Synthesis and electrochemical performance of amorphous nickel hydroxide codoped with Fe<Superscript>3+</Superscript> and CO<Stack><Subscript>3</Subscript><Superscript>2−</Superscript></Stack>

Amorphous nickel hydroxide codoped with Fe³⁺ and CO₃²⁻ was synthesized by micro-emulsion precipitation method combined with rapid freezing technique. The microstructure and composition of the sample were characterized by X-ray diffraction and IR analysis. The electrochemical performance of the sample was analyzed by cyclic voltammetry, electrochemical impedance spectroscopy, and charge–discharge tests. The results showed that the Fe³⁺ and CO₃²⁻ codoping enhances the amorphous feature of the prepared nickel hydroxide. Moreover, the Fe³⁺ and CO₃²⁻ codoping could increase the specific capacity and improve the electrochemical reversibility of the amorphous nickel hydroxide electrode.     

Structure and electrochemical performance of Y(III) and Al(III) codoped amorphous nickel hydroxide

Amorphous nickel hydroxide codoped with rare earths Y(III) and Al(III) has been synthesized by the chemical precipitation method combined with the rapid freezing technique. The microstructure and morphology of the prepared sample were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectra. The electrochemical performance of the sample was characterized by the charge/discharge test and cyclic voltammetry. The results show that this amorphous nickel hydroxide codoped with Y(III) and Al(III) has many structural defects and therefore results in a relatively high specific capacity (351.83 mA h g^?1 at a charge/discharge rate of 0.2 C) and good electrochemical reversibility.     

Synthesis,structure stability and magnetic properties of nanocrystalline Ag–Ni alloy

Silver–nickel alloy nanoparticles with an average size of 30–40 nm were synthesized by chemically reducing the mixture of silver and nickel salts using sodium borohydride. The structure and the magnetic properties of the alloy samples with different compositions were investigated. The phase stability of the material was analysed after annealing the sample in vacuum at various temperatures. The material exhibits single fcc phase which is stable up to 400 °C and Ni precipitation sets in when the sample is annealed to 500 °C. The thermal analysis using DSC was carried out to confirm the same. The alloy compositions are found to be in close correlation with the metal salt ratios in the precursors. The synthesized samples exhibit weak paramagnetic to ferromagnetic behaviour. The magnetic measurements reveal that by adjusting the precursor ratio, the Ni content in the material can be altered and hence its magnetic properties tailored to suit specific requirements. The formation of Ag–Ni alloy is confirmed by the observed Curie temperature from the magneto thermogram. Annealing the sample helps to produce significant enhancement in the magnetization of the material.     

Synthesis and electrochemical performance of α-nickel hydroxide codoped with Al3+ and Ca2+

α-Nickel hydroxide codoped with Al³⁺ and Ca²⁺ was prepared by chemical coprecipitation method. The phase structure and surface morphology of the prepared samples were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The electrochemical performances of the prepared samples were analyzed by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and charge/discharge tests. XRD and SEM tests reveal that the Al³⁺/Ca²⁺ codoped α-nickel hydroxide has a relatively good crystallization and a very coarse surface. Electrochemical tests show that the Al³⁺/Ca²⁺ codoped α-nickel hydroxide has higher proton diffusion coefficient, lower electrochemical reaction resistance, and higher discharge capacity (395.3 mAh g^?1 at 0.2 C) than the Al³⁺ singly doped α-nickel hydroxide, which indicates its potential application as an electrode material for secondary alkaline batteries.     

Electrochemical performances of FePO<Subscript>4</Subscript>-positive active mass prepared through a new sol–gel method

This investigation is a contribution to the research on alternative cathode materials with much more promising performances for lithium batteries. It deals with the electrochemical properties of iron phosphate compound FePO₄, chemically prepared through the so-called sol–gel Pechini process, terminated by a calcination of the product precursor at temperatures (T _c) ranging between 350°C and 650°C. A crystalline phase was obtained for temperatures ≥400°C. The particle size decreased with the decrease in T _c, giving rise to a Brunauer–Emmett–Teller (BET)-specific surface area, S _BET, as high as 28 m² g⁻¹ for the sample annealed at 400°C. The electrochemical properties of FePO₄-based composite cathodes were characterized on three-electrode laboratory cells. Charge–discharge cycling determined a maximum reversible capacity of 132 mAh g⁻¹, which fell with the increase in T _c. A direct correlation was established between the activity of the material and its active surface area.     

