Pulse Electrodeposition Technique Research Articles

Pulsed Electro Decoration of Carbon Nanotubes with FexZn1−xS

Pulsed Electro Decoration of Carbon Nanotubes with FexZn1−xS

Constructing 3D sandwich-like structured Ti foam/TiO2−x/SnO2-Sb composite electrodes for the degradation of PPCPs

The fabrication of Sb-doped SnO2 electrode with high catalytic activity and excellent durability for decomposition PPCPs (Pharmaceuticals and personal care products, PPCPs) is challenging. Herein, a Ti3+/Ovs-related TiO2−x is prepared by short-time annealing at low temperature in mixed gas with Zr as a cocatalyst. DFT calculations indicate that the introduction of Ti3+/Ovs defects could promote the formation of more ·OH. Then, the nanoflower rod-like SnO2-Sb catalytic layer supported on dual-defects TiO2−x is successfully synthesized by one-step pulse electrodeposition (PLED) combined with hydrothermal methods (H). This newly pulse electrodeposition technique solves the short lifetime problem of SnO2-Sb nanoflower electrodes current hydrothermal-based methods. 1O2 and ·OH are found to be the primary reactive oxygen species (ROSs) by radical quenching tests and electron paramagnetic resonance analysis. The optimized Ti foam/TiO2−x /SnO2-Sb electrode could degrade over 96.3 % of 20 mg L−1 amoxicillin (AMX) within 30 min, corresponding kinetic constant 0.10228 min−1. This will provide inspiration for the construction of defect engineering and new insights for the development of low-cost and high electrooxidation activity Sb-doped SnO2 electrode.

Synthesis and characterization of open cell Ni-Cr foam developed using Pulse electro deposition technique for filtration applications

Nickel–Chromium (Ni-Cr) foam is a highly versatile material, combining excellent high-temperature and corrosion resistance with lightweight and energy absorption properties, making it a popular choice for a wide range of applications. This study explores the development of Ni-Cr foam using Pulse electrodeposition techniques, specifically ultrasonic-assisted pulse electroplating of nickel (UAPEPN) and ultrasonic-assisted pulse electroplating of chromium (UAPEPCr). The study evaluates the surface morphology, coating thickness and minimum mass gain of Ni-Cr foam after each process. A dedicated test rig was designed to measure the pressure drop across the foam, revealing a pressure drop of 0.29 bar at an input pressure of 70 PSI and a flow rate of 17.53 LPM of oil. The porosity percentage and permeability of the foam were evaluated at each developmental stage, with values noted as 91% and 1.0032 × 10−8 m2, respectively, after the UAPEPCr stage. Uniaxial tensile and compression tests were conducted to measure the foam’s maximum strength and energy absorption per unit volume, yielding valuable insights into the material’s performance characteristics.

Nanoscale hydroxyapatite/chitosan polymer coatings: Synthesis and characterization

AbstractThe present work involves the coating synthesis of nano‐hydroxyapatite/chitosan (nHA/CS) on a Mg‐2 wt% Zn scaffold with the pulse electrodeposition (PED) technique. In practice, to render coatings more corrosion‐resistant and biocompatibility in simulated body fluids, the impact of PED factors, such as mean current density (j), a duty cycle, and coating duration (t), was investigated. Further, Fourier transform infrared spectroscopy, scanning electron microscope, x‐ray diffraction, energy‐dispersion spectrometer, and water contact angle (WCA) were studied to characterize coatings. The corrosion resistance of coatings was investigated by impedance evaluations and potentiodynamic polarization. The results obtained from analyses revealed that the optimum conditions for synthesizing the nHA/CS coating were achieved when applying j = 20 mA/cm2, a duty cycle = 0.4, and a duration of 60 minutes. The coatings' microstructure and Ca/P ratio were influenced by PED factors, which included nano spherical‐shaped and 1.65. Furthermore, the corrosion rate was decreased from 19.603 to 1.492 mm yr−1 after being modified by optimum coating. Moreover, the high hydrophilic properties are assigned to this coating with a WCA of 29.9 compared to other coatings and the Mg scaffold. The biological properties of the optimum coating were assessed through in‐vitro experiments involving MG63 cells, which included the evaluations of cell adhesion and cytotoxicity. The results obtained from the corrosion and in‐vitro experiments indicate that the nanocomposite coating, upon optimization, holds potential as a scaffold for bone tissue engineering.Highlights Using Mg‐2 wt% Zn scaffold as a substrate for nanocomposite coatings. Pulse electrodeposition method for the synthesis of nano‐hydroxyapatite/chitosan (nHA/CS) coatings. Pulse electrodeposition (PED) method to modify morphology, corrosion resistance, and biocompatibility. Optimum PED parameters: j = 20 mA/cm2, duty cycle = 0.4, and t = 60 min.

