Effect of annealing temperature on optical and electrochemical properties of chitosan–ZnO nanostructure

Chitosan–ZnO nanostructures were prepared by chemical precipitation method using different concentration of zinc chloride and sodium hydroxide solutions. Nanorod-shaped grains with hexagonal structure for samples annealed at 300 °C and porous structure with amorphous morphology for samples annealed at 600 °C were revealed in SEM analysis. X-ray diffraction patterns confirmed the hexagonal phase ZnO with crystallite size found to be in the range of ~24.15–34.83 nm. Blue shift of UV–Vis absorption shows formation of nanocrystals/nanorods of ZnO with marginal increase in band gap. Photoluminescence spectra show that blue–green emission band at 380–580 nm. The chitosan–ZnO nanostructures used on surface of a glassy carbon electrode gives the oxidation peak potential at ~0.6 V. The electrical conductivity of chitosan–ZnO composites were observed at 2.1?×?10^?5 to 2.85?×?10^?5?S/m. The nanorods with high surface area and nontoxicity nature of chitosan–ZnO nanostructures observed in samples annealed at 300 °C were suitable as a potential material for biosensing.     

Sensitive voltammetric determination of cysteamine using promazine hydrochloride as a mediator and modified multi-wall carbon nanotubes carbon paste electrodes

This paper presents a sensitive electrochemical method for the determination of cysteamine (CA) using promazine hydrochloride-modified multi-wall carbon nanotubes carbon paste electrode (PrH/MWCNTs CPE). Because of the good electrochemical activity of MWCNTs and the acceptable performance of promazine hydrochloride (PrH) as an electrocatalytic mediator, the modified electrode significantly enhanced the sensitivity for the detection of CA in comparison to the bare carbon paste electrode (CPE). All chemical parameters such as pH of solution, concentration of PrH and kinetic parameters of the system were investigated. Linear sweep voltammetric (LSV) method was used to follow the electrocatalytic effect of CA on the current–potential response of PrH. Under optimum conditions, the obtained net peak current ?I _p(I _sample???I _blank) was linear with CA concentrations in two dynamic ranges of 2.0–346.5 μmol l^?1 (?I _p?=?(0.0195?±?0.0043)C _CA?+?(0.7648?±?0.0397) (r ²?=?0.9948)) and 346.5–1,912.5 μmol l^?1 (?I _p?=?(0.0100?±?0.0026)C _CA?+?(3.8981?±?0.0828) (r ²?=?0.9911)) with a detection limit of 0.8 μmol l^?1. Finally, the PrH/MWCNTs CPE was successfully applied for the determination of CA in urine and drug samples with satisfactory results.     

Voltammetric sensor for simultaneous determination of ascorbic acid,acetaminophen, and tryptophan in pharmaceutical products

A novel carbon paste electrode modified with carbon nanotubes and 5-amino-2′-ethyl -biphenyl-2-ol was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for electrocatalytic oxidation of ascorbic acid (AA), is described. The electrode was employed to study the electrocatalytic oxidation of AA, using cyclic voltammetry, chronoamperometry, and square-wave voltammetry (SWV) as diagnostic techniques. It has been found that the oxidation of AA at the surface of modified electrode occurs at a potential of about 250 mV less positive than that of an unmodified carbon paste electrode. SWV exhibits a linear dynamic range from 2.0?×?10^?7 to 5.0?×?10^?4 M and a detection limit of 1.0?×?10^?7 M for AA. In addition, this modified electrode was used for simultaneous determination of AA, acetaminophen (AC), and tryptophan (TRP). Finally, the modified electrode was used for determination of AA, AC, and TRP in pharmaceutical products.     

