Sonochemically synthesized MnO2 nanoparticles as electrode material for supercapacitors

In this study, manganese oxide (MnO₂) nanoparticles were synthesized by sonochemical reduction of KMnO₄ using polyethylene glycol (PEG) as a reducing agent as well as structure directing agent under room temperature in short duration of time and characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET) analysis. A supercapacitor device constructed using the ultrasonically-synthesized MnO₂ nanoparticles showed maximum specific capacitance (SC) of 282 Fg⁻¹ in the presence of 1 M Ca(NO₃)₂ as an electrolyte at a current density of 0.5 mA cm⁻² in the potential range from 0.0 to 1.0 V and about 78% of specific capacitance was retained even after 1000 cycles indicating its high electrochemical stability.     

SILAR deposited Bi2S3 thin film towards electrochemical supercapacitor

Bi₂S₃ thin film electrode has been synthesized by simple and low cost successive ionic layer adsorption and reaction (SILAR) method on stainless steel (SS) substrate at room temperature. The formation of interconnected nanoparticles with nanoporous surface morphology has been achieved and which is favourable to the supercapacitor applications. Electrochemical supercapacitive performance of Bi₂S₃ thin film electrode has been performed through cyclic voltammetry, charge-discharge and stability studies in aqueous Na₂SO₄ electrolyte. The Bi₂S₃ thin film electrode exhibits the specific capacitance of 289 Fg⁻¹ at 5 mVs⁻¹ scan rate in 1 M Na₂SO₄ electrolyte.     

Electrochemical supercapacitor studies of hierarchical structured Co2+-substituted SnO2 nanoparticles by a hydrothermal method

Hierarchical structured Co-doped SnO₂ nanoparticles are prepared by a low temperature hydrothermal process. The structural and surface morphologies of the SnO₂ and Sn_1?xCo_xO₂ nanoparticles are studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The Sn_1?xCo_xO₂ nanoparticles form with a tetragonal rutile structure during the hydrothermal process without further calcination. The pseudocapacitance behavior of the Sn_1?xCo_xO₂ nanoparticles is characterized by cyclic voltammetry (CV) in 1.0 M H₂SO₄ electrolyte. The specific capacitance (SC) is found to increase with an increase in cobalt content. A maximum SC of 840 F g^?1 is obtained for a Sn_0.96Co_0.04O₂ composite at a 10 mV s^?1 scan rate.     

Controllable synthesis of rice-shape Alq3 nanoparticles with single crystal structure

We report the controllable growth of rice-shape nanoparticles of Alq₃ by an extremely facile self-assembly approach. Possible mechanisms have been proposed to interpret the formation and controlled process of the single crystal nanoparticles. The field-emission performances (turn-on field 7 V μm⁻¹, maximum current density 2.9 mA cm⁻²) indicate the potential application on miniaturized nano-optoelectronics devices of Alq₃-based. This facile method can potentially be used for the controlled synthesis of other functional complexes and organic nanostructures.     

SnO2-decorated multiwalled carbon nanotubes and Vulcan carbon through a sonochemical approach for supercapacitor applications

Multiwalled carbon nanotubes (MWCNTs) and Vulcan carbon (VC) decorated with SnO₂ nanoparticles were synthesized using a facile and versatile sonochemical procedure. The as-prepared nanocomposites were characterized by means of transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier transform infra red spectroscopy. It was evidenced that SnO₂ nanoparticles were uniformly distributed on both carbon surfaces, tightly decorating the MWCNTs and VC. The electrochemical performance of the nanocomposites was evaluated by cyclic voltammetry and galvanostatic charge/discharge cycling. The as-synthesized SnO₂/MWCNTs nanocomposites show a higher capacity than the SnO₂/VC nanocomposites. Concretely, the SnO₂/MWCNTs electrodes exhibit a specific capacitance of 133.33 F g⁻¹, whereas SnO₂/VC electrodes exhibit a specific capacitance of 112.14 F g⁻¹ measured at 0.5 mA cm⁻² in 1 M Na₂SO₄.     

