One-step hydrothermal synthesis of marigold flower-like nanostructured MoS<Subscript>2</Subscript> as a counter electrode for dye-sensitized solar cells

MoS₂ thin films with marigold flower-like nanostructures were grown on conductive fluorine-doped tin oxide (FTO) substrates through a one-step hydrothermal synthesis for their application as counter electrodes (CEs) in dye-sensitized solar cells (DSSCs). Different MoS₂ thin film samples (A–D) were grown on FTO slides using different concentrations of precursors (sodium molybdate and thioacetamide), while keeping the Mo/S molar ratio constant (1:4.6), in all samples. The effect of varying precursor concentrations (3.2–12.6 mM on MoS₂ basis) on the structure of the nanostructured thin films and their performance as DSSC-CEs was investigated. Scanning electron microscopy revealed a material with an infolded petal-like morphology. With increasing precursor concentration, the petal-like structures tended to form bunched nanostructures (100–300 nm) resembling marigold flowers. X-ray diffraction analysis, X-ray photoelectron, and Raman spectroscopy studies showed that the thin films were composed of hexagonal MoS₂ with good crystallinity. Hall effect measurements revealed MoS₂ to be a p-type semiconductor with a carrier mobility of 219.80 cm² V^?1 s^?1 at room temperature. The electrochemical properties of the thin films were examined using cyclic voltammetry and electrochemical impedance spectroscopy. The marigold flower-like MoS₂ thin films showed excellent electrocatalytic activity towards the I¯/I₃¯ reaction and low charge transfer resistance (R_ct) values of 14.77 Ω cm^?1, which was close to that of Pt electrode (12.30 Ω cm^?1). The maximum power conversion efficiency obtained with MoS₂ CE-based DSSCs was 6.32%, which was comparable to a Pt CE-based DSSC (6.38%) under one sun illumination. Similarly, the maximum incident photon-to-charge carrier efficiency exhibited by MoS₂ CE-based DSSCs was 65.84%, which was also comparable to a Pt CE-based DSSC (68.38%). The study demonstrated that the marigold flower-like nanostructured MoS₂ films are a promising alternative to the conventional Pt-based CEs in DSSCs.

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Carbon ceramic electrodes modified with mixed oxides SiO<Subscript>2</Subscript>/SnO<Subscript>2</Subscript> for determination of levofloxacin

The preparation of a carbon ceramic electrode modified with SnO₂ (CCE/SnO₂) using tin dibutyl diacetate as precursor was optimized by a 2³ factorial design. The factors analyzed were catalyst (HCl), graphite/organic precursor ratio, and inorganic precursor (dibutyltin diacetate). The statistical treatment of the data showed that only the second-order interaction effect, catalyst × inorganic precursor, was significant at 95% confidence level, for the electrochemical response of the system. The obtained material was characterized by scanning electron microscopy (MEV), X-ray diffraction (XRD), RAMAN spectroscopy, XPS spectra, and voltammetric techniques. From the XPS spectra, it was confirmed the formation of the Si–O–Sn bond by the shift in the binding energy values referred to Sn 3d3/2 due to the interaction of Sn with SiOH species. The incorporation of SnO₂ provided an increment of the electrode response for levofloxacin, with Ipa = 147.0 μA for the ECC and Ipa = 228.8 μA for ECC/SnO₂, indicating that SnO₂ when incorporated into the silica network enhances the electron transfer process. Under the optimized working conditions, the peak current increased linearly with the levofloxacin concentration in the range from 6.21×10^?5 to 6.97×10^?4 mol L^?1 with quantification and detection limits of 3.80×10^?5 mol L^?1 (14.07 mg L^?1) and 1.13×10^?5 mol L^?1 (4.18 mg L^?1), respectively.     