A Novel Ni-doped ZnMn2O4/Mn2O3 nanocomposite synthesized by pulsed potential as superior zinc ion battery cathode material

The research and development of suitable cathode materials for Zn2+ storage is crucial to meet the large-scale energy storage application of zinc-ion batteries (ZIBs). However, manganese-based oxide cathodes, the most-studied category of cathode materials, suffer from capacity decline and weak electrical conductivity. Herein, Ni-doped ZnMn2O4/Mn2O3 nanocomposite has been synthesized using pulsed potential electrodeposition technique and then applied as cathode material for ZIBs. The Ni2+ doping effectively boosts the electrical conductivity and electrochemical performance of electrodes. Furthermore, simultaneous production of ZnMn2O4 /Mn2O3 nanocomposite as a two-phase compound and incorporation of Ni2+ in crystal structure leads to an improvement in reversibility and cyclability of Ni-doped ZnMn2O4/Mn2O3 nanocomposite. Moreover, the Ni-doped ZnMn2O4/Mn2O3 nanocomposite presents a specific capacity of 235.10 mAh g−1 (0.2 A g−1), higher than Undoped nanocomposite (215 mAh g−1). Besides, the Ni-doped ZnMn2O4/Mn2O3 nanocomposite shows superior electrochemical performance, with a reversible capacity of 114.67 mAh g−1 and capacity retention of 91.32%, obtained after 3000 cycles at 2 A g−1, while the Undoped -ZnMn2O4/Mn2O3 nanocomposite possesses the capacity of 61.85 mAh g−1 with 64.54% capacity retention at the same condition. The obtained results suggest that the synergistic effect of doping and two-phase compound synthesis provide new features for the practical application of ZIBs.

The semiconductor properties and tin segregation mechanism in the passive film formed on the electrodeposited Ni-Sn coatings

The nanocrystalline Ni-Sn coatings (average grain size 15.78 nm) formed of relatively ordered circular particles covering the entire surface characterized with nodule-like endings were successfully electrodeposited using pulse electrodeposition technique. Scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) and X-ray diffraction (XRD) were used to analyse the film microstructure. The corrosion resistance and semiconducting properties of Ni-Sn coatings were investigated in borate buffer solution. The EIS measurements showed that Ni-Sn alloys developed, in the passive zone, a good corrosion resistance as demonstrated by a thin film thickness, the low capacitance value, high polarization resistance, and the high value of electric field strength. Mott-Schottky analysis showed that the passive film formed on Ni-Sn coatings presents an p-n heterojunction characteristic indicating that the charge carrier densities are composed of cation (NA) and anion (ND) vacancies. The high density of point defects (NA + ND ∼ 1021cm−3) induces a high electronic conductivity in the Ni-Sn coatings passive film. The XPS analysis showed that the passive film formed on Ni-Sn alloys is composed of NiO, Ni(OH)2, NiOOH, SnO, and SnO2 species and an enrichment of Sn in the passive film. The mechanisms of passive film growth and Sn segregation in the Ni-Sn passive film are suggested in conjunction with the Point Defect Model (PDM). The good corrosion resistance and high electronic conductivity achieved in this work suggest that Ni-Sn Coating is a good candidate for water electrolysis applications.