Electrochemical redox supercapacitors using PVdF-HFP based gel electrolytes and polypyrrole as conducting polymer electrode

Electrochemical redox supercapacitors have been fabricated using polymeric gel electrolytes polyvinylidene fluoride co-hexafluoropropylene (PVdF-HFP)–ethylene carbonate (EC)–propylene carbonate (PC)–MClO₄: M = Li, Na, (C₂H₅)₄N and electrochemically deposited polypyrrole as conducting polymer electrode. The performance of the capacitors have been characterized using a.c impedance spectroscopy, cyclic linear sweep voltammetry and galvanostatic charge–discharge techniques. The capacitors shows larger values of overall capacitance of about 14–25 mF cm^− 2 (equivalent to a single electrode specific capacitance of 78–137 F g^− 1 of polypyrrole), which corresponds to the energy density of 11–19 W h kg^− 1 and power density of 0.22–0.44 kW kg^− 1. The values of capacitance have been found to be almost stable up to 5000 cycles and even more. A comparison indicates that the capacitive behaviour and the capacitance values are not much affected with the size of cations of the salts incorporated in gel electrolytes, rather predominant role of anions is possible at the electrode–electrolyte interfaces. Furthermore the coulombic efficiencies of all the cells were found to be nearly 100% that is comparable to the liquid electrolytes based capacitors.     

High surface area monodispersed Fe3O4 nanoparticles alone and on physical exfoliated graphite for improved supercapacitors

Highly conductive, unsophisticated and easy to be obtained physical exfoliated graphite (PHG) supporting well dispersed magnetite, Fe₃O₄/PHG nanocomposite, has been prepared by a one-step chemical strategy and physico-chemical characterized. The nanocomposite, favoured by the a-polar nanoparticles (NPs) capping, results in a self-assembled monolayer of monodispersed Fe₃O₄, covering perfectly the hydrophobic surfaces of PHG. The nanocomposite as an electrode material was fabricated into a supercapacitor and characterized by cyclic voltammetry (CV) and galvanostatic charge–discharge measurements. It shows, after a suitable annealing, significant electrochemical properties (capacitance value of 787 F/g at 0.5 A g⁻¹ and a Fe₃O₄/PHG weight ratio of 0.31) and good cycling stability (retention 91% after 30,000 cycles). Highly monodispersed very fine Fe₃O₄ NPs, covered by organic chains, have been also synthesized. The high surface area Fe₃O₄ NPs, after washing to leave a low content of organic chains able to avoid aggregation without excessively affecting the electrical properties of the material, exhibit remarkable pseudocapacitive activities, including the highest specific capacitance over reported for Fe₃O₄ (300 F/g at 0.5 A g⁻¹).     

Ultrasonic assisted-Fenton-like degradation of nitrobenzene at neutral pH using nanosized oxides of Fe and Cu

Ultrasonic-assisted heterogeneous Fenton reaction was used for degradation of nitrobenzene (NB) at neutral pH conditions. Nano-sized oxides of α-Fe₂O₃ and CuO were prepared, characterized and tested in degradation of NB (10 mg L⁻¹) under sonication of 20 kHz at 25 °C. Complete degradation of NB was effected at pH 7 in presence of 10 mM H₂O₂ after 10 min of sonication in presence of α-Fe₂O₃ (1.0 g L⁻¹), (k = 0.58 min⁻¹) and after 25 min in case of CuO (k = 0.126 min⁻¹). α-Fe₂O₃ showed also effective degradation under the conditions of 0.1 g L⁻¹ oxide and 5.0 mM of H₂O₂, even though with a lower rate constant (0.346 min⁻¹). Sonication plays a major role in enhancing the production of hydroxyl radicals in presence of solid oxides. Hydroxyl radicals-degradation pathway is suggested and adopted to explain the differences noted in rate constants recorded on using different oxides.     

Cobalt terephthalate MOF-templated synthesis of porous nano-crystalline Co3O4 by the new indirect solid state thermolysis as cathode material of asymmetric supercapacitor

In this work, two different types of Co₃O₄ nano-crystals were synthesized by (i) conventional direct solid state thermolysis of cobalt terephthalate metal-organic framework (MOF-71) and (ii) new indirect solid state thermolysis of Co(OH)₂ derived by alkaline aqueous treatment of MOF-71. The products were then characterized by X-ray diffraction technique (XRD), Fourier transforms infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Reflection electron energy loss spectroscopy (REELS), Brunauer, Emmett, and Teller (BET), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) techniques. By REELS analysis the energy band gap of MOF-71 was determined to be 3.7 eV. Further, electrochemical performance of each Co₃O₄ nanostructure was studied by the cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) in a three-electrode system in KOH electrolyte. An asymmetric supercapacitor was fabricated using indirect Co₃O₄ nanoparticles as cathode and electrochemically reduced graphene oxide as anode, and the electrochemical properties were studied and showed a high energy density of 13.51 Wh kg⁻¹ along with a power density of 9775 W kg⁻¹ and good cycling stability with capacitance retention rate of 85% after 2000 cycles.     

