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At least 109 records · Page 6

Surface coatings and catalyst production by electrodeposition

Electrodeposition and electrocodeposition in low gravity are discussed. The goal is to provide a better understanding of the role of convection and buoyancy in the mechanisms of formation of some electrodeposited surfaces, fluid flow in the vicinity of electrodepositing surfaces, the influence of a moving medium upon codeposition, the effect of gravity upon the dispersion (coagulation) of neutral particles that are desired for codeposition and preparation of improved surface coatings and metal catalysts.

May, Chester B.↗

Fabricating Copper Nanotubes by Electrodeposition

Copper tubes having diameters between about 100 and about 200 nm have been fabricated by electrodeposition of copper into the pores of alumina nanopore membranes. Copper nanotubes are under consideration as alternatives to copper nanorods and nanowires for applications involving thermal and/or electrical contacts, wherein the greater specific areas of nanotubes could afford lower effective thermal and/or electrical resistivities. Heretofore, copper nanorods and nanowires have been fabricated by a combination of electrodeposition and a conventional expensive lithographic process. The present electrodeposition-based process for fabricating copper nanotubes costs less and enables production of copper nanotubes at greater rate.

Yang, E. H.↗

Epitaxial Electrodeposition of Wide Bandgap Cuprous Bromide on Silver via a Silver Bromide Buffer Layer

Cuprous halides are an important class of wide bandgap p-type semiconductors used in opto-electronics. Cuprous bromide (CuBr) shows potential for short-wavelength devices due to a large exciton binding energy (108 meV) and near-ultraviolet bandgap (3.1 eV). However, the growth of high-quality epitaxial CuBr films by electrodeposition has remained a challenge. Here, we introduce a low-cost electrochemical procedure for producing epitaxial CuBr(111) on a Ag(111) substrate by a [111]-oriented silver bromide (AgBr) buffer layer. The AgBr buffer layer forms during the electrodeposition of the CuBr. The mismatch between CuBr(111) and AgBr(111) is –1.3%. A plausible mechanism for nucleation and growth of the epitaxial CuBr is proposed. X-ray techniques including high resolution X-ray diffraction and X-ray pole figures are used to determine the epitaxial relationship. CuBr(100) is also produced on a Ag(100) surface by a AgBr(100) buffer layer that is rotated in-plane 45° relative to the Ag(100) surface. In conclusion, this in-plane rotation reduces the lattice mismatch from +39.5% for an unrotated film to –1.4% for a 45° rotated film.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of Thick Tungsten Coating on Cu Alloy Substrate Prepared by Electrodeposition

The W coating with the thickness over 1 mm was obtained by pulse electrodeposition on large CuCrZr alloy in a Na{sub 2}WO{sub 4}–WO{sub 3} molten salt. The composition of this system keeps unchanged with the duration of electrodeposition. The coating’s structure, morphology and contents were investigated by XRD, XPS and SEM. The electrodepostion tungsten coating was compact and without void. The residual stress in surface of W coating was calculated to be a compressive stress with the value of 225 MPa. The W coating comprised an inner tooth-like layer and an outer columnar layer. The bonding strength between W coating and CuCrZr susbtrate was near 60 MPa; the thermal conductivity parallel to the crystal growth direction was measured to be 150.86 W m{sup −1} K{sup −1}.

36 MATERIALS SCIENCE↗

Trimethyl phosphate based neutral ligand room temperature ionic liquids for electrodeposition of rare earth elements

In this communication, a new class of task-specific ionic liquids (ILs) with cationic rare earth elements (REEs) is reported. These novel ILs have a wide electrochemical window of about 6 V, enabling direct electrodeposition of REE metals at room temperature. The ILs were prepared by dissolving bis(trifluoromethane)sulfonimide (NTf 2 – ) based rare earth salts (Ln(NTf 2 ) 3 ) (Ln:Lanthanide) in trimethyl phosphate (TMP) neutral ligand. Specifically, four REEs (Nd, Dy, Gd, and Pr) have been investigated in TMP based IL systems. All four metals were successfully deposited at room temperature. In conclusion, this demonstrates the applicability of the IL systems for electrodeposition of a wide range of REEs, which opens a new avenue of research for the quest to supplant high temperature molten salt systems for rare earth deposition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis of hyperbranched polymer films via electrodeposition and oxygen-tolerant surface-initiated photoinduced polymerization