Hydrothermally synthesized Ni(OH)<Subscript>2</Subscript>@Zn(OH)<Subscript>2</Subscript> composite with enhanced electrochemical performance for supercapacitors

Two kinds of electrode materials Ni(OH)₂ and Ni(OH)₂@Zn(OH)₂ composite are fabricated on nickel foam. Electrochemical experiments indicate Ni(OH)₂@Zn(OH)₂ composite deserves further study due to high specific capacitance and good cycle stability, so that it can achieve energy storage and conversion as much as possible. When the hydrothermal time is different, the electrochemical performance of the sample is also different. Accurately, samples can obtain better electrochemical performance at 15 h, and the maximum specific capacitance of Ni(OH)₂@Zn(OH)₂ is 7.87 F cm^?2 compared to Ni(OH)₂ (0.61 F cm^?2) at 5 mA cm^?2. Even at 50 mA cm^?2, specific capacitance is 5.24 F cm^?2 and rate capability is 66.6%. Furthermore, Ni(OH)₂@Zn(OH)₂-15 h loses 19.8% after 1000 cycles, revealing the composite has an outstanding stable cycle. These properties also indicate Ni(OH)₂@Zn(OH)₂-15 h is a promising electrode material.     

Sr,Zn co-doped TiO<Subscript>2</Subscript> xerogel film made of uniform spheres for high-performance dye-sensitized solar cells

This study comes up with the facile preparation of Sr,Zn co-doped TiO₂ xerogel film for boosting the short circuit current density of dye-sensitized solar cells (DSCs). The film contains 2.5-μm-diameter spheres assembled from 60 nm nanoparticles. X-ray photoelectron spectroscopy (XPS) shows that Sr²⁺ and Zn²⁺ ions to be well incorporated into the TiO₂ crystal lattice without forming specific strontium and zinc compositions. The crystallite size, phase composition, and band structure of the spheres depend on the dopants concentration. Isolated energy levels near valence band as a result of the foreign ions introduction improve the photocatalytic activity of the prepared TiO₂ spheres, enhancing the short circuit current density of the cells. The DSC co-doped with 0.075 at.% Sr and 0.4 at.% Zn showed the highest power conversion efficiency of 7.87 % and short circuit current density of 18.75 mA cm^?2 thanks to lower charge transfer resistance (2.16 Ω cm²), lower electron transit time (1.19 ms), and higher electron diffusion coefficient (18.1 × 10⁴ cm² S^?1) compared to the other cells, demonstrated by electrochemical impedance spectroscopy (EIS). The concept of the simultaneous introduction of alkaline earth ions and transition ions into TiO₂ xerogel films will open up a new insight into the fabrication of high performance DSCs.     

Synthesis,Characterization and Photocatalytic Application of TiO<Subscript>2</Subscript>/SnO<Subscript>2</Subscript> Nanocomposite Obtained Under Non-thermal Plasma Condition at Atmospheric Pressure

A plasma-assisted synthesis of TiO₂/SnO₂ nanocomposite is described. In this approach, a precursor containing a mixture of [TiCl₃ and SnCl₂] exposed to electric discharge was oxidized by plasma-generated reactive species (HO^·/H₂O = 2.85 eV/SHE). SnO₂ microstructures with a diameter of 10–40 µm were coated by thin layers TiO₂ nanorods with mean diameter of 6–8 nm. The obtained TiO₂/SnO₂ nanocomposite was characterized by transmission and scanning electron microscopy, X-ray diffraction and Fourier transform infrared. TiO₂/SnO₂ nanocomposite was found to be a promising new material for the photocatalytic discoloration of aqueous Remazol Brilliant Blue-R dye under daylight and UVA light sources, due to the combined effects of large specific surface area and heterojunction which efficiently separates the electron–hole pairs delaying the charge recombination. The leaching test indicated that the nanocomposite is stable easily reusable.     

Electrochemical performance of novel Li<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> glass-ceramic nanocomposites as electrodes for energy storage devices

