Facile synthesis of flat crystal ZnO thin films by solution growth method: A micro-structural investigation

Flat crystal ZnO thin films were prepared by chemical bath deposition technique onto glass substrates. XRD patterns of the films deposited at about 80 °C and annealed at 200 °C for 1 h in oxygen environment revealed the existence of polycrystalline hexagonal wurtzite phase with c-axis orientation of crystallites in the films. The crystallite size and lattice strain from X-ray line broadening profile were evaluated using the Scherrer method and Williamson–Hall method. Structural parameters such as dislocation density, stacking faults probability, lattice constants, lattice stress, unit cell volume, internal parameter, texture and number of crystallites per unit area have also been calculated. Surface morphology of the films was analyzed by scanning electron microscopy and atomic force microscopy. Photoluminescence spectrum at room temperature exhibited two luminescence centers, one is for UV emission (near band edge emission) located at 3.18 eV and another is for deep level emission located at 2.56 eV.     

Hollow Co9S8 from metal organic framework supported on rGO as electrode material for highly stable supercapacitors

We demonstrate a hydrothermal method to fabricate a composite of reduced graphene oxide (rGO) with hollow Co₉S₈ derived from metal organic framework (MOF), which exhibits a high specific capacitance of 575.9 F/g at 2 A/g and 92.0% capacitance retention after 9000 cycles.     

Electrochemical and FTIR spectroscopic study of CO2 reduction at a nanostructured Cu/reduced graphene oxide thin film

Here we report a facile approach to synthesize a novel nanostructured thin film comprising Cu nanoparticles (NPs) and reduced graphene oxide (rGO) on a glassy carbon electrode (GCE) via the direct electrochemical reduction of a mixture of cupper and graphene oxide (GO) precursors. The effect of the applied potential on the electrochemical reduction of CO₂ was investigated using linear sweep voltammetric (LSV) and chronoamperometric (CA) techniques. Carbon monoxide and formate were found as the main products based on our GC and HPLC analysis. The electrochemical reduction of CO₂ at the Cu/rGO thin film was further studied using in situ ATR-FTIR spectroscopy to identify the liquid product formed at different applied cathodic potentials. Our experimental measurements have shown that the nanostructured Cu/rGO thin film exhibits an excellent stability and superb catalytic activity for the electrochemical reduction of CO₂ in an aqueous solution with a high current efficiency of 69.4% at − 0.6 V vs. RHE, promising for the efficient electrochemical conversion of CO₂ to valuable products.     

Synthesis of a PEBAX-1074/ZnO nanocomposite membrane with improved CO_2 separation performance

In this investigation, polymeric nanocomposite membranes(PNMs) were prepared via incorporating zinc oxide(ZnO) into poly(ether-block-amide)(PEBAX-1074) polymer matrix with different loadings. The neat membrane and nanocomposite membranes were prepared via solution casting and solution blending methods, respectively. The fabricated membranes were characterized by field emission scanning electron microscopy(FESEM) to survey cross-sectional morphologies and thermal gravimetric analysis(TGA)to study thermal stability. Fourier transform infrared(FT-IR) and X-ray diffraction(XRD) analyses were also employed to identify variations of the chemical bonds and crystal structure of the membranes, respectively. Permeation of pure gases, CO_2, CH_4 and N_2 through the prepared neat and nanocomposite membranes was studied at pressures of 3–18 bar and temperature of 25 °C. The obtained results showed that the fabricated nanocomposite membranes exhibit better separation performance compared to the neat PEBAX membrane in terms of both permeability and selectivity. As an example, at temperature of 25 °C and pressure of 3 bar, CO_2 permeability, ideal CO_2/CH_4 and CO_2/N_2 selectivity values for the neat PEBAX membrane are 110.67 Barrer, 11.09 and 50.08, respectively, while those values are 152.27 Barrer,13.52 and 62.15 for PEBAX/ZnO nanocomposite membrane containing 8 wt% ZnO.     

A study on solution deposited CuSCN thin films: Structural,electrochemical, optical properties

A cost-effective successive ionic layer adsorption and reaction (SILAR) method was used to deposit copper (I) thiocyanate (CuSCN) thin films on glass and steel substrates for this study. The deposited thin films were characterized for their structural, morphological, optical and electrochemical properties using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–visible spectroscopy and VersaSTAT potentiostat. A direct band gap of 3.88 eV and 3.6 eV with film thickness of 0.7 μm and 0.9 μm was obtained at 20 and 30 deposition cycles respectively. The band gap, microstrain, dislocation density and crystal size were observed to be thickness dependent. The specific capacitance of the CuSCN thin film electrode at 20 mV/s was 760 F g⁻¹ for deposition 20 cycles and 729 F g⁻¹ for deposition 30 cycles.     