A facile low temperature synthesis of TiO2 nanorods for high efficiency dye sensitized solar cells

Titania (TiO₂) nanorods have been synthesized with controlled size for dye-sensitized solar cells (DSSCs) via hydrothermal route at low hydrothermal temperature of 100 °C for 24 h. The titania nanorods were characterized using XRD, SEM, TEM/HRTEM, UV-vis Spectroscopy, FTIR and BET specific surface area (S _BET), as well as pore-size distribution by BJH. The results indicated that the bulk traps and the surface states within the TiO₂ nanorods films have enhanced the efficiency of DSSCs. The size of the titania nanorods was 6.7 nm in width and 22 nm in length. The high surface area can provide more sites for dye adsorption, while the fast photoelectron-transfer channel can enhance the photogenerated electron transfer to complete the circuit. The specific surface area S _BET was 77.14 m²?g^?1 at the synthesis conditions. However, the band gap energy of the obtained titania nanorods was 3.2 eV. The oriented nanorods with appropriate lengths are beneficial in improving the electron transport property and thus leading to the increase of photocurrent, together enhancing the power conversion efficiency. A nearly quantitative absorbed photon-to-electrical current conversion achieved upon excitation at wave length of 550 nm and the power efficiency was enhanced from 5.6 % for commercial TiO₂ nanoparticles Degussa (P25) cells to 7.2 % for TiO₂ nanorods cells under AM 1.5 illumination (100 mW?cm^?2). The TiO₂ cells performance was improved due to their high surface area, hierarchically mesoporous structures and fast electron-transfer rate compared with the Degussa (P25).     

Electrochemical synthesis and performance of PANI electrode material for electrochemical capacitor

Polyaniline (PANI) electrode materials doped with sulfuric acid (H₂SO₄) were prepared by cyclic voltammetry (CV) method in different reaction conditions. The structure and morphology of PANI samples were characterized by Fourier transform infrared spectroscopy and scanning electron microscope. The electrochemical properties of PANI samples were studied by CV, galvanostatic charge/discharge, and electrochemical impedance spectroscopy tests. Additionally, the effects of reaction conditions including aniline concentration, voltammetry scan rate, and deposition time on the morphology and properties of PANI samples were investigated in detail. The results showed that the PANI synthesized under the optimal conditions of 0.2 mol?L^?1 aniline, scan rate 20 mV?s^?1, and deposition time 50 min is in the form of nanorods with a cross-linked network structure. It exhibits an outstanding capacitive performance with good cycle stability and high rate performance. Besides, the specific capacitance of PANI is as high as 757 F?g^?1.     

Voltammetric determination of hydroxylamine in water samples using a 1-benzyl-4-ferrocenyl-1H-[1,2,3]-triazole/carbon nanotube-modified glassy carbon electrode

A modified glassy carbon electrode has been constructed using a 1-benzyl-4-ferrocenyl-1H-[1,2,3]-triazole along with multiwalled carbon nanotubes. The electrochemical behaviour of modified electrode has been investigated by cyclic voltammetry. Electrocatalytic activity of the modified electrode was investigated for the oxidation of hydroxylamine in 0.1 M phosphate-buffered solution of pH 8. The modified electrode showed electrocatalytic response to the oxidation of hydroxylamine at the potential of 330 mV. The linear range and detection limit for the detection of hydroxylamine in the optimum condition were found to be 4.0?×?10^?7 to 6.75?×?10^?4 M and 28.0?±?1.0 nM, respectively. Finally, the method was employed for the determination of hydroxylamine in water samples.     

Hydrothermal synthesis of carbon- and reduced graphene oxide-supported CoMoO4 nanorods for supercapacitor

Hybrid CoMoO₄ nanorods with carbon (C) and graphene oxide (rGO) are successfully synthesized via one-step hydrothermal process. Hybrid α-CoMoO₄ nanorods have shown excellent electrochemical performances compared to pristine CoMoO₄ in alkaline electrolyte. Specifically, CoMoO₄/C nanorod exhibits a maximum specific capacitance of 451.6 F g^?1 at the current density of 1 A g^?1, whereas CoMoO₄/rGO shows high specific capacitance of 336.1 F g^?1 at the same current density. Both the hybrid nanorods show good rate capability even at high current density of 20 A g^?1 and long-term cyclic stability. The observed electrochemical features of the hybrid CoMoO₄ nanostructure could be attributed to the presence of highly conductive carbonaceous material on unique one-dimensional nanorod microstructure which enhances the electrical conductivity of the nanorods thereby allowing faster electrolyte ion diffusion during the redox process.     