Physical,electrochemical and supercapacitive properties of activated carbon pellets from pre-carbonized rubber wood sawdust by CO2 activation

The physical and electrochemical properties of the activated carbon pellet electrodes have been investigated. Activated carbon pellets were prepared from single step carbonization process of pre-carbonized rubber wood sawdust at a temperature of 800 °C that followed with a CO₂ activation process at temperature in the range of 700–1000 °C. The BET characterization on the sample found that the surface area of the carbon pellet increased with the increasing of the activation temperature. The optimum value was as high as 683.63 m² g⁻¹. The electrical conductivity was also found to increase linearly with the increasing of the activation temperature, namely from 0.0075 S cm⁻¹ to 0.0687 S cm⁻¹ for the activation temperature in the range of 700–1000 °C. The cyclic voltammetry characterization of the samples in aqueous solution of 1 M H₂SO₄ also found that the specific capacitance increased with the increasing of the activation temperature. Typical optimum value was shown by the sample activated at 900 °C with the specific capacitance was as high as 33.74 F g⁻¹ (scan rate 1 mV s⁻¹). The retained ratio was as high as 32.72%. The activated carbon pellet prepared from the rubber wood sawdust may found used in supercapacitor applications.     

Fe3O4/hydroxyapatite/graphene quantum dots as a novel nano-sorbent for preconcentration of copper residue in Thai food ingredients: Optimization of ultrasound-assisted magnetic solid phase extraction

Fe₃O₄/hydroxyapatite/graphene quantum dots (Fe₃O₄/HAP/GQDs) nanocomposite was synthesized and used as a novel magnetic adsorbent. This nanocomposite was characterized using scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and magnetization property. The Fe₃O₄/HAP/GQDs was applied to pre-concentrate copper residues in Thai food ingredients (so-called “Tom Yum Kung”) prior to determination by inductively coupled plasma-atomic emission spectrometry. Based on ultrasound-assisted extraction optimization, various parameters affecting the magnetic solid-phase extraction, such as solution pH, amount of magnetic nanoparticles, adsorption and desorption time, and type of elution solvent and its concentration were evaluated. Under optimal conditions, the linear range was 0.05–1500 ng mL⁻¹ (R² > 0.999), limit of detection was 0.58 ng mL⁻¹, and limit of quantification was 1.94 ng mL⁻¹. The precision, expressed as the relative standard deviation of the calibration curve slope (n = 5), for intra-day and inter-day analyses was 0.87% and 4.47%, respectively. The recovery study of Cu for real samples was ranged between 83.5% and 104.8%. This approach gave the enrichment factor of 39.2, which guarantees trace analysis of Cu residues. Therefore, Fe₃O₄/HAP/GQDs can be a potential and suitable candidate for the pre-concentration and separation of Cu from food samples. It can easily be reused after treatment with deionized water.     

Effects of morphology on photocatalytic performance of Zinc oxide nanostructures synthesized by rapid microwave irradiation methods

In this study, two different chemical solution methods were used to synthesize Zinc oxide nanostructures via a simple and fast microwave assisted method. Afterwards, the photocatalytic performances of the produced ZnO powders were investigated using methylene blue (MB) photodegradation with UV lamp irradiation. The obtained ZnO nanostructures showed spherical and flower-like morphologies. The average crystallite size of the flower-like and spherical nanostructures were determined to be about 55 nm and 28 nm, respectively. X-ray diffraction (XRD), scanning electronic microscopy (SEM), Brunauer–Emmett–Teller (BET), room temperature photoluminescence (RT-PL) and UV–vis analysis were used for characterization of the synthesized ZnO powders. Using BET N₂-adsorption technique, the specific surface area of the flower-like and spherical ZnO nanostructures were found to be 22.9 m²/gr and 98 m²/gr, respectively. Both morphologies show similar band gap values. Finally, our results depict that the efficiency of photocatalytic performance in the Zinc oxide nanostructures with spherical morphology is greater than that found in the flower-like Zinc oxide nanostructures as well as bulk ZnO.     