The novel Li₃V₂(PO₄)₃ glass-ceramic nanocomposites were synthesized and investigated as electrodes for energy storage devices. They were fabricated by heat treatment (HT) of 37.5Li₂O–25V₂O₅–37.5P₂O₅?mol% glass at 450 °C for different times in the air. XRD, SEM, and electrochemical methods were used to study the effect of HT time on the nanostructure and electrochemical performance for Li₃V₂(PO₄)₃ glass-ceramic nanocomposites electrodes. XRD patterns showed forming Li₃V₂(PO₄)₃ NASICON type with monoclinic structure. The crystalline sizes were found to be in the range of 32–56 nm. SEM morphologies exhibited non-uniform grains and changed with variation of HT time. The electrochemical performance of Li₃V₂(PO₄)₃ glass-ceramic nanocomposites was investigated by using galvanostatic charge/discharge methods, cyclic voltammetry, and electrochemical impedance spectroscopy in 1 M H₂SO₄ aqueous electrolyte. The glass-ceramic nanocomposites annealed for 4 h, which had a lower crystalline size, exhibited the best electrochemical performance with a specific capacity of 116.4 F g^?1 at 0.5 A g^?1. Small crystalline size supported the lithium ion mobility in the electrode by decreasing the ion diffusion pathway. Therefore, the Li₃V₂(PO₄)₃ glass-ceramic nanocomposites can be promising candidates for large-scale industrial applications in high-performance energy storage devices.     

Reactor neutrons irradiation effect on the photocatalytic activity of SnO<Subscript>2</Subscript> thin films

SnO₂ thin films synthesized by sol-gel are irradiated with reactor neutrons up to fast neutron fluence of 9.6 × 10¹⁷ neutrons cm^–2 at 40°C. The influence of defects generated by neutrons irradiation, through the properties modification, on the photo-catalytic activity of SnO₂ films is investigated. It is found that the photoactivity of the irradiated films is enhanced after reactor neutrons irradiation. An improvement of 41% is observed for the sample irradiated at a neutron fluence of 9.6 × 10¹⁷ neutrons cm^–2. This is attributed to several parameters modified by the reactor neutron irradiation principally the crystallite size and space charge region which are closely related to the photocatalytic performance.     

Effect of crystallization route on the properties of LiMn2O4 thin films prepared by spin coating

LiMn₂O₄ thin films were prepared by spin coating through intermediate amorphous layer route (IALR) and intermediate crystallized layer route (ICLR). The phase identification, surface morphology, and electrochemical properties of the films prepared by different crystallization routes were studied by X-ray diffraction, scanning electron microscopy, and galvanostatic charge–discharge experiments. The results show that both films prepared by different crystallization routes are homogeneous and crack free. Compared with the film prepared by IALR, the film prepared by ICLR shows smaller grain size and is smoother and denser. The LiMn₂O₄ film prepared by ICLR delivers the specific capacity of 39.8 μAh?cm^?2?μm^?1, which is higher than 35.6 μAh?cm^?2?μm^?1 for the one prepared by IALR. The capacity loss of the film prepared by ICLR after being cycled 100 times is 3.4 %, which is smaller than that of 5.5 % for the film prepared by IALR. The film prepared by ICLR shows higher specific capacity and better cycling behavior than the one prepared by IALR.     

Effects of deposition temperature and annealing temperature on the morphology and electrochemical capacitance of Ni(OH)2 thin films

In this paper, we report 3D nickel (II) hydroxide thin films with porous nanostructures prepared on Ni foam by direct current electrodeposition from aqueous solution of Ni(NO₃)₂ through basic chemicals. The effect of deposition temperature on Ni(OH)₂ thin film morphology is examined by field emission scanning electron microscopy, which is found to have significant influence on capacitance performance of Ni(OH)₂ thin films. Moreover, the effect of annealing temperature on electrochemical capacitance and long-time stability of Ni(OH)₂ thin films is investigated. An optimum-specific capacitance value of 2,447?farads?g^?1 is obtained for Ni(OH)₂ thin film deposited at 20?°C and annealed at 100?°C.     