Hypothesis Hyperbranched polymers, not only possess higher functionality, but are also easier to prepare compared to dendrimers and dendric polymers. Combining electrodeposition and surface-initiated photoinduced electron transfer-reversible addition-fragmentation chain transfer (SI-PET-RAFT) polymerization is hypothesized to be a novel strategy for preparing hyperbranched polymer films on conductive surfaces without degassing. Experiments In this study, polymer brush grafted films with four different architectures (i.e. linear, branched, linear- block -branched, and branched- block -linear) were prepared on gold-coated glass substrates using electrodeposition, followed by SI-PET-RAFT polymerization. The resulting film structure and thickness, surface topology, absorption property, and electrochemical behavior were confirmed by spectroscopy, microscopy, microbalance technique, and impedance measurement. Findings These hyperbranched polymer brushes were capable of forming a thicker but more uniformly covered films compared to linear polymer brush films, demonstrating that hyperbranched polymer films can be potentially useful for fabricating protective polymer coatings on various conductive surfaces.

36 MATERIALS SCIENCE↗

Geometric control of magnetic domain morphology in electrodeposited Ni rich NiPt mesoscopic wires

In this paper, we study the electrodeposited Ni—Pt magnetic wires, exploring the mechanisms by which changes in geometry and composition influence the local magnetic structure. The samples were prepared by electrodeposition, their elemental composition was analyzed by energy dispersive X-ray spectroscopy, and phase analysis was carried out by an X-ray diffraction measurement. Magnetic force microscopy measurements, and magnetic force microscopy measurements in magnetic field were carried out to study the domain morphology of the prepared samples. Magnetization characteristics were measured via vibrating sample magnetometry mode of a superconducting quantum interference device. Here, the results were analyzed and compared with micromagnetic simulations. It is shown that a strong perpendicular magnetic anisotropy is responsible for the characteristic checkerboard-like surface magnetization patterns, which can be tuned by geometrical constriction and Ni content. Understanding these relationships provides insights into the design of magnetic materials with tailored properties for advanced applications, like magnetic sensors.

Binary alloy↗

Experimental investigation of grain boundaries misorientations and nano twinning induced strengthening on addition of silicon carbide in pulse electrodeposited nickel tungsten composite coating

Nanoindentation was performed on silicon carbide (SiC) reinforced pulse electrodeposited nickel-tungsten (Ni-W) composite coating. Addition of 5 vol.% of SiC in Ni-W coating increased the hardness from 10.31 ± 0.65 GPa to 14.32 ± 0.63 GPa and elastic modulus from 119.74 ± 3.15 GPa to 139.26 ± 2.09 GPa. Increased hardness and elastic modulus directly translates to the improved strengthening in the coating. An experimental investigation of strengthening mechanism was carried out in Ni-W-5 vol.% SiC alloy. Two simultaneous phenomena viz. grain refinement and increased internal strain was observed, which increased the dislocation density from 5.51 × 10{sup 18} m{sup −2} to 1.346 × 10{sup 19} m{sup −2} on reinforcement of 5 vol.% of SiC in Ni-W coating. Increased dislocation density promoted the formation of grain boundary misorientations and nano twinning. Low angle grain boundary, high angle grain boundary and nano twinning were identified using high resolution transmission electron microscope (HR-TEM) image and their role in strengthening mechanism was discussed in details. - Highlights: • SiC reinforced pulse electrodeposition Ni-W coating was deposited on steel. • Nanoindentation showed the increased mechanical properties on addition of SiC. • Grain refinement and increased internal strain was observed in Ni-W-SiC coating. • Dislocation density increased on reinforcement of SiC in Ni-W coating. • Increased dislocation density triggered grain boundary misorientation and twinning.

