Importance of poly(ethylene glycol) conformation for the synthesis of silver nanoparticles in aqueous solution

Silver nanoparticles (NPs) were prepared using silver nitrate (AgNO₃) as a precursor in an aqueous solution of poly(ethylene glycol) (PEG), which acted as both a reducing and stabilizing agent. The UV/Vis spectra showed that PEG 100 (100 kg/mol) has a remarkable capability to produce silver NPs at 80 °C, but the production of silver NPs by both PEG 2 (2 kg/mol) and PEG 35 (35 kg/mol) was negligible. This difference was explained by the conformation of PEG in the reaction solution: the entangled conformation for PEG 100 and the single-coiled conformation for PEG 2 and PEG 35, which were confirmed by pulse-field-gradient ¹H NMR and viscosity measurements. In an aqueous solution, the entangled conformation of PEG 100 facilitated the reduction reaction by caging silver ions and effectively prevented the agglomeration of formed NPs. The reaction in an aqueous PEG 100 solution was observed to be stable under the conditions of a prolonged reaction time or an increased temperature, while no reduction reaction occurred in the PEG 2 solution. The synthesis of silver NPs by PEG 100 was well controlled to produce fine silver NPs with 3.68 ± 1.03 nm in diameter, the size of which remained relatively constant throughout the reaction.     

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.     

Morphology and size dependence of silver microstructures in fatty salts-assisted multiphoton photoreduction microfabrication

The morphology and size dependence of silver microstructures in a novel microfabrication process, fatty salts-assisted multiphoton photoreduction (MPR), were investigated by using the fatty salts with different carbon chain lengths (C _n : n=4,5,7,9) under varied powers and irradiation times of a femtosecond near-infrared laser with the wavelength of 800 nm. Not only the feature size of the silver structures was reduced but also the surface smoothness was improved by increasing the chain length of the fatty salts. The highest resolution of a silver line was obtained to be 285 nm, which exceeded the diffraction limit. The fatty salts-assisted MPR microfabrication approach would provide an efficient protocol for fabricating metallic micro/nanostructures with fine morphology and size and could play an important role in the fabrication of the metallic micro/nanostructures for applications in photonics and electronics as well as in sensors.     

Sonochemical synthesis of silver nanorods by reduction of sliver nitrate in aqueous solution

The sonochemical synthesis of sliver nanorods has been achieved by ultrasonic irradiation of the aqueous solution of sliver nitrate, methenamine (HMTA) and poly (vinyl pyrrolidone) (PVP) for 60 min. The silver nanorods obtained have lengths of 4–7 μm and mean diameters of about 100 nm. The structures of the samples were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), selected area electron diffraction (SAED) and X-ray powder diffraction (XRD), and the chemical composition of the sample was examined by energy-dispersive X-ray spectrum (EDS). The effects of the irradiation time, the concentration of PVP and the reaction temperature on the morphology of silver nanorods were discussed, and the mechanism of the silver nanorods formation was tentatively inferred.     

Shape-dependent plasmon resonances of Ag nanostructures

Different silver nanostructures have been rapidly synthesized under microwave irradiation from a solution of silver nitrate (AgNO₃) and β$\beta$-D glucose; neither additional reducing nor capping agent were required in this soft green solution approach. Not only spherical nanoparticles, but also necklace and wires have been synthesized. The plasmon resonances of the synthesized silver nanostructures were tuned by varying the irradiation time and hence by changing size and morphology of nanostructures. The obtained nanostructures were characterized by X-Ray diffraction (XRD), Uv–Vis spectroscopy (Uv–Vis), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). The change of peak position and the shape of the absorption spectra were clearly observed during the whole reaction process; in fact, it was evidenced that initially Ag nanoparticles were formed, which, as reaction time elapsed, self-assembled and fused with each other to yield nanowires.     

