Electrochemical impedance characterization of FeSn2 electrodes for Li-ion batteries

This work reports the electrochemical characterization of a micro-scale FeSn₂ electrode in a lithium battery. The electrode is proposed as anode material for advanced lithium ion batteries due to its characteristics of high capacity (500 mAh g⁻¹) and low working voltage (0.6 V vs. Li). The electrochemical alloying process is studied by cyclic voltammetry and galvanostatic cycling while the interfacial properties are investigated by electrochemical impedance spectroscopy. The impedance measurements in combination with the galvanostatic cycling tests reveal relatively low overall impedance values and good electrochemical performance for the electrode, both in terms of delivered capacity and cycling stability, even at the higher C-rate regimes.     

Synthesis of ordered nanoporous carbon and its application in Li-ion battery

Ordered nanoporous carbon (ONC) was comprehensively tested for the first time as electrode material in lithium-ion battery. Structure characterization shows the order nanoporous structure and tiny crystallite structure of as-synthesized ONC. The electrochemical properties of this carbon were studied by galvanostatic cycling and cyclic voltammetry. Of special interest is that ONC gave no peak on its positive sweep of the cyclic voltammetry, which was different from other known anode materials. Besides, X-ray photoelectron spectroscopy (XPS) and XRD were also used to investigate the electrochemical characteristics of ONC.     

Performance improvement of pasted nickel electrodes with multi-wall carbon nanotubes for rechargeable nickel batteries

Carbon nanotubes (CNTs) were employed as a functional additive to improve the electrochemical performance of pasted nickel-foam electrodes for rechargeable nickel-based batteries. The nickel electrodes were prepared with spherical β-Ni(OH)₂ powder as the active material and various amounts of CNTs as additives. Galvanostatic charge/discharge cycling tests showed that in comparison with the electrode without CNTs, the pasted nickel electrode with added CNTs exhibited better electrochemical properties in the chargeability, specific discharge capacity, active material utilization, discharge voltage, high-rate capability and cycling stability. Meanwhile, the CNT addition also lowered the packing density of Ni(OH)₂ particles in the three-dimensional porous nickel-foam substrate, which could lead to the decrease in the active material loading and discharge capacity of the electrode. Hence, the amount of CNTs added to Ni(OH)₂ should be optimized to obtain a high-performance nickel electrode, and an optimum amount of CNT addition was found to be 3 wt.%. The superior electrochemical performance of the nickel electrode with CNTs could be attributed to lower electrochemical impedance and less γ-NiOOH formed during charge/discharge cycling, as indicated by electrochemical impedance spectroscopy and X-ray diffraction analyses. Thus, it was an effective method to improve the electrochemical properties of pasted nickel electrodes by adding an appropriate amount of CNTs to spherical Ni(OH)₂ as the active material.     

Electrochemical characterisation of multilayer organic coatings

The protective properties of eight high performance commercial multilayer organic coatings for aeronautical use (based on polyurethane, epoxy and polyurethane-compatible epoxy resins) on anodised 2024-T3 Al alloy were evaluated in neutral aerated 3.5% NaCl aqueous solution using the electrochemical impedance spectroscopy (EIS) technique. The investigation was performed on specimens supplied and prepared from Alenia in accordance with their technical specifications. Results obtained in this paper show that all coating systems exhibit excellent protective properties even after prolonged immersion in the test solution (one year). Although the dielectric properties of all multilayer coatings are quite similar, EIS was proved to be able to discriminate among them, making possible a rank of these protective systems to prevent or to reduce corrosion. Capacitance measurements performed on the same coatings allow their behaviour to be forecasted.     