Nanosized IrO<Subscript>2</Subscript> electrocatalysts for oxygen evolution reaction in an SPE electrolyzer

Nanosized IrO₂ electrocatalysts (d ~ 7–9 nm) with specific surface area up to 100 m² g⁻¹ were synthesized and characterized for the oxygen evolution reaction in a solid polymer electrolyte (SPE) electrolyzer. The catalysts were prepared by a colloidal method in aqueous solution and a subsequent thermal treatment. An iridium hydroxide hydrate precursor was obtained at ~100 °C, which was, successively, calcined at different temperatures from 200 to 500 °C. The physico-chemical characterization was carried out by X-ray diffraction (XRD), thermogravimetry–differential scanning calorimetry (TG–DSC) and transmission electron microscopy (TEM). IrO₂ catalysts were sprayed onto a Nafion 115 membrane up to a loading of 3 mg cm⁻². A Pt catalyst was used at the cathode compartment with a loading of 0.6 mg cm⁻². The electrochemical activity for water electrolysis of the membrane-electrode assemblies (MEAs) was investigated in a single cell SPE electrolyzer by steady-state polarization curves, impedance spectroscopy and chrono-amperometric measurements. A maximum current density of 1.3 A cm⁻² was obtained at 1.8 V and 80 °C for the IrO₂ catalyst calcined at 400 °C for 1 h. A stable performance was recorded in single cell for this anode catalyst at 80 °C. The suitable catalytic activity and stability of the most performing catalyst were interpreted in terms of proper combination between nanostructure and suitable morphology.     

Synthesis of Co-coated lithium manganese oxide and its characterization as cathode for lithium ion battery

Co-coated LiMn₂O₄ was synthesized by electroless plating. The phase identification, surface morphology, and electrochemical properties of the synthesized powders were studied by X-ray diffraction, scanning electron microscopy, electrochemical impedance spectroscopy, and galvanostatic charge–discharge experiments, respectively. The result shows that Co-coated LiMn₂O₄ particle has a coarse surface with a lot of holes. The specific capacity of Co-coated LiMn₂O₄ is 118 mAh g⁻¹, which is a bit less than 123 mAh g⁻¹ for the uncoated LiMn₂O₄. The capacity retention of Co-coated LiMn₂O₄ is 11% higher than the uncoated LiMn₂O₄ when the electrode is cycled at room temperature for 20 times. When cycled at the temperature of 55 °C, the capacity retention of Co-coated LiMn₂O₄ becomes 15% higher than the uncoated one.     

Pseudo-capacitive properties of LiCoO<Subscript>2</Subscript>/AC electrochemical capacitor in various aqueous electrolytes

LiCoO₂ particles were synthesized by a sol-gel process. X-ray diffraction analysis reveals that the prepared sample is a single phase with layered structure. A hybrid electrochemical capacitor was fabricated with LiCoO₂ as a positive electrode and activated carbon (AC) as a negative electrode in various aqueous electrolytes. Pseudo-capacitive properties of the LiCoO₂/AC electrochemical capacitor were determined by cyclic voltammetry, charge–discharge test, and electrochemical impedance measurement. The charge storage mechanism of the LiCoO₂-positive electrode in aqueous electrolyte was discussed, too. The results showed that the potential range, scan rate, species of aqueous electrolyte, and current density had great effect on capacitive properties of the hybrid capacitor. In the potential range of 0–1.4 V, it delivered a discharge specific capacitance of 45.9 Fg^–1 (based on the active mass of the two electrodes) at a current density of 100 mAg^–1 in 1 molL^–1 Li₂SO₄ aqueous electrolyte. The specific capacitance remained 41.7 Fg^–1 after 600 cycles.     