Mesoporous cadmium bismuth niobate (CdBi_2Nb_2O_9) nanospheres for hydrogen generation under visible light

Herein, we report visible light active mesoporous cadmium bismuth niobate(CBN) nanospheres as a photocatalyst for hydrogen(H_2) generation from copious hydrogen sulfide(H_2S). CBN has been synthesized by solid state reaction(SSR) and also using combustion method(CM) at relatively lower temperatures.The as-synthesized materials were characterized using different techniques. X-ray diffraction analysis shows the formation of single phase orthorhombic CBN. Field emission scanning electron microscopy and high resolution-transmission electron microscopy showed the particle size in the range of ~0.5–1 μm for CBN obtained by SSR and 50–70 nm size nanospheres using CM, respectively. Interestingly, nanospheres of size 50–70 nm self assembled with 5–7 nm nanoparticles were observed in case of CBN prepared by CM.The optical properties were studied using UV–visible diffuse reflectance spectroscopy and showed band gap around ~3.0 eV for SSR and 3.1 eV for CM. The slight shift in band gap of CM is due to nanocrystalline nature of material. Considering the band gap in visible region, the photocatalytic activity of CBN for hydrogen production from H_2S has been performed under visible light. CBN prepared by CM has shown utmost hydrogen evolution i.e. 6912 μmol/h/0.5 g which is much higher than CBN prepared using SSR.The enhanced photocatalytic property can be attributed to the smaller particle size, crystalline nature,high surface area and mesoporous structure of CBN prepared by combustion method. The catalyst was found to be stable, active and can be utilized for water splitting.     

The adsorption and activation of formic acid on different anatase TiO_2 surfaces

Formic acid photodegradation is one of the most important reactions in organic pollution control, and helps to improve the hydrogen generation efficiency in titanium dioxide catalyzed water photodecomposition. Based on density functional theory and Reax FF molecular dynamics, the adsorption, diffusion and activation of formic acid on the different anatase TiO_2(101),(001),(010) surfaces are investigated.The result shows that the adsorption of COOH on anatase TiO_2 surface shrinks the energy gap between the dehydrogenation intermediate COOH and HCOO. On the anatase TiO_2(101) surface, the formic acid breaks the O–H bond at the first step with activation energy 0.24 eV, and the consequent break of α-H become much easier with activation energy 0.77 eV. The dissociation of α-H is the determination step of the HCOOH decomposition.     

Photoelectrocatalytic activity of immobilized Yb doped WO_3 photocatalyst for degradation of methyl orange dye

Pure WO_3 and Yb:WO_3 thin films have been synthesized by spray pyrolysis technique. Effect of Yb doping concentration on photoelectrochemical, structural, morphological and optical properties of thin films are studied. X-ray diffraction analysis shows that all thin films are polycrystalline nature and exhibit monoclinic crystal structure. The 3 at% Yb:WO_3 film shows superior photoelectrochemical(PEC) performance than that of pure WO_3 film and it shows maximum photocurrent density(Iph= 1090 μA/cm~2) having onset potentials around +0.3 V/SCE in 0.01 M HClO_4. The photoelectrocatalytic process is more effective than that of the photocatalytic process for degradation of methyl orange(MO) dye. Yb doping in WO_3 photocatalyst is greatly effective to degrade MO dye. The enhancement in photoelectrocatalytic activity is mainly due to the suppressing the recombination rate of photogenerated electron-hole pairs. The mineralization of MO dye in aqueous solution is studied by measuring chemical oxygen demand(COD) values.     

Investigation of structural,optical and luminescent properties of sprayed N-doped zinc oxide thin films

N-doped ZnO (NZO) thin films are synthesized via spray pyrolysis technique in aqueous medium treating zinc acetate and N,N-dimethylformamide as precursors. Influence of N doping on structural, optical and luminescence properties have been investigated. Films are nanocrystalline having hexagonal crystal structure. Raman analysis depicts an existence of NZnO structure in NZO thin film. XPS spectrum of N 1s shows the 400 eV peak terminally bonded, well screened molecular nitrogen (γ-N₂). Lowest direct band gap of 3.17 eV has been observed for 10 at% NZO thin film. The UV, blue, and green deep-level emissions in photoluminescence of NZO films are due to Zn interstitials and O vacancies.     

A non-precious metal catalyst for oxygen reduction prepared by heat-treating a mechanical mixture of carbon black,melamine and cobalt chloride

A non-precious metal catalyst CoMe]C for the oxygen reduction reaction is prepared by heat-treating a mechanical mixture of carbon black, melamine and cobalt chloride at 600 under nitrogen atmosphere for 2 h. The catalytic activity of CoMe/C is characterized by the electrochemical linear sweep voltammetry technique. The onset reduction potential of the catalyst is 0.55 V （vs. SCE） at a scanning rate of 5 mV/s in 0.5 mol/L H2SO4 solution. The formation of the ORR activity sites of CoMe/C is facilitated by metallic β- cobalt.     