Synthesis of carbon-coated Fe3O4 nanorods as electrode material for supercapacitor

Carbon-coated Fe₃O₄ and pure Fe₃O₄ nanorods are synthesized via hydrothermal reaction and subsequent sintering procedure. The as-prepared products characterized by X-ray diffraction and scanning electron microscopy analysis indicate that carbon coating does not affect the structure and morphology of Fe₃O₄. Transmission electron microscope shows that Fe₃O₄ nanorods are homogeneously coated by carbon layer with a thickness of approximately 2 nm. The electrochemical properties measured by cyclic voltammetry, galvanostatic charge–discharge cycling and electrochemical impedance spectroscopy tests show that carbon-coated Fe₃O₄ (Fe₃O₄/C) nanorods present improved electrochemical performance due to the carbon layer. A specific capacitance of 275.9 F?g^?1 is achieved at a current density of 0.5 A g^?1 in 1 M Na₂SO₃ aqueous solution for the Fe₃O₄/C nanorods in comparison to that of 208.6 F?g^?1 for pure Fe₃O₄.     

Electrochemical and catalytic investigations of epinephrine,acetaminophen and folic acid at the surface of titanium dioxide nanoparticle-modified carbon paste electrode

In the present paper, the use of a carbon paste electrode modified with 1-(4-(1, 3-dithiolan-2-yl)-6, 7-dihydroxy-2-methyl-6, 7-dihydrobenzofuran-3-yl)ethanone (DDE) and TiO₂ nanoparticles prepared by a simple and rapid method was described. The modified electrode showed excellent properties for electrocatalytic oxidization of epinephrine (EP), acetaminophen (AC) and folic acid (FA). The apparent charge transfer rate constant, k _s?=?1.14 s^?1, and transfer coefficient, α?=?0.54, for electron transfer between the modifier and carbon paste electrode were calculated. It has been found that under optimum condition (pH?=?7.0) in cyclic voltammetry, the oxidation of EP occurs at a potential about 280 mV less positive than that of an unmodified carbon paste electrode. The values of transfer coefficients (α?=?0.46), catalytic rate constant (k?=?1.2?×?10⁴ M^?1 s^?1) and diffusion coefficient (D?=?2.70?×?10^?5 cm² s^?1) were calculated for EP. Differential pulse voltammetry (DPV) exhibited two linear dynamic ranges of 0.5 to 50.0 μM and 50.0 to 1,000 μM for EP. This modified electrode is quite effective not only for the detection of EP, AC and FA but also for the simultaneous determination of these species in a mixture. The limit of detection for EP, AC and FA is 0.10, 1.80 and 2.36 μM, respectively.     

One-pot,large-scale synthesis silica-encapsulated NIR alloy quantum dots CdSeTe within short time

Hydrothermal process has been employed to synthesize titanium oxide (TiO₂) bottle brush. The nanostructured bottle brushes with tetragonal nanorods of ~75 nm diameter have been synthesized by changing the nature of the precursors and hydrothermal processing parameters. The morphological features and structural properties of TiO₂ films were investigated by field emission scanning electron microscopy, X-ray diffraction, high-resolution transmission electron spectroscopy, Fourier transform Raman spectroscopy, and X-ray photoelectron spectroscopy. The influence of such nanostructures on the performance of dye-sensitized solar cells (DSSCs) is investigated in detail. The interface and transient properties of these nanorods and bottle brush-based photoanodes in DSSCs were analyzed by electrochemical impedance spectroscopic measurements in order to understand the critical factors contributing to such high power conversion efficiency. Surface area of sample was recorded using Brunauer–Emmett–Teller measurements. It is found that bottle brush provides effective large surface area 89.34 m² g^?1 which is much higher than TiO₂ nanorods 63.7 m² g^?1. Such effective surface area can facilitate the effective light harvesting, and hence improves the dye adsorption and the photovoltaic performance of DSSCs, typically in short-circuit photocurrent and power conversion efficiency. A best power conversion efficiency of 6.63 % has been achieved. We believe that the present device performance would have wide interests in dye-sensitized solar cell research.     

