for the Pt plating solutions were used, the coatings obtained were unacceptable because of cracking, poor adhesion, or thin and powdery Pt deposits. Therefore, alternative plating parameters were investigated, and the conditions resulting in acceptable coatings are reported here.

36 MATERIALS SCIENCE↗

On Controlling the Hydrophobicity of Nanostructured Zinc-Oxide Layers Grown by Pulsed Electrodeposition

The possibility of fabricating highly hydrophobic nanostructured zinc-oxide layers by the inexpensive method of pulsed electrodeposition from aqueous solutions without water-repellent coatings, adapted for large-scale production, is shown. The conditions of the deposition of highly hydrophobic nanostructured zinc-oxide layers exhibiting the “rose-petal” effect with specific morphology, optical properties, crystal structure and texture are determined. The grown ZnO nanostructures are promising for micro- and nanoelectronics as an adaptive material able to reversibly transform to the hydrophilic state upon exposure to ultraviolet radiation.

36 MATERIALS SCIENCE↗