Enhanced electrochemical properties of LiMnPO<Subscript>4</Subscript>/C via Li-site substitution with Mg

Li_0.94Mg_0.03MnPO₄/C composite cathode materials for lithium ion battery with different carbon contents are synthesized by sol–gel method followed by heat treatment in the air. Environmental scanning electron microscopy measurements show that both firing temperature and carbon content affect the morphology of the end products. X-ray powder diffraction analysis indicates that the samples are olivine-structured. The galvanostatic charge–discharge results show that the optimal firing temperature registers 400 °C and that the electrochemical performances of Li_0.94Mg_0.03MnPO₄/C are improved by elevating its carbon amount. The sample with an initial conductive carbon content of 20 wt.% gives the best performances; when tested at the rate of 0.02C, 0.1C, and 1.0C between 2.8 and 4.4 V, its initial discharge capacity reaches 145.8, 103.0, and 72.8 mAhg⁻¹, respectively, and maintains at 100.1, 77.6, and 65.4 mAhg⁻¹, respectively, after 100 cycles.     

Investigation on PVDF-HFP microporous membranes prepared by TIPS process and their application as polymer electrolytes for lithium ion batteries

Poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) microporous membranes were prepared via thermally induced phase separation (TIPS) process. Then they were immersed in a liquid electrolyte to form polymer electrolytes. The effects of polymer content in casting solution on the morphology, crystallinity, and porosity of the membranes were studied by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and a mercury porosimeter, respectively. Ionic conductivity, lithium-ion transference number, and electrochemical stability window of corresponding polymer electrolytes were characterized by AC impedance spectroscopy, DC polarization/AC impedance combination method, and linear sweep voltammetry, respectively. The results showed that spherulites and “net-shaped” structure coexisted for the membranes. Polymer content had no effect on crystal structure of the membranes. The maximum transference number was 0.55. The temperature dependence of ionic conductivity followed the Vogel–Tammann–Fulcher (VTF) relation. The maximum ionic conductivity was 2.93 × 10⁻³ Scm⁻¹ at 20 °C. Electrochemical stability window was stable up to 4.7 V (vs. Li⁺/Li).     

Effect of LiBOB as additive on electrochemical properties of lithium–sulfur batteries

The effect of varying amounts (in the range 1–10 wt.%) of LiBOB (lithium bis(oxalato) borate) as additive in mixed liquid electrolyte on the electrochemical performance of lithium–sulfur batteries is investigated at room temperature. The electrochemical impedance spectroscopy (EIS) of lithium anode with LiBOB has two semicircles, corresponding to charge transfer impedance and ion migration impedance, respectively. The lithium anode with LiBOB shows a higher ion migration impedance, which could reduce the ionic diffusion rate in the anode. Scanning electron microscopy (SEM) observations shows that lithium anode with LiBOB has a smoother and denser surface morphology than the anode without LiBOB. The lithium–sulfur batteries with LiBOB shows the improvement of both the discharge capacity and cycle performance, a maximum discharge capacity of 1,191 mA h g⁻¹ is obtained with 4 wt.% LiBOB. The lithium–sulfur batteries with 4 wt.% LiBOB can maintain a reversible capacity of 756 mA h g⁻¹ after 50 cycles.     

Joined ellipsometry and voltametry investigation on the second discharge plateau in Ni(OH)2

The electrochemical properties of nickel hydroxide, produced via an electrodialysis process are studied by means of cyclic voltametry and in-situ ellipsometry methods. The Ni(OH)₂ electrodes are thin layers of nickel hydroxide powder deposited on a polished platinum substrate. Electrochemical and optical properties are investigated in a voltage domain including the so-called “second discharge process”. The reduction of nickel hydroxide proceeds at two successive potentials with a recovering of the initial optical data only after the second discharge step. The first discharge step leads to a nickel hydroxide not fully discharged while the second discharge step is coupled both to a sudden change in the nickel hydroxide properties and an agglomeration of particles phenomenon. Project financed by the E.U., program Brite Euram BRPR-CT97-0515 (NEARBY) Paper presented at the 7th Euroconference on Ionics, Calcatoggio, Corsica, France, Oct. 1–7, 2000.     