A new composite polymer electrolyte based on poly(ethyleneoxide)/ polysiloxane/BMImTFSI/organomontmorillonite

Composite polymer electrolytes based on poly(ethylene oxide)-polysiloxane/l-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide/organomontmorillonite(PEO-PDMS/1L/OMMT) were prepared and characterized.Addition of both an ionic liquid and OMMT to the polymer base of PEO-PDMS resulted in an increase in ionic conductivity.At room temperature,the ionic conductivity of sample PPB100-OMMT4 was 2.19×10~3 S/cm.The composite polymer electrolyte also exhibited high thermal and electrochemical stability and may potentially be applied in lithium batteries.     

Synthesis and properties of polyfluorene copolymers bearing thiophene and porphyrin

To search for more wider absorption and higher charge carriers mobilities materials of polymer solar cell, a series of soluble alternating polyfluorene copolymers were synthesized by palladium-catalyzed Suzuki coupling reaction. Their structures were determined by 1H NMR, IR and UV-vis. And their UV-vis absorption spectra indicated that they had strong absorption over 600 nm spectral range and nearly cover 400-700 nm visible region. The band gaps of copolymers calculated according to cyclic voltammetry （CV） were between 1.96 and 2.03 eV. Polymer：TiO2 bulk-heterojunction films were made from mixtures of polymer and titanium isopropoxide, a precursor for TiO2, via hydrolysis in air overnight. The photoluminescence at 380-800 nm of the blend film of PT-TPP20 （5 mg/mL）：Ti（OC3H7）4 （80 μL/mL） （20% volume fraction） was significantly quenched in the 50% Ti（OC3H7）4 blend film, indicating that rapid and efficient separation of photoinduced electron-hole pairs.     

Liquid phase synthesis of dendritic nickel carbide alloy with high conductivity for advanced energy storage

Alloy materials have attracted increasing attentions because they possess superior electrical conductivity which can contribute to excellent electrochemical performance. Herein a dendritic Ni_3C alloy material has been prepared by the pyrolysis of nickel acetylacetonate employing oleylamine as a reductant and 1-octadecene or octadecane as the solvent. The current–voltage curves indicating that the electrical conductivity of Ni_3C is higher than that of nickel oxide. Electrochemical testing indicates that a high specific capacity of 390 C/g is found in alkaline electrolyte at 0.5 A/g, and deliver excellent rate characteristic as well as cycle life. The excellent electrochemical performance may be attributed to its high electrical conductivity and dendritic nanostructure that can promote diffusion of electrolyte ions. In addition, the AC//Ni_3C asymmetric supercapacitor has been assembled at a cell voltages between 0 and 1.6 V, achieving a maximum energy density of 37 Wh/kg(at a power density of 0.3995 k W/kg), and this manifests that the Ni_3C alloy is a promising electrode material for electrochemical energy storage.     

Electrochemical synthesis of orientation-ordered ZnO nanorod bundles

The high density and orientation-ordered ZnO nanorod bundles with wurtzite structures were prepared on Cu substrates by electrochemical deposition in solution of ZnCl₂ + tartaric acid at a temperature of 90 °C. This approach is a unique and size controlled synthetic method for the large-scale preparation of ZnO nanorod bundles. Cyclic voltammogram measured in solution of the mixture of ZnCl₂ and tartaric acid shows a restraining role of tartaric acid for the electro-reduction of Zn(II). The formation mechanism of ZnO on the surface of the cathode can be explained that the high temperature (⩾90 °C) promotes the corrosion of electrodeposited Zn via reacting with H₂O and O₂ to form the stable passive phase of ZnO. The compositions of the nanorod bundles can be entirely ZnO or Zn and ZnO composites determined by the temperature and deposition rate. The photoluminescence (PL) properties indicate that these ZnO deposits are highly crystallized and of excellent optical quality.     

Glucose biosensor based on new carbon nanotube-gold-titania nano-composites modified glassy carbon electrode

In this paper, a novel biosensor was prepared by immobilizing glucose oxidase （GOx） on carbon nanotube-gold-titania nanocomposites （CNT/Au/TiO2） modified glassy carbon electrode （GCE）. SEM was initially used to investigate the surface morphology of CNT/Au/TiO2 nanocomposites modified GCE, indicating the formation of the nano-porous structure which could readily facilitate the attachment of GOx on the electrode surface. Cyclic voltammogram （CV） and electrochemical impedance spectrum （EIS） were further utilized to explore relevant electrochemical activity on CNT]Au/TiO2 nanocomposites modified GCE. The observations demonstrated that the immobilized GOx could efficiently execute its bioelectrocatalytic activity for the oxidation of glucose. The biosensor exhibited a wider linearity range from 0.1 mmol L-1 to 8 mmol L^-1 glucose with a detection limit of 0.077 mmol L^- 1.     