Fluorimetric Method Based on Diazotization-Coupling Reaction for Determination of Clenbuterol

A novel fluorimetric method based on diazotization-coupling reaction (DCR) for the determination of clenbuterol is described. In acidic solution, clenbuterol was first diazotized with sodium nitrite, followed by coupling with bisphenol A to produce an azo-compound in NH₃- NH₄Cl buffer. It has found the diazotized clenbuterol- bisphenol A- NH₃- NH₄Cl (DCBN) system has strong fluorescence efficiency compare with the bisphenol A solution. There is a linear relationship between the increased intensity of the fluorescence emission spectra (λ_ex/λ_em?=?276 nm/306 nm) and the concentration of clenbuterol. The effects of the amount of sodium nitrite, diazo reaction time, the amount of bisphenol A, coupling reaction time and coupling reaction temperature have been examined. Under the optional conditions, clenbuterol can be determined over the concentration range of 0.02 to 2.0 μg mL^?1 with a correlation coefficient of 0.9953. The detection limit is 0.01 μg mL^?1 at a signal-to-noise ratio of 3. The relative standard deviation (RSD) for 11 repetitive determinations of 0.9 μg mL^?1 clenbuterol is 0.22 %. The utility of this method was demonstrated by determining clenbuterol in meat samples.     

Enhanced electrocatalytic oxidation of hydroxylamine on Pt/polypyrrole composite modified glassy carbon electrode

A sensitive hydroxylamine sensor is developed by electrodeposition of Pt nanoparticles on pre-synthesized polypyrrole nanoparticles modified glassy carbon electrode. The modified electrode presents distinctly electrocatalytic activity toward hydroxylamine oxidation. The kinetic parameters such as the overall numbers of electrons involved in hydroxylamine oxidation, the electron transfer coefficient, standard heterogeneous rate constant, and diffusion coefficient are evaluated. The current response increases linearly with increasing hydroxylamine concentrations and exhibits two wide linear ranges of 5.0?×?10^?7–1.1?×?10^?3 and 1.1?×?10^?3–18.8?×?10^?3 M with a detection limit of 0.08 μM (s/n?=?3). The proposed electrode presents excellent operational and storage ability for determining hydroxylamine. Moreover, the sensor shows good sensitivity, selectivity, and reproducibility properties.     

Electrochemical methods for determination of thymine in medical pipefish samples based on HPMαFP/Ppy/GCE-modified electrode

A sensitive electrochemical method was developed for the voltammetric determination of thymine at a composite film-modified electrode 1-phenyl-3-methyl-4-(2-furoyl)-5-pyrazolone (HPMαFP)/polypyrrole (Ppy)/glassy carbon electrode (GCE). The electrochemical parameters of thymine were investigated by cyclic voltammetry and differential pulse voltammetry. In pH?=?7.4, one sensitive oxidation peak of thymine with E _pa?=?0.968 V was observed on the HPMαFP/PPy-modified electrode. The difference of peak potential (?E _pa) was 188 mV lower than that for bare GCE. Compared to the bare GCE and Ppy/GCE, the HPMαFP/Ppy/GCE-modified electrode showed an excellent electrocatalytic effect on the oxidation of thymine and displayed a shift of the oxidation potential in the negative direction with significant increase in the peak current. Under the optimum condition, the concentration calibration range and detection limit are 2?×?10^?6–1?×?10^?4 and 4.85?×?10^?7?M for thymine. This developed method had been applied to the direct determination of thymine in medical pipefish samples with satisfactory results.     