36 MATERIALS SCIENCE↗

Microstructural characterization of SiO2/Ni nanocomposites electrodeposited from a sulphate bath modified by PEI

Highlights: • SiO{sub 2}/Ni + PEI nanocomposites are deposited from the sulphate bath containing PEI. • PEI allows incorporation of higher SiO{sub 2} vol% in SiO{sub 2}/Ni + PEI nanocomposites. • PEI in the form of a thin layer surrounds spherical Ni nanograins and SiO{sub 2} clusters. • PEI action ensures high hardness, tribological properties and corrosion resistance. - Abstract: SiO{sub 2}/Ni nanocomposite coatings containing well-dispersed SiO{sub 2} nanoparticles were electrodeposited from a sulphate bath with and without the addition of polyethylenimine (PEI) as a cationic surfactant. The surface morphology and microstructure in the cross-sections of the deposited nanocomposites were examined by scanning electron microscopy. More detailed microstructure characterization was performed using transmission, scanning-transmission and high resolution transmission electron microscopy. It was determined that the addition of 0.05 g/L and 0.1 g/L of PEI allows the incorporation of SiO{sub 2} nanoparticles in the nickel matrix to be increased in comparison with the nanocomposite deposited without a surfactant. Based on high spatial resolution microanalysis, performed using high count rate energy dispersive spectroscopy of characteristic X-rays in the scanning-transmission mode, the distribution of SiO{sub 2} nanoparticles in the nanocomposite was visualized on elemental maps. Image analysis of the electron microscopy images enabled the mean equivalent circle diameters of grains in the nickel matrix to be determined, together with the volume fraction of SiO{sub 2} nanoparticles in the nanocomposites. The volume fraction of SiO{sub 2} clusters in the SiO{sub 2}/Ni + PEI nanocomposites with the addition of 0.05 g/L and 0.1 g/L of PEI is equal to 18.4% and 13.3%, respectively. Furthermore, the PEI addition allows the nickel grain size in the matrix to be reduced. The combination of different imaging techniques confirmed that PEI is not only present as a surfactant in the electrolytic bath, but also incorporates into the microstructure of the nanocomposite. Nanocomposites electrodeposited in the presence of 0.05 g/L of PEI exhibit higher hardness, good tribological properties and improved corrosion resistance. Although increasing the PEI concentration in the bath up to 0.1 g/L strongly promotes grain size reduction and increase of the SiO{sub 2} volume fraction, it also causes an increase in the PEI fraction embedded in the microstructure, which results in deterioration of the properties of the SiO{sub 2}/Ni + PEI nanocomposites.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

The influence of Mo addition on the microstructure and its thermal stability for electrodeposited Ni films

Highlights: • The effect of Mo and saccharin additions on the stability of Ni layers was studied. • Both Mo and saccharin increased the defect density and reduced the grain size. • The higher Mo content resulted in a much better thermal stability. • At the same time, saccharin addition yielded a reduced stability of nanostructures. • The electrodeposited film had a better stability than the SPD-processed counterpart. - Abstract: An investigation was conducted to study the effect of molybdenum (Mo) alloying on the grain size and lattice defect structure in nanocrystalline nickel (Ni) films processed by electrodeposition. Moreover, the influence of saccharin addition to the electrolyte bath on the microstructure of Ni-Mo layers with low and high Mo contents was studied. It was found that the higher Mo content resulted in a larger dislocation density and twin fault probability as well as a smaller grain size. The addition of saccharin to the bath resulted in a further increase in the density of both dislocations and twin faults. It was also revealed that Mo alloying improved the thermal stability of the nanostructure in Ni films while saccharin addition yielded a reduction of stability. The reasons for these opposite behaviors were discussed in detail. In addition, the defect structure and its stability in Ni-Mo layers were compared with that for fine-grained bulk samples with the same composition but processed by severe plastic deformation.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Preparation and characterization of Cu-Ga-Se thin films synthesized by electrodeposition: Effect of complexing agent and supporting electrolyte

CuGaSe2 (CGS) is a semiconductor that has potential use as a photo electrode for solar water splitting. Its wide band gap and high absorption coefficient make it an ideal candidate for the top absorber in tandem structures. CGS can be synthesized by several techniques, being electrodeposition the most advantageous from a technical standpoint. Many reports show that electrodeposition of these films for producing the desired precursor atomic composition can be aided by using a complexing agent. However, the use of supporting electrolyte and the type of the electrolyte to improve the atomic composition in the films has never been reported. Using cyclic voltammetry, with complexing agents and deposition potentials between -0.5 and -0.9 V vs. Ag/AgCl reference electrode atomic ratios close to the ideal values ([Cu]/[Ga] = 1 and [Se]/[Cu + Ga] = 1), based on atomic composition and morphology analysis are reported in this work. From the X-ray diffraction (XRD), the as-deposited films exhibit poor crystallinity; however, the XRD patterns evidence the formation CuGaSe2 after annealing of the samples.