Self-assembled 3D La(OH)3 and La2O3 nanostructures: Fast microwave synthesis and characterization

Self-assembled three-dimensional (3D) urchin-like and flower-like La(OH)₃ nanostructures were successfully prepared for the first time via a facile and fast microwave-assisted solution-phase chemical method in 15 min. The obtained products were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The SEM results reveal that the urchin-like and flower-like La(OH)₃ nanostructures are ca. 3 μm and 6 μm in diameter, respectively. The urchin-like La(OH)₃ nanostructures are constructed by nanorods with diameters of about 300 nm and lengths of about 500 nm. The flower-like La(OH)₃ nanostructures are built from nanopetals about 100 nm thick. The effects of reaction time, microwave power, amount of tetraethyl ammonium bromide (TEAB), and surfactants on the preparation were systematically investigated. The possible formation mechanism of the 3D La(OH)₃ nanostructures was preliminarily discussed. Urchin-like and flower-like La₂O₃ nanostructures were obtained after calcining the La(OH)₃ nanostructures at 800 °C for 4 h. Urchin-like and flower-like La₂O₃:Eu³⁺ nanostructures were also prepared and their photoluminescence (PL) properties were investigated.     

Self-assembly of boehmite nanopetals to form 3D high surface area nanoarchitectures

A flower-like boehmite nanostructure was prepared through a template-free chemical route by the self-assembly process of nanosize petals 800–1000 nm long, 200–250 nm wide, 20–50 nm thick and having an average crystallite size of about 2.21 nm. X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), DTA/TGA analyses and Brunauer–Emmet–Teller (BET-N₂) analyses were used in order to characterize the product obtained. XRD results exhibited that the obtained nanostructures composed of pure orthorhombic AlOOH phase. The effects of Cl⁻ ions and TEA on the growth of boehmite three-dimensional nanoarchitectures in the presence of NO₃^-\mathrm{NO}_{3}^{-} ions were investigated. BET analyses of as-prepared material demonstrate that this nanostructure material has a high specific surface area, as high as 123 m² g⁻¹.     

Syntheses and characterization of Sr(OH)2 and SrCO3 nanostructures by ultrasonic method

The Sr(OH)₂ and SrCO₃ nanostructures were synthesized by reaction of strontium(II) acetate and sodium hydroxide or tetramethylammonium hydroxide (TMAH) via ultrasonic method. Reaction conditions, such as the concentration of the Sr²⁺ ion, aging time, power of the ultrasonic device and alkali salts show important roles in the size, morphology and growth process of the final products. The pure crystalline SrCO₃ were obtained by heating of product at 400 °C. The Sr(OH)₂ and SrCO₃ nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), thermal gravimetric (TG), differential thermal analyses (DTA) and the infrared spectroscopy (IR).     

Morphologically controlled preparation of CuO nanostructures under ultrasound irradiation and their evaluation as pseudocapacitor materials

Various morphologies of copper oxide (CuO) nanostructures have been synthesized by controlling the reaction parameters in a sonochemical assisted method without using any templates or surfactants. The effect of reaction parameters including molar ratio of the reactants, reaction temperature, ultrasound exposure time, and annealing temperature on the composition and morphology of the product(s) has been investigated. The prepared samples have been characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDAX), and thermogravimetric analysis (TGA). It has been found that Cu₂(OH)₃NO₃ nanoplatelets are achieved in mild conditions which can be then converted to various morphologies of CuO nanostructures by either using high concentrations of OH⁻ (formation of nanorods), prolonging sonication irradiation (nanoparticles), or thermal treatment (nanospheres). Application of the prepared CuO nanostructures was evaluated as supercapacitive material in 1 M Na₂SO₄ solution using cyclic voltammetry (CV) in different potential scan rates ranging from 5 to 100 mV s⁻¹. The specific capacitance has been calculated using CV curves. It has been found that the pseudocapacitor performance of CuO can be tuned via employing morphologically controlled samples. Accordingly, the prolonged sonicated sample (nanoparticles) showed the high specific capacitance of 158 F.g⁻¹.     