Si/polyaniline-based porous carbon composites with an enhanced electrochemical performance as anode materials for Li-ion batteries

Silicon/polyaniline-based porous carbon (Si/PANI-AC) composites have been prepared by a three-step method: coating polyaniline on Si particles using in situ polymerization, carbonizing, and further activating by steam. The morphology and structure of Si/PANI-AC composites have been characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and Raman spectra, respectively. The content and pore structure of the carbon coating layer in Si/PANI-AC have been measured by thermogravimetric analysis and N₂ adsorption-desorption isotherm, respectively. The results indicate some micropores about 1~2 nm in the carbon layer appear during activation and that crystal structure and morphology of Si particles can be retained during preparation. Si/PANI-AC composites exhibit high discharge capacity about 1000 mAh g^?1 at 1.5 A g^?1; moreover, when the current density returns to 0.2 A g^?1, the discharge capacity is still 1692 mAh g^?1 and remains 1453 mAh g^?1 after 70 cycles. The results indicate that the porous carbon coating layer in composites plays an important role in the improvement of the electrochemical performance of pure Si.     

Facile synthesis of porous CuS film as a high efficient counter electrode for quantum-dot-sensitized solar cells

In this paper, porous CuS film has been successfully prepared by a facile method and employed as a counter electrode (CE) in quantum-dot-sensitized solar cells (QDSSCs) for its highest catalytic activity. This CuS thin film was deposited on FTO substrate via spin coating process which is simple to operate, and its electrochemical properties were further studied by EIS and Tafel measurement. With the cycling time of depositing CuS up to 8, it displays high electrocatalytic activity toward polysulfide reduction, rationalizing the improved QDSSCs performance. Using the CdS/CdSe-sensitized QDSSCs, the cells exhibit improved short-circuit photocurrent density (J _sc) and fill factor (FF), achieving solar cell conversion efficiency (η) as high as 5.60 % under AM 1.5 illumination of 100 mW cm^?2. This work provides a novel and simple method for the preparation of CEs, which could be utilized in other metal sulfides CEs for QDSSCs.     

Photocatalytic properties of zinc oxide nanorods grown by different methods

A comparison of photocatalytic properties of ZnO nanostructures fabricated by different methods was carried out. The photocatalytic properties of as grown and Ar-ion-treated ZnO materials were tested using photocatalytic degradation of an aqueous solution of methyl orange dye serving as a model water contaminant. The reaction rate constants of methyl orange photodegradation for untreated ZnO nanorods grown by the method of gas-transport reactions and hydrothermal method were equal to 5.3 × 10^?5 and 3.7 × 10^?4 s^?1, respectively, whereas for the case of the Ar-ion-treated samples they reached 1.85 × 10^?4 and 5.9 × 10^?4 s^?1, respectively. Based on the analysis of the photoluminescence spectra, it is assumed that the difference in photocatalytic activity is connected with different type of defects predominant on the surfaces of ZnO nanorods grown by the hydrothermal and gas-transport reactions methods. The experimental results show that ZnO nanostructures grown by the hydrothermal method would be promising for producing efficient catalysts.     

Study of the electrochemical performance of VO2+/VO2 + redox couple in sulfamic acid for vanadium redox flow battery

The present work was performed in order to evaluate sulfamic acid as the supporting electrolyte for VO²⁺/VO₂ ⁺ redox couple in vanadium redox flow battery. The oxidation process of VO²⁺ has similar electrochemical kinetics compared with the reduction process of VO₂ ⁺. The exchange current density and standard rate constant of VO²⁺/VO₂ ⁺ redox reaction on a graphite electrode in sulfamic acid are determined as 7.6?×?10^?4 A cm^?2 and 7.9?×?10^?5 cm s^?1, respectively. The energy efficiency of the cell employing sulfamic acid as supporting electrolyte in the positive side can reach 75.87 %, which is adequate for redox flow battery applied in energy storage. The addition of NH₄ ⁺ to the positive electrolyte can enhance the electrochemical performance of the cell, with larger discharge capacity and energy efficiency. The preliminary exploration shows that the vanadium sulfamate electrolyte is promising for vanadium redox flow battery and is worthy of further study.     