Lattice-controllable in-situ synthesis of Co-Ni-mixed sulfide/polypyrrole nanostructures on carbon paper for hydrogen evolution reaction in alkaline media

Developing high-performance and low-cost electrocatalysts for the hydrogen evolution reaction (HER) favorably promotes large-scale hydrogen production from water. Here, we design a nanocomposite of Co9S8-Ni9S8 nanodiscs (CNS) in-situ grown from polypyrrole hollow nanospheres (PHS) on carbon paper (CP) via unipolar pulse electrodeposition (UPED) technique as HER catalyst in alkaline media. The lattice structure along with the interlacing nanodiscs-like morphology of the Co9S8-Ni9S8 mischcrystal is controllable by UPED method. The optimal CNS/PHS/CP electrode obtained with pulse potential of − 0.80 V exhibits favorable catalytic activity with low overpotential (186 mV at 10 mA cm−2), superior stability performance (for 100 h with no current density decay), and high electrochemically active surface area up to 1925 cm2, which should be attributed to the interlacing Co9S8-Ni9S8 mischcrystal with rich active sites, the ingenious combination with conductive polymer, and the integrated electron-proton conductive network. This work will provide a new sight to design low-cost bimetallic sulfide-based electrocatalysts for high-performance HER in water splitting.

Fabrication of corrosion-resistant conversion coating based on ZIF-8 on electro-galvanized steel utilizing pulse electrodeposition technique

In this work, through a novel method of synthesizing zeolitic imidazolate framework-8 (ZIF-8), a conversion coating (CC) was applied to a galvanized surface. A reverse pulse electrodeposition (PED) method was employed to apply ZIF-8 conversion coating in a 2-methylimidazole bath during 2, 4, and 6 h. Characterization techniques demonstrated that the ZIF-8 conversion coating (ZIF-8CC) was successfully synthesized after 6 h. The increase in hydrophilicity of the synthesized conversion coating was demonstrated by the contact angle test. The best performance of the single-layer conversion coating against corrosion was obtained in the case of ZIF-8CC@6 h. Then, an epoxy coating was applied to the samples with and without conversion coatings. The effect of the ZIF-8 conversion coating on the adhesion strength and the corrosion behavior of the epoxy coating was investigated. The results revealed the superior functioning of ZIF-8CC@6 h compared to the rest of the samples in terms of adhesion and protective performance of the epoxy coating.

Comparison of Physical/Chemical Properties of Prussian Blue Thin Films Prepared by Different Pulse and DC Electrodeposition Methods.

Prussian Blue (PB) thin films were prepared by DC chronoamperometry (CHA), symmetric pulse, and non-symmetric pulse electrodeposition techniques. The formation of PB was confirmed by infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX) and UV-Vis transmission measurements. X-ray diffraction (XRD) shows the stabilization of the insoluble form of PB. From scanning electron microscopy (SEM) studies, an increase in porosity is obtained for the shorter pulse widths, which tends to improve the total charge exchange and electrochemical stability of the films. While the film prepared by CHA suffered a degradation of 82% after 260 cycles, the degradation reduced to 24% and 34% for the samples prepared by the symmetric and non-symmetric pulse methods, respectively. Additionally, in the non-symmetric pulse film, the improvement in the charge exchange reached ~522% after 260 cycles. According to this study, the deposition time distribution affects the physical/chemical properties of PB films. These results then render pulse electrodeposition methods especially suitable to produce high-quality thin films for electrochemical devices, based on PB.

Experimental studies on wear and corrosion resistance of pulse electrodeposited Ni-TiO2 nanocomposite coatings on AISI 304 stainless steel

Nickel-nano titanium oxide (Ni-TiO2) composite coatings were developed on stainless steel 304 substrate using pulsed electro-deposition technique. Experiments were carried out employing orthogonal array, taking current density, frequency, and duty cycle as prime parameters. Coating characterization was done using FESEM with EDAX and XRD. Applying the Response Surface Methodology optimization method, the optimized values of the parameters were identified as duty cycle, frequency and current density with values of 24%, 10 Hz and 0.6 A cm−2 respectively. Vickers micro-hardness, surface roughness, wear resistance and corrosion resistance were measured initially for the as-coated sample. The sample that yielded the optimum parameters was then heat treated for an hour at 400 °C in a closed furnace and quenched in SAE 40 grade oil. Test results of post heat-treated sample produced maximum micro-hardness of 446.45Hv, reduced surface roughness of 0.292 μm, superior wear rate of 3.20E−07 mm3 N−1-m−1 and corrosion protection efficiency of 94.52% of Ni-TiO2 coating at low frequency, along with enhanced wear and corrosion resistance as compared with the as-coated sample.