The combined role of inhibitive pigment and organo-modified silica particles on powder coatings: Mechanical and electrochemical investigation

The addition of organo-modified silica particles (OSP) to powder coating containing zinc molybdenum phosphate pigment (ZMP) has been investigated. The OSP were directly incorporated at different concentrations (1, 2.5, 3.5 and 4.5 wt%) in a polyester powder monolayer coating with 10 wt% ZMP. The adhesion and anticorrosion properties were evaluated by means of adhesion studies and different electrochemical techniques: electrochemical impedance spectroscopy (EIS) and an accelerated cyclic electrochemical technique (ACET). The optimum quantity of OSP that gave maximum anticorrosive performance of the coating system was determined (1.0%), however two opposite effects of addition on the coatings led to a reduction of anticorrosive properties for higher contents. Finally, the electrochemical behaviour of the optimized combined system was compared to the effects achieved when both additives were separately added to powder coatings by means of an additional electrochemical test.     

High performance water-based paints with non-toxic anticorrosive pigments

Legal restrictions have impelled the replacement of solvent-borne resins and of toxic chromates and lead-bearing pigments in the elaboration of paints. Water-based anticorrosive paints have come a long way to improve their efficiency but their behaviour is said to be poorer than that of solvent-based paints. Nevertheless, recent advances in water-borne technologies have now resulted in improved resin systems that may be employed to produce heavy-duty coatings.

The objective of this paper is to formulate high performance water-borne paints pigmented with non-toxic phosphate inhibitors. The anticorrosive properties of the paints were evaluated by accelerated tests (salt spray and humidity cabinets) and electrochemical tests (electrochemical impedance spectroscopy, EIS). The anticorrosive properties of the pigments were also evaluated by electrochemical tests.

It was found that it is possible to formulate high performance anticorrosive paints by selecting adequate water-borne resins and ecological pigments.     

A new high-performance cathode material for rechargeable lithium-ion batteries: Polypyrrole/vanadium oxide nanotubes

Polypyrrole/vanadium oxide nanotubes (PPy/VOx-NTs) as a new high-performance cathode material for rechargeable lithium-ion batteries are synthesized by a combination of hydrothermal treatment and cationic exchange technique. The morphologies and structures of the as-prepared samples are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, thermogravimetry and differential scanning calorimeter (TG-DSC) and X-ray powder diffraction (XRD). The results indicate that the organic templates are mainly substituted by the conducting polymer polypyrrole without destroying the previous nanotube structure. Their electrochemical properties are evaluated via galvanostatic charge/discharge cycling, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). It is found that PPy/VOx-NTs exhibit high discharge capacity and excellent cycling performance at different current densities compared to vanadium oxide nanotubes (VOx-NTs). After 20 cycles, the reversible capacity of PPy/VOx-NTs (159.5 mAh g⁻¹) at the current density of 80 mA g⁻¹ is about four times of magnitude higher than that of VOx-NTs (37.5 mAh g⁻¹). The improved electrochemical performance could be attributed to the enhanced electronic conductivity and the improved structural flexibility resulted from the incorporation of the conducting polymer polypyrrole.     

An electrochemical impedance spectroscopy and scanning electron microscopy study of the influence of positive plate compression on the electrochemical behaviour of lead-acid batteries

This study has developed an electrochemical impedance spectroscopy (EIS) method for the in situ investigation of the influence of positive plate compression on the electrochemical behaviour of lead-acid batteries during charge/discharge cycling. The EIS data for a fully charged and fully discharged battery are internally consistent with the expected kinetics of a battery in the opposite states of charge, and demonstrate that EIS measurements may be recorded with a high level of reproducibility. Furthermore, this study has necessitated the development of a special cell incorporating horizontally orientated battery plates that can be subjected to elevated pressure through the stacking of lead bricks on top of the cell, as well as a physically robust reference electrode system that can withstand the application of pressure. For this purpose, a platinum-wire pseudo-reference electrode has been developed, and has been shown to exhibit sufficient electrode stability over the period of an EIS recording, enabling the measurement of reproducible and meaningful EIS data. Additionally, the influence of positive plate compression on the behaviour of the lead-acid battery has been investigated by using scanning electron microscopy (SEM). Clearly, the experimental data show that plate compression enhances significantly the kinetics and concomitant performance of the lead-acid battery, and this is related to the enhanced reactivity of the active material, as rationalized by using the agglomeration-of-spheres (AOS) model.     