Nanofibers of V<Subscript>2</Subscript>O<Subscript>5</Subscript>/C@MWCNTs as the cathode material for lithium-ion batteries

Vanadium pentoxide (V₂O₅) nanofibers (NFs) with a thin carbon layer of 3–5 nm, which wrapped on V₂O₅ nanoparticles, and integrated multiwalled carbon nanotubes (MWCNTs) have been fabricated via simple electrospinning followed by carbonization process and post-sintering treatment. The obtained composite displays a NF structure with V₂O₅ nanoparticles connected to each other, and good electrochemical performance: delivering initial capacity of 320 mAh g^?1 (between 2.0 and 4.0 V vs. Li/Li⁺), good cycling stability (223 mAh g^?1 after 50 cycles), and good rate performance (~?150 mAh g^?1 at 2 A g^?1). This can attribute to the carbon wrapped on the V₂O₅ nanoparticles which can not only enhance the electric conductivity to decrease the impendence of the cathode materials but also maintain the structural stability to protect the nanostructure from the corruption of electrolyte and the strain stress due to the Li-ion intercalation/deintercalation during the charge/discharge process. And, the added MWCNTs play the role of framework of the unique V₂O₅ coated by carbon layer and composited with MWCNT NFs (V₂O₅/C@MWCNT NFs) to ensure the material is more stable.     

SnO2 sheet/graphite composite as anode material with improved electrochemical performance for lithium-ion batteries

The SnO₂ sheet/graphite composite was synthesized by a hydrothermal method for high-capacity lithium storage. The microstructures of products were characterized by XRD and FE-SEM. The electrochemical performance of SnO₂ sheet/graphite composite was measured by galvanostatic charge/discharge cycling and EIS. The first discharge and charge capacities are 1,072 and 735 mAh g^?1 with coulombic efficiency of 68.6 %. After 40 cycles, the reversible discharge capacity is still maintained at 477 mAh g^?1. The results show that the SnO₂ sheet/graphite composite displays superior Li-battery performance with large reversible capacity and good cyclic performance.     

EQCM study of redox properties of PEDOT/MnO<Subscript>2</Subscript> composite films in aqueous electrolytes

Electrochemical behavior of poly-3,4-ethylenedioxythiophene composites with manganese dioxide (PEDOT/MnO₂) has been investigated by cyclic voltammetry and electrochemical quartz crystal microbalance at various component ratios and in different electrolyte solutions. The electrochemical formation of PEDOT film on the electrode surface and PEDOT/MnO₂ composite film during the electrochemical deposition of manganese dioxide into the polymer matrix was gravimetrically monitored. The mass of manganese dioxide deposited into PEDOT at different time of electrodeposition and apparent molar mass values of species involved into mass transfer during redox cycling of PEDOT/MnO₂ composites were evaluated. It was found that during the redox cycling of PEDOT/MnO₂ composite films with various MnO₂ content, the oppositely directed fluxes of counterions (anions and cations) occur, resulting in a change of the slope of linear parts of the Δf–E plots with changing the mass fraction of MnO₂ in the composite film.Rectangular shape of cyclic voltammograms of PEDOT/MnO₂ composites with different loadings of manganese dioxide was observed, which is characteristic of the pseudocapacitive behavior of the composite material. Specific capacity values of PEDOT/MnO₂ composites obtained from cyclic voltammograms were about 169 F g^?1. The specific capacity, related to the contribution of manganese dioxide component, was about 240 F g^?1.     

Kinetics of electrochromic process in thin films of cathodically deposited nickel hydroxide

Ni(OH)₂ films have been obtained by cathodic deposition from 1 M Ni(NO₃)₂ on a glass with a current-conducting SnO₂ layer. The films have a porous structure and consist of chaotically joined formations of 100–150 nm in size. They contain a considerable amount of adsorbed water, because of which their refraction index was n?=?~1.5, whereas for crystalline nickel hydroxide, it was n?=?2.37. It has been shown that in the course of discoloration of films through a shift of their potential towards more negative values, an electric field is formed in the bulk of film, which accelerates the entry of cations into it (protons as [H₃O]⁺) from the electrolyte and electrons from ohmic contact. In this case, the initial dependence i(t), where i?~?t ^?1/4, is bound up with gradual increase in proton surface concentration. It is proposed to determine separately the dependence of the effective codiffusion coefficient of charge carriers (protons and electrons) on decoloration potential by the analysis of plots of current, injected charge, and luminous transmittance of films against time. This procedure involves a series of periodic stops of potential during the recording of current–potential curves for an electrochromic electrode and allows one to monitor the ratio of the film forms NiOOH and Ni(OH)₂ in the course of film reduction.     