Flexible Graphene-Copper Nanocomposite for Potential Wearable Electronics Applications

The demand for flexible and wearable electrochemical sensors has surged due to their low cost and portability. This study produces and characterizes low-cost and environmentally friendly flexible laser engraved graphene/Cu nanoparticles composite materials as a potential electrode for electronic applications. The electrode is fabricated by directly engraving Polyimide substrate using a CO2 laser machine to produce Laser Engraved Graphene (LEG). The electrode is then modified with copper nanoparticles via a one-step pulse electrodeposition technique to be characterized structurally, mechanically, and electrochemically using SEM, XRD, bending test, electrochemical impedance spectroscopy, and cyclic voltammetry to assess their stability and electrocatalytic activity. The laser irradiation of PI results in 3D porous graphene structure formation that increases electron transfer rate and the electrochemically active surface area. Copper deposition improves the sensitivity of LEG by its high conductivity.

Effect of duty cycle variation on Nickel electrodeposits at 10 Hz frequency

In this paper, nano nickel coating was made by pulsed electrodeposition technique to improve the surface properties of base metal. The developed nickel coating was characterized using SEM, Xrd, Vickers microhardness, Potentiodynamic polarization and ball on plate wear testing. X-ray diffraction studies shown that predominant (111) crystalline plane and finer grain size were obtained with lower duty cycle at 10 Hz frequency of pulse current. Pitting corrosion resistance of coated samples was evaluated at 3.5 wt. % of sodium chloride solution. An improvement of corrosion protection efficiency and good mechanical properties were achieved at lower duty cycle. As the duty cycle decreases, the corrosion current and wear rate decrease, and the micro hardness value increases. The average grin size was observed to be 75 nm and the newly developed nickel coated surface shown strong metallurgical bonding with the low carbon steel substrate material.

Pulse-electrodeposition of PtNi nanoparticles on a novel substrate of multi-walled carbon nanotubes/poly(eriochrome blue-black B) as an active and durable catalyst for the electrocatalytic oxidation of methanol

• A facile producer is developed for deposition of Pt-Ni nanoparticles by improving the size, dispersion, and promoting the catalyst utilization on a polymeric substrate. • Electropolymerization of eriochrome blue-black B is reported for the first time. • The pulsed electrodeposition of the metal ions has more catalytic properties with higher current density and lower onset potential than chronoamprometric method. • PtNi@p-EBB is an effective electrocatalyst with long-time stability for methanol oxidation in alkaline media. Herein, a simple and novel methodology for fabricating a high-methanol-tolerant electrocatalyst based on poly(eriochrome blue-black B)/multi-walled carbon nanotubes, coated with nickel and platinum nanoparticles is described. The polymer thin film was prepared using cyclic voltammetry and pulsed electrodeposition technique was used to decorate the polymer layer with nickel and platinum nanoparticles. The energy dispersive X-ray analysis (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), and inductively coupled plasma analyses were performed to characterize the prepared catalyst. The morphological studies reveal that the PtNi-nanoparticles were distributed without accumulation throughout the polymer layer. The development of pulse electrodeposition technique for immobilization of PtNi-nanoparticles on the polymeric substrate significantly improves the size, dispersion, and promotes the catalyst utilization. The PtNi@p-EBB/MWNT catalyst show high stability and high current density (1550 mA.mg -1 Pt).

Magnetic properties and Curie temperature tuning in copper-Permalloy alloys obtained by electrodeposition

Permalloy copper (CuPy) structures, produced by low cost vacuum free pulsed electrodeposition technique, present relevant results as magnetic material properties hardening and Curie temperature decay in function of Cu concentration. Such properties modification are here related to the slight crystalline phase shift of face cubic centered (FCC) structure to lower angles, evidenced by X-ray measurements, with lattice parameter increase and successively magnetization weakening by Ni atoms substitution by Cu. The fine tuning of Curie temperature decrease reported here, Tc≈800K from pure Permalloy to Tc≈380K for alloy with 67% of Cu, could allow utilization of such technique to develop magnetic sensors and memories with thermal activation achieved near room temperature.