Visible light driven photocatalytic activity of ZnO/CuO nanocomposites coupled with rGO heterostructures synthesized by solid-state method for RhB dye degradation

Metal oxide frame works along with carbon materials have been attracting tremendous attention of researches as the potential materials for energy and environmental remediation. In the present work heterostructures of (ZnO/CuO)/rGO ternary nanocomposites were synthesized by solid-state method. The crystalline structure of the nanoparticles was obtained from the XRD analysis. Optical band gap of the ZnO nanoparticles (3.1 eV) is tuned to 2.8 eV in the synthesized (ZnO/CuO)/rGO ternary nanocomposites. Field emission scanning electron microscope images of the (ZnO/CuO)/rGO ternary nanocomposites revealed formation of well-developed flowers like morphology of (ZnO/CuO) nanoparticles on rGO sheets. Photoluminescence spectroscopy analysis of (ZnO/CuO)/rGO ternary nanocomposites show enhancement in the electron-hole pair separation and thereby diminishing electron-hole pairs recombination rates effectively. In the present work, the photocatalytic activity of the ZC₃G₁₅ ternary nanocomposites show 99% and 93% of degradation efficiency respectively against RhB dye and 4-chlorophenol for 20 min under visible light irradiation. Thus, the simple solid-state method provides the effective ternary nanocomposites heterostructures light harvesting material for energy and environmental remediation.     

Radioluminescence in ZnO

ZnO powders were obtained by proteic sol–gel process using zinc sulfate as the precursor. They have an energy gap of 3.3 eV and display a radioluminescence signal centered in 550 nm, which corresponds to 2.6 eV. This signal has appeared due to defects in the gap (energy sublevels) caused by the distortions in its crystalline structure, which result from the loss of sulfur at high temperature. These powders were characterized by radioluminescence, XRD, SEM, EDS and DTA/TG.     

Electrochemical impedance spectroscopy of ZnO nanostructures

The paper reports on the use of electrochemical impedance spectroscopy to determine the doping character and carrier density of freshly prepared and annealed ZnO nanostructures. The ZnO nanostructures were obtained by chemical oxidation of metallic Zn in a 5% N,N-dimethylformamide (DMF) aqueous solution at 95 °C for 24 h. The as-grown nanostructured ZnO samples display a high donor density of 3.71 ± 0.88 × 10²¹ cm^?3. Annealing at 100 and 200 °C did not have any effect on the donor density while thermal annealing at 300 °C in air for 1 h induced a decrease in the doping concentration without affecting the surface morphology.     

KOH activated carbon derived from biomass-banana fibers as an efficient negative electrode in high performance asymmetric supercapacitor

Here we demonstrate the fabrication, electrochemical performance and application of an asymmetric supercapacitor(AS) device constructed with β–Ni(OH)_2/MWCNTs as positive electrode and KOH activated honeycomb-like porous carbon(K-PC) derived from banana fibers as negative electrode. Initially,the electrochemical performance of hydrothermally synthesized β–Ni(OH)_2/MWCNTs nanocomposite and K-PC was studied in a three-electrode system using 1 M KOH. These materials exhibited a specific capacitance(Cs) of 1327 F/g and 324 F/g respectively at a scan rate of 10 m V/s. Further, the AS device i.e.,β–Ni(OH)_2/MWCNTs//K-PC in 1 M KOH solution, demonstrated a Cs of 156 F/g at scan rate of 10 m V/s in a broad cell voltage of 0–2.2 V. The device demonstrated a good rate capability by maintaining a Cs of 59 F/g even at high current density(25 A/g). The device also offered high energy density of 63 Wh/kg with maximum power density of 5.2 kW/kg. The AS device exhibited excellent cycle life with 100% capacitance retention at 5000 th cycle at a high current density of 25 A/g. Two AS devices connected in series were employed for powering a pair of LEDs of different colors and also a mini fan.     

Preparation of vertically-aligned nickel nanowires with anodic aluminum oxide templates and their application as field emitters

In this study, well-ordered and vertically-aligned nickel nanowires (NiNWs) with a controllable length were grown inside the nanopores of anodic alumina oxide templates (AAOTs) using a simple electrochemical deposition (ECD) method. The electron field emission characteristics of the prepared NiNWs within AAOTs with two pore diameters (100 and 200 nm) and length in the range of 2.7–22 μm were measured and discussed. The turn-on field/the enhancement factor of 8.5 and 7-μm-long NiNWs prepared within 100 and 200 pore diameter AAOTs, respectively, were about 3.46 V/μm/17,621 and 4.8 V/μm/5001, respectively, according to I–V measurements.