14 SOLAR ENERGY↗

Electrodeposited porous metal oxide films with interconnected nanoparticles applied as anode of lithium ion battery

Highlights: • Highly porous NiO film is prepared by a co-electrodeposition method. • Porous NiO film is composed of interconnected nanoparticles. • Porous structure is favorable for fast ion/electron transfer. • Porous NiO film shows good lithium ion storage properties. - Abstract: Controllable synthesis of porous metal oxide films is highly desirable for high-performance electrochemical devices. In this work, a highly porous NiO film composed of interconnected nanoparticles is prepared by a simple co-electrodeposition method. The nanoparticles in the NiO film have a size ranging from 30 to 100 nm and construct large-quantity pores of 20–120 nm. As an anode material for lithium ion batteries, the highly porous NiO film electrode delivers a high discharge capacity of 700 mA h g{sup −1} at 0.2 C, as well as good high-rate performance. After 100 cycles at 0.2 C, a specific capacitance of 517 mA h g{sup −1} is attained. The good electrochemical performance is attributed to the interconnected porous structure, which facilitates the diffusion of ion and electron, and provides large reaction surface area leading to improved performance.

36 MATERIALS SCIENCE↗

Effects of annealing temperature on the physicochemical, optical and photoelectrochemical properties of nanostructured hematite thin films prepared via electrodeposition method

Highlights: • Nanostructured hematite thin films were synthesized via electrodeposition method. • Effects of annealing on size, grain boundary and PEC properties were examined. • Photocurrents generation was enhanced when the thin films were annealed at 600 °C. • The highest photocurrent density of 1.6 mA/cm{sup 2} at 0.6 V vs Ag/AgCl was achieved. - Abstract: Hematite (α-Fe{sub 2}O{sub 3}) is a promising photoanode material for hydrogen production from photoelectrochemical (PEC) water splitting due to its wide abundance, narrow band-gap energy, efficient light absorption and high chemical stability under aqueous environment. The key challenge to the wider utilisation of nanostructured hematite-based photoanode in PEC water splitting, however, is limited by its low photo-assisted water oxidation caused by large overpotential in the nominal range of 0.5–0.6 V. The main aim of this study was to enhance the performance of hematite for photo-assisted water oxidation by optimising the annealing temperature used during the synthesis of nanostructured hematite thin films on fluorine-doped tin oxide (FTO)-based photoanodes prepared via the cathodic electrodeposition method. The resultant nanostructured hematite thin films were characterised using field emission-scanning electron microscopy (FE-SEM) coupled with energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), UV-visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) for their elemental composition, average nanocrystallites size and morphology; phase and crystallinity; UV-absorptivity and band gap energy; and the functional groups, respectively. Results showed that the nanostructured hematite thin films possess good ordered nanocrystallites array and high crystallinity after annealing treatment at 400–600 °C. FE-SEM images illustrated an increase in the average hematite nanocrystallites size from 65 nm to 95 nm when the annealing temperature was varied from 400 °C to 600 °C. As the crystallites size increases, the grain boundaries reduce and this suppresses the recombination rate of electron–hole pairs on the nanostructured hematite thin films. As a result, the measured photocurrent densities of nanostructured hematite thin films also increased. The highest measured photocurrent density of 1.6 mA/cm{sup 2} at 0.6 V vs Ag/AgCl in 1 M NaOH electrolyte was achieved for the nanostructured hematite thin film annealed at 600 °C. This study had confirmed that strong interdependencies exist between the average hematite nanocrystallites size and grain boundaries with annealing temperature on the eventual PEC water splitting performance of nanostructured hematite thin films. The annealed hematite thin films at a higher temperature will enhance the nanocrystals growth and thus, suppressing the electron–hole pairs recombination rate, lowering the grain boundary resistance and enabling higher photocurrent flow at the molecular level. As a result, the photocurrent density and thus, the overall PEC water splitting performance of the nanostructured hematite thin films are significantly enhanced.