Electrochemical composite formation of thiophene and N-methylpyrrole polymers on carbon fiber microelectrodes: Morphology,characterization by surface spectroscopy,and electrochemical impedance spectroscopy

Electrochemical composite thin film formation (∼0.6–0.7 μm) of thiophene and N-methylpyrrole on carbon fiber microelectrodes (diameter ∼7 μm) was carried out by cyclic voltammetry in order to understand and improve the surface properties and capacitance behaviour of carbon fibers. Carbon fiber microelectrodes were coated with polythiophene and N-methylpyrrole was electrografted onto the thiophene electrode. The electrocoated carbon fiber surface mophology was characterized by scanning electron microscopy and atomic force microscopy and by FTIR-reflectance spectroscopy for their composition. The effect of monomer concentration and scan number on electropolymerization has also been investigated. The impedance behaviour of composite electrodes was characterized by electrochemical impedance spectroscopy. The composite of polythiophene and poly-N-methylpyrrole exhibits better charge storage properties than polythiophene coated carbon fiber microelectrodes.     

Effects of conductive ceramic on the electrochemical performance of ZnO for Ni/Zn rechargeable battery

A novel ZnO/conductive-ceramic nanocomposite was prepared by a homogeneous precipitation method. The conductive ceramic with the nominal chemical composition of (ZnO)_0.92(Bi₂O₃)_0.054(Co₂O₃)_0.025(Nb₂O₅)_0.00075(Y₂O₃)_0.00025, as the nucleation sites of ZnO, was prepared by ball milling and surface modification process and its effects on electrochemical performance of ZnO were investigated by charge/discharge cycling, slow rate cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Compared with pure ZnO, the ZnO/conductive-ceramic electrode exhibited improved electrochemical properties, such as superior cycle stability, higher discharge capacity and utilization ratio. When the conductive ceramic content reached 14 wt.%, the discharge capacity of the ZnO/conductive-ceramic nanocomposite hardly declined over 50 cycling test, the average utilization ratio could reach 99.5%, and the electrodes had no obvious weight loss after cycling tests.     

Electrochemical performances of nanostructured vanadium oxides

Vanadium oxide nanotubes (VOx-NTs) and nanourchin (4-phenylbutylamine/vanadium oxide) have been synthesized via one-step hydrothermal treatment. Compounds were analyzed through X-ray powder diffraction, scanning electron microscope, X-ray photoelectron spectroscopy, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). CV curves illustrate reversible redox behavior with charge-discharge cycling corresponding to the reversible lithium intercalation/deintercalation. The EIS spectra were carried out in order to investigate the Li⁺ insertion mechanism at the electrode/electrolyte interface and evaluate the diffusion of Li⁺ within the bulk of cathode material.     

The electrochemical behaviour of an exfoliated graphite electrode in simulated seawater containing oil

An exfoliated graphite (EG) electrode was prepared and the electrochemical response to oil in simulated seawater was studied by means of the potential step technique and electrochemical impedance spectroscopy (EIS). The capacitance and other electrochemical characteristics of the electrode were affected by the presence of oil. The effects of temperature and salinity on the electrochemical behaviour of the EG electrode in NaCl solution containing oil were investigated by EIS. The results showed that the higher the temperature or the salinity, the higher the double layer capacitance of the electrode.     

Electrochemical impedance spectroscopy; a tool for organic coatings optimizations

Electrochemical impedance spectroscopy (EIS) was applied to the optimization of automotive electrodeposited coatings, container interior coatings and industrial maintenance coatings. The electrochemical impedance data were used to predict corrosion protection, film porosity, solution absorption into the coatings and film delamination properties. Variables such as resin contents, crosslink densities, cure temperatures, and solvent types and contents were evaluated for these various types of coatings. In general the electrochemical impedance data correlated well with conventional exposure tests results such as salt fog, cyclic scab corrosion and delamination tests. The impedance spectra permits a rather rapid (15–75 min per sample) assessment of the film's characteristics even when no visually observable changes have occurred. Electrochemical impedance spectroscopy provides a technique to optimize coatings while reducing the time of coating evaluations and gives insight into the chemical and physical properties of the coatings.     