Pulse Electrodeposition of Cu on Porous Ag Framework for Electrochemical CO2 Conversion to Ethanol

Electrochemical conversion of carbon dioxide (CO2) gas is a simple and cost-benefit method to produce economically valuable materials such as carbon monoxide (CO), multi-carbon (C2+) oxygenate, and hydrocarbons. In particular, ethanol (EtOH) production is attractive to be applied for conventional transport fuels. However, there has been a lack of techniques to yield predominant EtOH from CO2. Copper (Cu), as the well-known and exclusive C2+ catalyst, thermodynamically prefers the production of (C2H4) compared to EtOH. Previous studies suggested that increased concentration of carbon monoxide (CO) as the intermediate of CO2 ameliorated the EtOH selectivity.1,2 Because the solubility of CO is very little in an aqueous electrolyte solution, surface diffusion of CO has been considered to enhance the local CO concentration. It suggests that catalyst interface is crucial to increasing EtOH yield, while little knowledge was developed.We prepared porous Ag inverse opal (AgIO) frameworks with a uniform pore size of ~ 600 nm. The CO2 gas was electrochemically reduced to CO with > 90% selectivity at -1.05 V vs. RHE. In addition, the CO settled in the pore, providing an opportunity for sequential electrochemical/chemical reactions. We deposited the ultra-thin Cu layer (2~10 nm) upon the Ag surface through the pulse electrodeposition technique (PED). This catalyst, indicated as PEDCu/AgIOs, performed ~33 % Faradaic efficiency (FE) of EtOH at -1.05 V vs. RHE. Moreover, PEDCu/AgIOs showed a high oxygenates ratio relative to hydrocarbons (FEoxygenate/FEC2H4) of 2.28, while H2 evolution was significantly suppressed. These results suggested that as-prepared thin Cu film was partially segregated, and the Ag surface was exposed, forming the mixed Ag and Cu interfaces in the given electrochemical condition. This hypothesis was confirmed by negligible EtOH from the Ag-free CuIOs structure. More importantly, the resulting EtOH selectivity outperformed Cu nanoparticles (~7 nm diameter) dispersed on AgIOs (7.45 % FE) and aggregated Cu nanostructures on AgIOs (17.65 % FE) prepared by the constant current mode of electrodeposition. We, therefore, anticipated that CO spillover was promoted by the remaining and ultra-thin Cu layer. Further experiments were conducted by controlling of the thickness, pore size, and interpore size of AgIO frameworks to understand their roles. PEDCu/AgIOs with larger AgIOs thickness and smaller pore size showed higher EtOH selectivity, while the interpore size did not significantly affect the product selectivity. In the presentation, I will discuss key parameters to determine EtOH selectivity and the presumable pathway of EtOH production in details. References Ting, L. R. L.; Piqué, O.; Lim, S. Y.; Tanhaei, M.; Calle-Vallejo, F.; Yeo, B. S., Enhancing CO2 Electroreduction to Ethanol on Copper–Silver Composites by Opening an Alternative Catalytic Pathway. ACS Catal. 2020, 10 (7), 4059-4069.Gurudayal; Perone, D.; Malani, S.; Lum, Y.; Haussener, S.; Ager, J. W., Sequential Cascade Electrocatalytic Conversion of Carbon Dioxide to C-C Coupled Products. ACS Appl. Energy Mater. 2019, 2 (6), 4551-4559.

Preparation of superhard nanometer material cBN reinforced Ni-W-P nanocomposite coating and investigation of its mechanical and anti-corrosion properties