Simple chemical route for nanorod-like cobalt oxide films for electrochemical energy storage applications

We used a simple chemical synthesis route to deposit nanorod-like cobalt oxide thin films on different substrates such as stainless steel (ss), indium tin oxide (ITO), and microscopic glass slides. The morphology of the films show that the films were uniformly spread having a nanorod-like structure with the length of the nanorods shortened on ss substrates. The electrochemical properties of the films deposited at different time intervals were studied using cyclic voltammetry (CV), galvanostatic charge–discharge (GCD), and electrochemical impedance spectroscopy (EIS). The film deposited after 20 cycles on ss gave the highest specific capacity of 67.6 mAh g^?1 and volumetric capacity of 123 mAh cm^?3 at a scan rate 5 mV s^?1 in comparison to 62.0 mAh g^?1 and 113 mAh cm^?3 obtained, respectively, for its counterpart on ITO. The film electrode deposited after 20 cycles on ITO gave the best rate capability and excellent cyclability with no depreciation after 2000 charge–discharge cycles.     

Electrodeposited Ni(OH)<Subscript>2</Subscript> nanostructures on electro-etched carbon fiber paper for highly stable supercapacitors

Herein, we introduce a facile, inexpensive and fast, and additive-/template-free method to fabricate highly stable nickel hydroxide nanofibers for supercapacitor applications. Ni(OH)₂ nanofibers were electrodeposited on electro-etched carbon fiber paper by a potential step method (Ni(OH)₂-ECFs) and characterized using scanning electron microscopy and X-ray diffraction analysis. Electrochemical performance of Ni(OH)₂-ECF was studied in symmetric two-electrode assembly by cyclic voltammetry, galvanostatic charge–discharge method, and electrochemical impedance spectroscopy. A specific capacitance of 277.5 F g^?1 was achieved for the symmetric supercapacitor based on two identical Ni(OH)₂-ECFs. Our findings demonstrate high-rate capability with excellent stability (approximately 100 % capacitance retention) for Ni(OH)₂-ECF supercapacitor, originated from the intimate contact between Ni(OH)₂ and ECF. Our studies suggest the Ni(OH)₂-ECF electrode as an excellent material for supercapacitor applications.     

Concurrent synthesis of SnO/SnO<Subscript>2</Subscript> nanocomposites and their enhanced photocatalytic activity

The SnO/SnO₂ nanocomposites were synthesized using semisolvothermal reaction technique. These nanocomposites were prepared using different combination of solvents viz., ethanol, water, and ethylene glycol at 180 °C for 24 h. The synthesized nanocomposites were analyzed with various characterization techniques. Structural analysis indicates the formation of tetragonal phase of SnO₂ for the sample prepared in ethanol, whereas for other solvent combinations, the mixture of SnO and SnO₂ having tetragonal crystal structures were observed. The optical study shows enhanced absorbance in the visible region for all the prepared SnO/SnO₂ nanocomposites. The observed band gap was found to be in the range of 3.0 to 3.25 eV. Microstructural determinations confirm the formation of nanostructures having spherical as well as rod-like morphology. The size of nanoparticles in ethanol-mediated solvent was found to be in the range of 5 to 7 nm. Thermogravimetric analysis indicate the weight gain around 1.3 wt% confirming the conversion of SnO to SnO₂ material. The photocatalytic activity of synthesized nanocomposites was evaluated by following the aqueous methylene blue (MB) degradation. The sample prepared in ethylene glycol-mediated solvent showed highest photoactivity having apparent rate constant (K_app) 0.62 × 10^?2 min^?1.     

Heterostructured CoO/3D-TiO<Subscript>2</Subscript> nanorod arrays for photoelectrochemical water splitting hydrogen production