Sonochemical synthesis of cobalt aluminate nanoparticles under various preparation parameters

Cobalt aluminate (CoAl₂O₄) nanoparticles were synthesized using a precursor method with the aid of ultrasound irradiation under various preparation parameters. The effects of the preparation parameters, such as the sonochemical reaction time and temperature, precipitation agents, calcination temperature and time on the formation of CoAl₂O₄ were investigated. The precursor on heating yields nanosized CoAl₂O₄ particles and both these nanoparticles and the precursor were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The use of ultrasound irradiation during the homogeneous precipitation of the precursor reduces the duration of the precipitation reaction. The mechanism of the formation of cobalt aluminate was investigated by means of Fourier transformation infrared spectroscopy (FT-IR) and EDX (energy dispersive X-ray). The thermal decomposition process and kinetics of the precursor of nanosized CoAl₂O₄ were investigated by means of differential scanning calorimetry (DSC) and thermogravimetry (TG). The apparent activation energy (E) and the pre-exponential constant (A) were 304.26 kJ/mol and 6.441 × 10¹⁴ s^?1, respectively. Specific surface area was investigated by means of Brunauer Emmett Teller (BET) surface area measurements.     

Enhanced sonocatalytic degradation of organic dyes from aqueous solutions by novel synthesis of mesoporous Fe3O4-graphene/ZnO@SiO2 nanocomposites

Fe₃O₄-graphene/ZnO@mesoporous-SiO₂ (MGZ@SiO₂) nanocomposites was synthesized via a simple one pot hydrothermal method. The as-obtained samples were investigated using various techniques, as follows: scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and specific surface area (BET) vibrating sample magnetometer (VSM), among others. The sonocatalytic activities of the catalysts were tested according to the oxidation for the removal of methylene blue (MB), methyl orange (MO), and rhodamine B (RhB) under ultrasonic irradiation. The optimal conditions including the irradiation time, pH, dye concentration, catalyst dosage, and ultrasonic intensity are 60 min, 11, 50 mg/L, 1.00 g/L, and 40 W/m², respectively. The MGZ@SiO₂ showed the higher enhanced sonocatalytic degradation from among the three dyes; furthermore, the sonocatalytic-degradation mechanism is discussed. This study shows that the MGZ@SiO₂ can be applied as a novel-design catalyst for the removal of organic pollutants from aqueous solutions.     

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.     

Sonochemical synthesis of two nanostructured silver(I) coordination polymers based on semi-rigid bis(benzimidazole) ligands

Nanoparticles of two silver(I) coordination polymers (CPs), [Ag₂(L1)₂(DCTP)]_n (1) and [Ag₂(L2)(DCTP)]_n (2) (L1 = 1,3-bis(5,6-dimethylbenzimidazol-1-ylmethyl)benzene, L2 = 1,4-bis(benzimidazol-1-yl)-2-butene, H₂DCTP = 2,5-dichloroterephthalic acid), were synthesized by the sonochemical approach and hydrothermal method. Both CPs were characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction, scanning electron microscopy (SEM), and thermogravimetric analyses (TGA). CP 1 exhibits a 2D 4-connected sql net with the point symbol {4⁴.6²}. While CP 2 displays a 2D 3,4-connected 3,4L13 net with the point symbol {4.6²}₂{4².6².8²}. The structural diversity indicates that semi-rigid bis(benzimidazole) co-ligands play important roles in tuning the structures of the mixed Ag(I) CPs. The ultrasound irradiation time, temperature, and power showed significant effects on the morphology and growth process of the nanoparticles of two silver(I) CPs. The luminescence and photocatalytic properties of the nanoparticles of CPs 1–2 on the degradation of methyl blue (MB) were also investigated in detail.     