In this work, superhard nanoparticle cubic boron nitride (cBN) was introduced into Ni-W-P bath, and Ni-W-P/cBN composite coatings with different cBN concentrations were successfully prepared by pulse electrodeposition technique. In addition, the effects of different cBN dosages on the wear resistance and corrosion resistance of Ni-W-P/cBN composite coatings were also studied. Vickers microhardness tester and multifunctional material surface testing machine was used to evaluate the hardness and wear resistance of composite coatings. The corrosion resistance properties of the coatings were analyzed and characterized by EIS and potentiodynamic polarization. The results show that when the cBN content in the bath is 2 g/L, the comprehensive properties of the Ni-W-P/cBN composite coating are improved most significantly. Benefiting from the mechanical enhancement effect of cBN, the microhardness of the Ni-W-P/cBN (2 g/L) composite coating is increased to 543.0 HV, and the friction coefficient is reduced to 0.39 (the original Ni-W-P coating has a lower Microhardness 343.4 HV and higher friction coefficient 0.68). Furthermore, it is found that the corrosion resistance of the composite coating is greatly improved by electrochemical technology. The corrosion potential of Ni-W-P/cBN (2 g/L) composite coating is − 0.46 V, corrosion current is 9.3 μA/cm2 and corrosion rate is 0.11 mm/ year. (The corrosion potential of Ni-W-P coating is −0.53 V, corrosion current is 30.4 μA/cm2 and corrosion rate is 0.36 mm/ year).

Characterisation, hardness and corrosion behaviour of electrodeposited ZnFe and ZnFe/BN composite coatings

ABSTRACT ZnFe and ZnFe/BN composite coatings were successfully electrodeposited on 304 stainless steel substrates by pulse electrodeposition technique. The effect of various concentrations of BN particles in the plating solution on the structural, hardness and corrosion properties of electrodeposited ZnFe alloy and ZnFe/BN composites were investigated. The deposition process and electrochemical behaviour of alloy and composite coatings were analysed by the Cyclic Voltammetry (CV) method. X-ray diffraction (XRD), and scanning electron microscopy (SEM) were used for the structural, and morphological characterisation of the coatings. Vickers micro hardness indentation was used to determine the hardness of the deposits. The corrosion behaviour of ZnFe alloy and ZnFe/BN composites was investigated by open circuit potential (OCP), Tafel plots, and electrochemical impedance spectroscopy (EIS) methods. As the BN particle content in ZnFe/BN composite coatings rose, the microhardness, and corrosion resistance of coatings increased, which was due to the function of grain refinement and changing dispersion strengthening. Meanwhile, grain sizes were strongly affected from the presence of BN particles and their content. The ZnFe/BN composite coatings with the BN particle concentration of 20 g L−1 had the highest corrosion resistance, and microhardness.

The microstructural features and corrosion behavior of Hydroxyapatite/ZnO nanocomposite electrodeposit on NiTi alloy: Effect of current density

In the present study, hydroxyapatite/ZnO nanocomposite coatings were developed on NiTi superelastic alloy via pulse electrodeposition technique under three different current densities. The morphological observations (FESEM) indicated that under 6 mA/cm2, a compact, uniform composite layer could form, whereas lower or higher current densities resulted in non-uniform, porous coatings with uneven distribution of nanoparticles. XRD and FTIR studies revealed that pure hydroxyapatite was not achieved below 6 mA/cm2. Topographic features (AFM) were assessed and demonstrated a continuous rise in roughness parameters as current density increased. The corrosion behavior was investigated through potentiodynamic polarization as well as impedance spectroscopy techniques. According to the extracted data, the porosity and non-uniformity of coatings formed under 3 and 9 mA/cm2 caused a detrimental effect on the corrosion resistance of surfaces. The layer obtained under 6 mA/cm2 showed resistance (Rc) which was almost two times greater than those deposited under 3 and 9 mA/cm2 current densities. Last but not least, the bioactivity of coatings was evaluated in simulated body fluid. It was observed that more compact deposits offered more active sites for apatite nucleation, resulting in refined cauliflower-like grains. Accordingly, it can be asserted that the best composite coating was achieved under 6 mA/cm2 current density.

Investigation on Corrosion Behavior of Reduced Graphene Oxide/Zirconia Nanocomposite Coated by Pulse Electrodeposition Technique on Api-X65 Steel

Investigation on Corrosion Behavior of Reduced Graphene Oxide/Zirconia Nanocomposite Coated by Pulse Electrodeposition Technique on Api-X65 Steel

Investigation on Corrosion Behavior of Reduced Graphene Oxide/Zirconia Nanocomposite Coated by Pulse Electrodeposition Technique on API-X65 Steel

Investigation on Corrosion Behavior of Reduced Graphene Oxide/Zirconia Nanocomposite Coated by Pulse Electrodeposition Technique on API-X65 Steel