Homogeneous p-type cobalt (II) oxide (CoO) nanoparticles were successfully deposited on n-type three-dimensional branched TiO₂ nanorod arrays (3D-TiO₂) through photochemical deposition and thermal decomposition to form a novel CoO/3D-TiO₂ p-n heterojunction nanocomposite. Due to the narrow band gap of CoO nanoparticles (~2.4 eV), the as-synthesized CoO/3D-TiO₂ exhibited an excellent visible light absorption. The amounts of deposited CoO nanoparticles obviously influence the hydrogen production rate in the photoelectrochemical (PEC) water splitting. The as-synthesized CoO/3D-TiO₂-5 obtains the highest PEC hydrogen production rate of 0.54 mL h^?1 cm^?2 after five-time CoO deposition cycles (at a potential of 0.0 V vs Ag/AgCl). The photocurrent density of CoO/3D-TiO₂-5 is 1.68 mA cm^?1, which is ca. 2.5 times greater than that of pure 3D-TiO₂. The results showed that the formation of internal electrical-field between the CoO/3D-TiO₂ heterojunction, which has a direction from n-type TiO₂ to p-type CoO, facilitated the charge separation and transfer and resulted in a high efficiency and stable PEC activity.     

Conductivity of SnO<Subscript>2</Subscript>-In<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocrystalline composite films

The conductivity of films consisting of a mixture of SnO₂ and In₂O₃ nanocrystals at 200–500°C was studied. Based on the experimental data, it was assumed that in films containing less than 20 wt % In₂O₃, the current flows along SnO₂ nanocrystals. A model of conductivity in these films is presented; it includes an electron transfer from In₂O₃ to SnO₂, which forms positively charged In₂O₃ nanocrystals that contact the negatively charged SnO₂ nanocrystals. In the presence of In₂O₃ nanocrystals, the activation energy of the electron transfer between SnO₂ nanocrystals decreased substantially because of a decrease in the barrier of electron transfer between SnO₂ crystals under the action of the negative charge. As a result, a percolation cluster of charged SnO₂ crystals formed. At high contents of In₂O₃ (over 20 wt %), the conductivity increased dramatically. The curve of the temperature dependence of conductivity changed because of the appearance of a percolation cluster of In₂O₃ nanocrystals, in which the current passed. The conductivity of a mixed film of this kind differed from that of the nanocrystalline film of pure In₂O₃.     

Fabrication of amperometric cholesterol biosensor based on SnO<Subscript>2</Subscript> nanoparticles and Nafion-modified carbon paste electrode

This study reports the fabrication of an amperometric cholesterol biosensor based on cholesterol oxidase (ChOx), SnO₂NPs and Nafion-modified carbon paste enzyme electrodes (CPE/SnO₂NPs-ChOx/Naf). The electrochemical characterisations of BCPE and CPE/SnO₂NPs were performed using CV and EIS. The determination of cholesterol was carried out by electrochemical oxidation of H₂O₂ at 0.6 V vs. Ag/AgCl. The CPE/SnO₂NPs-ChOx/Naf presented a linear range from 0.20 μ.mol L^?1 to 4.95 μmol L^?1 with a low limit of detection (0.04 μ.mol L^?1). In addition, the optimal values for pH and temperature were found to be 7.5 and 35°C, respectively. The CPE/SnO₂NPs-ChOx/Naf was used for the determination of cholesterol in serum samples and good results were obtained.     

Magnetic,optical and electrical properties of Mn-doped CuCrO<Subscript>2</Subscript> thin films prepared by chemical solution deposition method

CuCrO₂ and CuCrO₂:Mn thin films were prepared on sapphire substrates by chemical solution deposition method. The effects of the annealing temperatures and Mn concentration on the structural, electrical and optical properties were investigated. The X-ray diffraction measurement was used to confirm the c-axis orientation of CuCrO₂ and CuCrO₂:Mn thin films. The maximum transmittances of the films in the visible region are about 65% with direct band gaps of 3.25 eV. All films showed the p-type conduction and semiconductor behavior. The electrical conductivity decreases rapidly with the increase of Mn content, the maximum of the electrical conductivity of 1.35 × 10⁻² S cm⁻¹ is CuCrO₂ film deposited at 600 °C temperature in 10⁻³ Torr vacuum, which is about four orders of magnitude higher than that of the Mn-doped CuCrO₂ thin film. The energy band of the samples is constructed based on the grain-boundary scattering in order to investigate the conduction mechanism. Moreover, the samples exhibit a clear ferromagnetism, which was likely ascribed to originating from the double-exchange interaction between the Mn³⁺ and Cr³⁺ ions.