36 MATERIALS SCIENCE↗

Pulsed laser irradiation-assisted electrodeposition of germanium in ionic liquid: From amorphous film to polycrystalline branched structures

Highlights: • Ge branched structures was prepared by electrodeposition in ([EMIm]Tf2N) ionic liquid with laser irradiation. • The crystallinity of Ge with laser irradiation is obviously improved compared to the Ge film without laser irradiation. • By controlling the deposition time, the nanostructures with different morphology and size are obtained. - Abstract: The effect of a pulsed laser on the electrodeposition of germanium on indium tin oxide glass in the ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([EMIm]Tf{sub 2}N) was investigated. Cyclic voltammetric analysis of GeCl{sub 4} in [EMIm]Tf{sub 2}N showed that laser irradiation produced a positive shift of the reduction potential and an increase in the reduction current. Laser irradiation influenced the morphology and crystallinity of the Ge deposits. A deposition time of 1200 s gave rise to amorphous Ge deposits when laser irradiation was not applied, whereas laser irradiation led to a polycrystalline branched structure. The length and width of the branched structures were about 9.58 and 2.18 μm, respectively, and the average grain size of the sample was ∼76 nm. The morphology and size of the Ge deposits could be controlled by adjusting the deposition time under laser irradiation. The mechanism of growth of the Ge deposits under laser irradiation was discussed in detail.

36 MATERIALS SCIENCE↗

Selective determination of grain size in the electrodeposition of nanocrystalline nickel foils

There are many synthesis methods through phase space to produce nanostructures in metals. Condensation methods with rapid solidification are extensively explored from the gas or liquid phase. In particular, electrodeposition using pulsed currents favors continuous nucleation in the processing of structures to produce free-standing sheets as well as protective coatings for surfaces. An analysis approach used to develop the method for refining the structure and surface finish for nanocrystalline gold-copper alloy coatings relates the energy in each deposition pulse to the constituent grain size that forms during growth. Application is now pursued to evaluate a select determination of the grain size for nanocrystalline nickel foils synthesized by pulsed electrodeposition. The mechanical behaviors of hardness and rate-sensitivity of strength are assessed as function of grain size.

36 MATERIALS SCIENCE↗

Electrodeposition of actinide compounds from an aqueous ammonium acetate matrix. Experimental development and optimization

Electrodeposition is a technique that is routinely employed in nuclear research for the preparation of thin solid films of actinide materials which can be used in accelerator beam bombardments, irradiation studies, or as radioactive sources. The present study investigates the deposition of both lanthanides and actinides from an aqueous ammonium acetate electrolyte matrix. Electrodepositions were performed primarily on stainless steel disks; with yield analysis evaluated using -spectroscopy. Experimental parameters were studied and modified in order to optimize the uniformity and adherence of the deposition while maximizing the yield. The initial development utilized samarium as the plating material, with and without a radioactive tracer. As a result, surface characterization studies were performed by scanning electron microscopy, electron microprobe analysis, radiographic imaging, and x-ray diffraction.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Effects of annealing on fission fragment release from electrodeposited Cf-252 thin-films

In this work, samarium thin-films doped with a 252 Cf radiotracer were used to study the effects of annealing on the release of fission fragments from electrodeposited films. An ammonium acetate molecular plating technique was utilized to perform the depositions. The fission fragment yields were measured using a unique technique involving the exposure of aluminum foils to the deposited material for a fixed time followed by gamma-ray spectroscopy to determine the rate at which the fission fragments implanted into the foils. Annealing of the electrodeposited films was found to have no effect on the release of fission fragments.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS

This paper presents an evaluation of an alternate method for preparing environmental samples for 129 I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Furthermore, precipitated silver iodide samples are usually mixed with niobium or silver powder prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.

129I↗