CMOS-compatible metal-stabilized nanostructured Si as anodes for lithium-ion microbatteries

The properties of fully complementary metal-oxide semiconductor (CMOS)-compatible metal-coated nanostructured silicon anodes for Li-ion microbatteries have been studied. The one-dimensional nanowires on black silicon (nb-Si) were prepared by inductively coupled plasma (ICP) etching and the metal (Au and Cu) coatings by successive magnetron sputtering technique. The Cu-coated nb-Si show the most promising electrochemical performance enhancements for the initial specific capacity as well as their cyclability compared to pristine nb-Si. The electrochemical and microstructural properties before and after cycling of the metal-coated nb-Si compared to their pristine counterparts are discussed in detail.     

Synthesis and electrochemical performance of Li4Ti5O12/Ag composite prepared by electroless plating

To improve the electrochemical and anti flatulence performance of Li₄Ti₅O₁₂, Ag modified Li₄Ti₅O₁₂ (LTO) with high electrochemical performance as anode materials for lithium-ion battery was synthesized successfully by two-step solid phase sintering and subsequent electroless plating process in the presence of silver. The effect of Ag modification on the physical and electrochemical properties were investigated by the extensive material characterization of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM). The results showed that the samples possessed single spinel structure, it could be observed that the LTO/Ag composite and the pure LTO shared the same vibration frequencies, which indicated that the crystal structure of LTO didn’t change after electroless plating process, and the particles were uniformly and regularly shaped within 0.5–1.0 µm. Electrochemical performance of the samples were evaluated by the charging and discharging, cyclic voltammetry, electrochemical impedance spectroscopy, cycling and rate tests. It's obvious that the LTO/Ag composite prepared at the 10 min of electroless plating showed the highest performance with capacitance of 182.3 mA h/g at 0.2 C current rates. What's more, the LTO/Ag composites still maintained 92% of its initial capacity even after 50 charge/discharge cycles. Modification of appropriate Ag not only benefits the reversible intercalation and deintercalation of Li⁺, but also improves the diffusion coefficient of lithium ion. Besides, modification of appropriate Ag lower electrochemical polarization leads to higher conductivity and cycle performance of LTO, which is consistent with the results of the best reversible capacities.     

Electrochemical and anticorrosion performances of zinc-rich and polyaniline powder coatings

In this work, hydrochloride polyaniline (PANI-Cl) powder was incorporated as a conductive pigment into powder zinc-rich primer (ZRP) formulations in order to enhance the electronic conduction paths between zinc particles inside the coating and the steel substrate (i.e. percolation). Coatings were applied onto steel substrates and immersed in a 3% NaCl solution at ambient temperature.The protective properties and electrochemical behaviour of coatings were investigated by monitoring the free corrosion potential versus time and by using EIS. It was found that corrosion potential remains cathodic and constant for a long time up to 100 days of immersion. From EIS results, it was shown that the coatings exhibit larger impedance values than those observed with liquid or other zinc-rich powder formulations containing carbon black. From Raman spectroscopy results, it may be proposed that zinc particles in contact with PANI-Cl pigments were passivated. Other zinc particles remain still active which ensures the cathodic protection of the substrate. Moreover, coatings exhibit good barrier properties.     

Electrochemical evaluation of binary Ni2V2O7 nanorods as pseudocapacitor electrode material

Pyrochlore structured nickel vanadate nanorods had been prepared by simple co-precipitation method. It was examined for pseudocapacitor electrode material. Morphological, optical and structural aspects of synthesized materials had been studied using a high-resolution transmission electron microscopy, UV–Visible absorption spectroscopy and powder X-ray diffraction analysis, respectively. The functional groups, stretching and bending vibrations were traced by Fourier transform infrared spectroscopy and the formation of nickel vanadate nanorods was confirmed by the binding energy analysis through X-ray photoelectron spectroscopic studies. The rod-shaped nanostructures of pyro nickel vanadate were confirmed by the scanning electron microscopy and HR-TEM analysis. Electrochemical techniques such as cyclic voltammetry, chronopotentiometry and electrochemical impedance spectroscopy techniques were used to analyse the supercapacitive behaviour of the prepared nanorods. Pyro nickel vanadate nanorods possesses excellent electrochemical stability up to 3000 cycles and the performance retention of about 94.1% was achieved even after 3000 repetitive charge-discharge cycles.     