Synthesis of LiCoPO4 as cathode material for lithium-ion batteries by the rheological phase method

LiCoPO₄ has been successfully synthesized by a simple rheological phase method. The effects of synthesis temperature on the properties of LiCoPO₄ are also investigated. The results show that a well-crystallized olivine structure LiCoPO₄ with no obvious impurity phase is obtained. The electrochemical properties of LiCoPO₄ were examined by galvanostatic charge/discharge tests, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The results indicate that the sintering temperature has a significant effect on the electrochemical properties of LiCoPO₄. The sample fired at 600 °C shows the best electrochemical properties. The initial discharge capacity is 101.0, 96.8, and 91.6 mAh g^?1 at 0.1, 0.2, and 1 C, respectively. The significantly improved electrochemical properties of LiCoPO₄ are attributed to the better crystallized rheological phase production with better dispersed and smaller particles, which can greatly facilitate the diffusion of Li⁺.     

Perovskite barium zirconate titanate nanoparticles directly synthesized from solutions

Perovskite barium zirconate titanate nanoparticles (25–20 nm in diameter) were synthesized at low temperatures and under ambient pressure using titanium alkoxide, zirconium alkoxide and barium hydroxide as the starting materials. Microstructural analyses by X-ray diffraction and transmission electron microscopy indicated that the powders were nano-scaled, well crystallized, and had a perovskite phase. It is proposed that an acid–base neutralization reaction is the key mechanism behind the formation of such nanoparticles.     

Magnetic and Gas Sensing Property of Nanosized NiFe2O4 Powders Synthesized by Pulsed Wire Discharge

Nickel ferrite (NiFe₂O₄) powders were synthesized by pulsed wire discharge method. X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses show that only nickel ferrite spinel and no other phase was observed in the powders. Mean size of the obtained particles strongly depended on the oxygen pressure: the higher oxygen pressure corresponds to larger powder size, as determined by Brunauer–Emmet–Teller (BET). The room temperature saturation magnetization of the synthesized powders was 42–46 emu/g depending on the powder size. These powders also showed high chlorine sensitivity at about 280–360°C, and a good linear sensitivity with chlorine concentration.     

Acrylamide based proton conducting polymer gel electrolyte for electric double layer capacitors

A new class of polymer gel electrolyte (PGE) was synthesized using acrylamide as host polymer and LiClO₄ as dopant. The polymer gel was subjected to electrochemical AC impedance analysis and thermal analysis. The polymer has conductivity in the order of 10⁻³ S cm⁻¹ at ambient temperature. Thermogravimetric analysis (TGA) revealed the effect of dopant on host polymer matrix. A supercapacitor was fabricated using acrylamide based polymer gel electrolyte with activated carbon as electrode material and it was subjected to various electrochemical techniques like cyclic voltammetry, electrochemical AC impedance analysis and galvanostatic charge–discharge tests at various current densities. From cyclic voltammetry a specific capacitance of 28 F/g was obtained at a scan rate of 10 mV/s. The capacitor had good self-discharge behavior and good cycle life of more than 10,000 cycles. The coulombic efficiency was more than 95%. These results indicate that this acrylamide-based polymer gel electrolyte doped with LiClO₄ is a potential electrolyte for electric double-layer capacitors (EDLCs).     