Optimization of simultaneous ultrasound assisted toxic dyes adsorption conditions from single and multi-components using central composite design: Application of derivative spectrophotometry and evaluation of the kinetics and isotherms

Present study is devoted on the efficient application of Sn (O, S)-NPs -AC for simultaneous sonicated accelerated adsorption of some dyes from single and multi-components systems. Sn (O, S) nanoparticles characterization by FESEM, EDX, EDX mapping and XRD revel its nano size structure with high purity of good crystallinity. Present adsorbent due to its nano spherical shape particles with approximate diameter of 40–60 nm seems to be highly effective in this regard. The effects of five variables viz. pH (3.5–9.5), 0.010–0.028 g of adsorbent and 0.5–6.5 min mixing by sonication is good and practical conditions for well and expected adsorption of MB and CV over concentration range of 3–15 mg L⁻¹. Combination of response surface methodology (RSM) based on central composite design (CCD) and subsequent of analysis of variance (ANOVA) and t-test statistics were used to test the significance of the independent variables and their interactions. Regression analysis reveal that experimental data with high repeatability and efficiency well represented by second-order polynomial model with coefficient of determination value of 0.9988 and 0.9976 for MB and CV, respectively following conditions like pH 8.0, 0.016 g adsorbent, 15 mg L⁻¹ of both dyes 4 min sonication time is proportional with achievement of experimental removal percentage of 99.80% of MB and 99.87% of CV in batch experiment. Evaluation and estimation of adsorption data with Langmuir and Freundlich isotherm well justify the results based on their correlation coefficient and error analysis confirm that Langmuir model is good model with adsorption capacity of 109.17 and 115.34 mg g⁻¹ in single system and 95.69 and 102.99 mg g⁻¹ in binary system for MB and CV, respectively. MB and CV kinetic and rate of adsorption well fitted by pseudo-second order equation both in single and binary systems and experimental results denote more and favorable adsorption of CV than respective value in single system. The pseudo-second-order rate constant k₂ in binary system larger than single system.     

Preparation and electrochemical properties of mesoporous Co3O4 crater-like microspheres as supercapacitor electrode materials

Mesoporous Co₃O₄ microspheres with unique crater-like morphology were obtained by utilizing the mesoporous silica material MCM-41 as a template. The analysis results of N₂ adsorption–desorption measurement indicate that the product has a large Brunauer–Emmett–Teller (BET) surface area of 60 m² g⁻¹ and a narrow pore size distribution centering around 3.7 nm. Its electrochemical properties were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements. The findings reveal that this novel morphology material has a smaller inner resistance of about 0.4 Ω and a higher onset frequency of 550 Hz. This material can provide a high specific capacitance of 102 F g⁻¹ and a large capacity retention of 74% in 500 continuous cycles test at a sweep rate of 3 mV s⁻¹. More significantly, the mass loading of electroactive species can reach as large as 2 mg cm⁻², which is one order of magnitude larger than common amount used.     

Hydrophilic polyaniline nanofibrous architecture using electrosynthesis method for supercapacitor application

An electrosynthesis process of hydrophilic polyaniline nanofiber electrode for electrochemical supercapacitor is described. The TGA–DTA study showed polyaniline thermally stable up to 323 K. Polyaniline nanofibers exhibit amorphous nature as confirmed from XRD study. Smooth interconnected fibers having diameter between 120–125 nm and length typically ranges between 400–500 nm observed from SEM and TEM analysis. Contact angle measurement indicated hydrophilic nature of polyaniline fibers. Optical study revealed the presence of direct band gap with energy 2.52 eV. The Hall effect measurement showed room temperature resistivity ∼3 × 10⁻⁴ Ω cm and Hall mobility 549.35 cm⁻²V⁻¹ s⁻¹_. The supercapacitive performance of nanofibrous polyaniline film tested in 1 M H₂SO₄ electrolyte and showed highest specific capacitance of 861 F g⁻¹ at the voltage scan rate of 10 mV/s.     

Spray pyrolyzed NiO–C nanocomposite as an anode material for the lithium-ion battery with enhanced capacity retention

NiO–C nanocomposite was prepared by a spray pyrolysis method using a mixture of Ni(NO₃)₂ and citric acid solution at 600 °C. The microstructure and morphology of the NiO–C composite were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) mapping, and thermogravimetric analysis (TGA). The results showed that the NiO nanoparticles were surrounded by amorphous carbon. Electrochemical tests demonstrated that the NiO–C nanocomposites exhibited better capacity retention (382 mAh g^− 1 for 50 cycles) than that of pure NiO (141 mAh g^− 1 for 50 cycles), which was also prepared by spray pyrolysis using only Ni(NO₃)₂ as precursor. The enhanced capacity retention can be mainly attributed to the NiO–C composite structure, composed of NiO nanoparticles surrounded by carbon, which can accommodate the volume changes during charge–discharge and improve the electrical conductivity between the NiO nanoparticles.     