Photocatalytic activity of 6.5 MeV electron-irradiated ZnO nanorods

The microwave-synthesized zinc-oxide (ZnO) nanonorods of average length of ～ 1500 nm and diameter ～ 100 nm were irradiated with 6.5 meV electrons. From sample to sample, the electron fluence was varied over the range 5×10¹⁴ to 2.5×10¹⁵ e-cm^?2. The pre- and post-electron-irradiated ZnO nanorods were characterized by X-ray diffraction, UV–VIS, EDAX, scanning electron microscopy, transmission electron microscopy, and BET methods. The results show that after electron irradiation, the ZnO nanorods could retain the hexagonal phase with the wurtzite structure; however, the average length of the ZnO nanorods reduced to ～ 800 nm. Moreover, the oxygen atoms from a fraction of ZnO molecules were dislodged, and the process contributed to the formation of Zn–ZnO mixed phase, with increased zinc to oxygen ratio. In the photo-degradation of Rhodamine-B, a significant enhancement in the photocatalytic activity of the electron-irradiated ZnO nanorods was observed. This could be attributed to the induced defects, reduced dimensions, and increased surface area of the ZnO nanorods, in addition to the formation of the Zn–ZnO phase. All these could collectively contribute to the effective separation of the photogenerated electrons from the holes on the ZnO nanorods, and therefore enhance the photocatalytic activity under UV exposure.     

Magnetic ionic liquid-assisted synthesis of polyaniline/AgCl nanocomposites by interface polymerization

A simple strategy for the one-step synthesis of polyaniline/AgCl nanocomposites at the water/magnetic ionic liquid interface was reported. By controlling the reactive conditions, highly dispersed polyaniline/AgCl nanocomposites with their size ranging around 50–80 nm were obtained with magnetic ionic liquid as the oxidant. Transmission electron microscopy was used to show the morphology of the nanocomposites. The nanocomposites were also characterized by Fourier transform infrared spectroscopy, X-ray diffraction, and thermogravimetric analysis. Moreover, polyaniline/AgCl nanocomposites on a glassy carbon electrode showed strong electrocatalytic activity for H₂O₂ and could be used to construct a H₂O₂ biosensor.     

Evaluation of carbon-supported copper phthalocyanine (CuPc/C) as a cathode catalyst for fuel cells using Nafion as an electrolyte

Carbon-supported copper phthalocyanine (CuPc/C) nanoclusters, as a novel suitable cathode catalyst in polymer electrolyte membrane fuel cells, have been synthesized via a combined solvent impregnation and milling procedure along with high-temperature treatment. For optimizing the electrocatalytic activity of the catalyst obtained, the electrode with varying Nafion ionomer contents in the catalyst layer was screened by cyclic voltammetry and linear sweep voltammetry employing a rotating disk electrode technique to investigate the effect of Nafion ionomer as for alkaline electrolyte. For comparative purposes, electrode with various contents of available anion-ionomer was also investigated. The results revealed that the content of Nafion ionomer can affect the oxygen reduction reaction activity of the CuPc/C catalyst and an optimal content of Nafion ionomer was around 3.5?×?10¹?μg?cm^?2, which corresponds well with the electrode prepared using available anion-ionomer. The electrode prepared using Nafion ionomer can produce a comparable performance to that of using available anion-ionomer, giving an onset potential at 0.1 V with a half-wave potential of ?0.03 V. Furthermore, Koutechy–Levich analysis showed that the value of electron transfer number is in the range of 3.40 to 3.74 when using electrode with varying Nafion ionomer contents from 2.5?×?10¹ to 1.6?×?10²?μg?cm^?2. The membrane electrode assembly fabricated with the CuPc/C cathode catalyst with a loading of 3.6 mg?cm^?2 and a Nafion membrane immersed in 3 M KOH for 48 h produced a power density of 3.8 mW?cm^?2 at room temperature.