Effect of chitosan on deposition of LiCoO2 thin film for Li-ion batteries

Deposition of LiCoO₂ thin film using chitosan-added precursor solution was found to be a cost-effective way to fabricate cathode for Li-ion thin film batteries. The structures and electrochemical performance of such LiCoO₂ cathode were characterized by using an X-ray diffracotmeter (XRD), FTIR and charge–discharge tests. After annealing at ca. 500 °C, the results of XRD showed that the LiCoO₂ gel started to crystallize and showed hexagonal phase with a space group of R3?m. The enhanced stability of the precursor solution by the addition of chitosan is attributed to the complexation between metal ions and the ?NH₂ groups of chitosan.The electrochemical behaviour for the deposited films calcined at 700 °C for 4 h was also characterized by charge–discharge test. The result revealed that the film deposited from chitosan-containing precursor solution possesses an initial discharge capacity of 129 mAh g^? 1.     

A PEG-assisted rheological phase reaction synthesis of 5LiFePO<Subscript>4</Subscript>⋅Li<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript>/C as cathode material for lithium ion cells

5LiFePO₄⋅Li₃V₂(PO₄)₃/C composite cathode material is synthesized by a polyethylene glycol (PEG)-assisted rheological phase method. As a surfactant and dispersing agent, PEG can effectively inhabit the aggregation of colloidal particles during the formation of the gel. Meanwhile, PEG will coat on the particles to play the role of carbon source during the sintering. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy, and electrochemical methods. XRD results indicate that the 5LiFePO₄⋅Li₃V₂(PO₄)₃/C composites are well crystallized and contain olivine-type LiFePO₄ and monoclinic Li₃V₂(PO₄)₃ phases. The composite synthesized at 650 °C exhibits the initial discharge capacities of 134.8 and 129.9 mAh g⁻¹ and the capacity retentions of 96.2 and 97.1 % after 50 cycles at 1C and 2C rates, respectively.     

Growth of monodisperse nanocrystals of cerium oxide during synthesis and annealing

Monodisperse cerium oxide nanocrystals have been successfully synthesised using simple ammonia precipitation technique from cerium(III) nitrate solution at different temperatures in the range 35–80 °C. The activation energy for growth of CeO₂ nanocrystals during the precipitation is calculated as 11.54 kJ/mol using Arrhenius plot. Average crystal diameter was obtained from XRD analysis, HR-TEM and light scattering (PCS). The analysis of size data from HR-TEM images and PCS clearly indicated the formation of highly crystalline CeO₂ particles in narrow size range. CeO₂ nanocrystals precipitated at 35 °C were further annealed at temperatures in the range 300–700 °C. The activation energy for crystal growth during annealing is also calculated and is close to the reported values. An effort is made to predict the mechanism of crystal growth during the precipitation and annealing.     

Structure and lithium storage performances of nickel hydroxides synthesized with different nickel salts

Nickel hydroxides with hierarchical micro-nano structures are prepared by a facile homogeneous precipitation method with different nickel salts (Ni(NO₃)₂·6H₂O, NiCl₂·6H₂O, and NiSO₄·6H₂O) as raw materials. The effect of nickel sources on the microstructure and lithium storage performance of the nickel hydroxides is studied. It is found that all the three prepared samples are α-nickel hydroxide. The nickel hydroxides synthesized with Ni(NO₃)₂·6H₂ or NiCl₂·6H₂O show a similar particle size of 20–30 μm and are composed of very thin nano-sheets, while the nickel hydroxide synthesized with Ni(SO₄)₂·6H₂O shows a larger particle size (30–50 μm) and consists of very thin nano-walls. When applied as anode materials for lithium-ion batteries (LIBs), the nickel hydroxide synthesized with NiSO₄·6H₂O exhibits the highest discharge capacity, but its cyclic stability is very poor. The nickel hydroxides synthesized with NiCl₂·6H₂O exhibit higher discharge capacity than the nickel hydroxides synthesized with Ni(NO₃)₂·6H₂O, and both of them show much improved cyclic stability and rate capability as compared to the nickel hydroxide synthesized with Ni(SO₄)₂·6H₂O. Moreover, pseudocapacitive behavior makes a great contribution to the electrochemical energy storage of the three samples. The discrepancies of lithium storage performance of the three samples are analyzed by ex-situ XRD, FT-IR, electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV) tests.