Synthesis of TiO2/WO3 nanoparticles via sonochemical approach for the photocatalytic degradation of methylene blue under visible light illumination

Through an ultrasound assisted method, TiO₂/WO₃ nanoparticles were synthesized at room temperature. The XRD pattern of as-prepared TiO₂/WO₃ nanoparticles matches well with that of pure monoclinic WO₃ and rutile TiO₂ nanoparticles. TEM images show that the prepared TiO₂/WO₃ nanoparticles consist of mixed square and hexagonal shape particles about 8–12 nm in diameter. The photocatalytic activity of TiO₂/WO₃ nanoparticles was tested for the degradation of a wastewater containing methylene blue (MB) under visible light illumination. The TiO₂/WO₃ nanoparticles exhibits a higher degradation rate constant (6.72 × 10⁻⁴ s⁻¹) than bare TiO₂ nanoparticles (1.72 × 10⁻⁴ s⁻¹) under similar experimental conditions.     

Sonochemical synthesis,structural, magnetic and grain size dependent electrical properties of NdVO4 nanoparticles

NdVO₄ nanoparticles are successfully synthesized by efficient sonochemical method using two different structural directing agents like CTAB and P123. The phase formation and functional group analysis are carried out using X-ray diffraction (XRD) and fourier transform infra red (FT-IR) spectra, respectively. Using Scherrer equation the calculated grain sizes are 27 nm, 24 nm and 20 nm corresponding to NdVO₄ synthesized by without surfactant, with CTAB and P123, respectively. The TEM images revealed that the shape of NdVO₄ particles is rice-like and rod shaped particles while using CTAB and P123 as surfactants. The growth mechanism of NdVO₄ nanoparticles is elucidated with the aid of TEM analysis. From electrical analysis, the conductivity of NdVO₄ nanoparticles synthesized without surfactant showed a higher conductivity of 5.5703 × 10⁻⁶ S cm⁻¹. The conductivity of the material depends on grain size and increased with increase in grain size due to the grain size effect. The magnetic measurements indicated the paramagnetic behavior of NdVO₄ nanoparticles.     

Template-free solvothermal synthesis of 3D hierarchical nanostructured boehmite assembled by nanosheets

In the absence of template and surfactant, hierarchical nanostructured boehmite was synthesized via a simple solvothermal route using aluminum nitrate as aluminum source and isopropanol–toluene mixture as solvent. The crystal structures, morphologies and textural properties of products were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and N₂ adsorption–desorption technique. The as-obtained hierarchical nanostructures consist of nanosheets keeping Brunauer–Emmett–Teller (BET) specific surface area and pore volume of ca. 264.7 m²/g and 1.2 cm³/g, respectively. The experimental results show that the longer reaction time and the lower reaction temperature are unfavorable to the formation of hierarchical nanostructures. Moreover, the properties of solvent have important influence on the morphology of product. The possible formation mechanism of boehmite hierarchical nanostructures was proposed and discussed.     

Fast and wide-band response infrared detector using porous PZT pyroelectric thick film

Porous lead zirconate titanate (PbZr_0.3Ti_0.7O₃, PZT30/70) thick films and detectors for pyroelectric applications have been fabricated on alumina substrates by screen-printing technology. Low temperature sintering of PZT thick films have been achieved at 850 °C by using Li₂CO₃ and Bi₂O₃ sintering aids. The microstructure of PZT thick film has been investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The dielectric properties were measured using HP 4284 at 1 kHz under 25 °C. The permittivity and loss tangent of the thick films were 94 and 0.017, respectively. Curie temperature of PZT thick film was 425 °C as revealed by dielectric constant temperature measurement. The pyroelectric coefficient was determined to be 0.9 × 10⁻⁸ Ccm⁻² K⁻¹ by dynamic current measurement. Infrared detector sensitive element of dual capacitance was fabricated by laser directly write technology. Detectivity of the detectors were measured using mechanically chopped blackbody radiation. Detectivity ranging from 1.23 × 10⁸ to 1.75 × 10⁸ (cm Hz^1/2 W⁻¹) was derived at frequency range from 175.5 Hz to 1367 Hz, and D^*’s −3 dB cut-off frequency bandwidth was 1.2 kHz. The results indicate that the infrared detectors based on porous thick films have great potential applications in fast and wide-band frequency response conditions.