Structural and electrochemical properties of mixed calcium-zinc spinel ferrites nanoparticles

In the current work, we provide the electrochemical (EC) characteristics and considerable size of Ca-doped ZnFe₂O₄ nanoparticles. Mixed transition metal oxides are widely used as excellent electrode materials in superior supercapacitors because of their superior capacitance, low cost, and environmental friendliness. The prepared nanoparticles were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscope (FE-SEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), and EC methods. The results exhibited that the as-synthesized nanoparticles had a cubic spinel crystal structure and efficient EC properties. The EC properties of the prepared electrodes were explored by cyclic voltammetry (CV), galvanostatic charge/discharge (GCD), and electrochemical impedance spectroscopy (EIS) studies. The Ca_0.1Zn_0.9Fe₂O₄ electrode demonstrated a specific capacitance (SC) ～208 Fg^-1 at a 2 mV/s scan rate due to significant morphological behavior. Therefore may be the prepared materials are the finest electrodes for supercapacitor applications.     

Effect of micron sized particle on the electrochemical properties of nickel-rich LiNi0.8Co0.1Mn0.1O2 cathode materials

Particle size plays an important role in the electrochemical properties of cathode materials for lithium-ion battery, and the sizes of cathode powders are often designed to specific scales to obtain desired rate capacity, cyclic stability, etc. Nano-sized or micron-sized primary/secondary particles were both reported to be helpful to heighten the electrochemical properties of the same material system. However, the relationship between particle size and electrochemical properties of Ni-rich LiNi_0.8Co_0.1Mn_0.1O₂ (NCM-811) has not been discussed in detail. Here, we prepared the pristine NCM-811 powders with various micro-sized particles by using solid state reaction, and investigated the influence of particle size on the electrochemical properties of typical NCM-811 cathode material, to clarify the importance of size effect. The result indicates that pristine NCM-811 cathode powders with D₅₀ = 7.7 μm displayed the best initial discharge specific capacity (224.5 and 169.1 mA h/g at 1/20 C and 1 C rate, respectively) and retention capacity (71.0% at 1 C rate) after 100th cycling at room temperature. The mutual acting mechanism in terms of layered structure, cation mixing degree, polarization state, charge-transfer resistance, and the diffusion ability of lithium-ion was confirmed by XRD, XPS, CV and EIS analyses, respectively.     

Crystalline and amorphous PEO based ceramic coatings on AA6061: Nanoindentation and corrosion studies

Present study reports the detailed nanomechanical and corrosion behaviours of crystalline and amorphous plasma electrolytic oxidation (PEO) coatings developed on Aluminium alloy-6061. The concentration of sodium silicate in the electrolyte is tailored to achieve crystalline and amorphous natures of the PEO coatings. X-ray diffraction (XRD), scanning electron microscopy (SEM) and nanoprofilometry techniques are utilized to investigate microstructural and morphological properties of the PEO coatings. XRD studies confirmed that crystalline ceramic phases are obtained at lower silicate concentration while amorphous nature occurred for comparatively higher concentration of silicate in the electrolyte. Nanoindentation technique is utilized to study the mechanical properties such as hardness (H) and Young's modulus (E) of the PEO coatings. The scatter of the data is treated with well-established Weibull statistical method. Finally, in depth corrosion behaviour of the coatings are investigated by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques. Amorphous coatings exhibited superior mechanical properties compared to the crystalline coatings. This is possibly linked with the presence of aluminosilicate phases and difference in silicon content in the coatings. However, as expected crystalline PEO coatings offer better corrosion resistance than the amorphous coatings and this behaviour is explained in terms of porosity contents of the coatings.