Fabrication and characterization of silver/titanium dioxide composite nanoparticles in ethylene glycol with alkaline solution through sonochemical process

This paper aims to study fabrication and characterization of silver/titanium oxide composite nanoparticle through sonochemical process in the presence of ethylene glycol with alkaline solution. By using ultrasonic irradiation of a mixture of silver nitrate, the dispersed TiO₂ nanoparticle in ethylene glycol associated with aqueous solution of sodium oxide yields Ag/TiO₂ composite nanoparticle with shell/core-type geometry. The powder X-ray diffraction (XRD) of the Ag/TiO₂ composites showed additional diffraction peaks corresponding to the face-centered cubic (fcc) structure of silver crystallization phase, apart from the signals from the cores of TiO₂. Transmission electron microscopy (TEM) images of Ag/TiO₂ composites, which average particle size is roughly 80 nm, reveal that the titanium oxide coated by Ag nanoparticle with a grain size of about 2–5 nm. Additionally, the formation of silver nanoparticles on TiO₂ was monitored by ultraviolet visible light spectrophotometer (UV–Vis). As measured the optical absorption spectra of as-synthesized Ag nanoparticle varying with time, the mechanism of surface formatting silver shell on the cores of TiO₂ could be explored by autocatalytic reaction; the conversion of Ag particle from silver ion is 98% for the reaction time of 1000 s; and the activity energy of synthesizing Ag nanoparticles on TiO₂ is 40 kJ/mol at temperature ranging from 5 to 25 °C. Hopefully, this preliminary investigation could be used for mass production of composite nanoparticles assisted by ultrasonic chemistry in the future.     

The synthesis and kinetic growth of anisotropic silver particles loaded on TiO2 surface by photoelectrochemical reduction method

Silver nanorods with average diameters of 120-230 nm and aspect ratio of 1.7-5.0 were deposited on the surface of TiO₂ films by photoelectrochemical reduction of Ag⁺ to Ag under UV light. The composite films prepared on soda-lime glass substrates were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and atomic force microscopy (AFM). The results show that the TiO₂ film after UV irradiation in AgNO₃ solution is composed of anatase phase TiO₂ and metallic silver with face centered cubic structure. Other compounds cannot be found in the final films. The maximum deposition content of silver particles on the surface of TiO₂ film was obtained with the AgNO₃ concentration of 0.1 M. The kinetic growth rates of silver particles can be controlled by photocatalytic activity of TiO₂ films. The studies suggest that the growth rates of silver particles increase with the enhancement of photocatalytic activity of TiO₂ films. The maximum growth rate of silver particles loaded on TiO₂ films can be up to 0.353 nm min⁻¹ among samples 1#, 2# and 3#, while the corresponding apparent rate constant of TiO₂ is 1.751 × 10⁻³ min⁻¹.     

Sonochemical growth of antimony sulfoiodide in multiwalled carbon nanotube

This paper presents for the first time the nanocrystalline, semiconducting ferroelectrics antimony sulfoiodide (SbSI) grown in multiwalled carbon nanotubes (CNTs). It was prepared sonochemically using elemental Sb, S and I in the presence of methanol under ultrasonic irradiation (35 kHz, 2.6 W/cm²) at 323 K for 3 h. The CNTs filled with SbSI were characterized by using techniques such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, high-resolution transmission electron microscopy, selected area electron diffraction, and optical diffuse reflection spectroscopy. These investigations exhibit that the SbSI filling the CNTs is single crystalline in nature and in the form of nanowires. It has indirect forbidden energy band gap E_gIf = 1.871(1) eV.     

A twice liquid arc discharge approach for synthesis of visible-light-active nanocrystalline Ag:ZnO photocatalyst

Ag:ZnO hybrid nanostructures were successfully prepared by a twice arc discharge method in liquid. The visible light photocatalytic activities were successfully demonstrated for the degradation of Rhodamine B (Rh. B), Methyl orange (MO), and Methylene blue (MB) as standard organic compounds under the irradiation of 90 W halogen light for 2 h. The Ag:ZnO nanostructures were characterized by X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet-visible absorption spectroscopy (UV-Vis). The results revealed that the Ag:ZnO nanostructures extended the light absorption spectrum toward the visible region and significantly enhanced the Rh. B photodegradation under visible light irradiation. 3 mM Ag:ZnO nanostructures exhibited highest photocatalytic efficiency. It has been confirmed that the Ag:ZnO nanostructures could be excited by visible light (E<3.3 eV). The significant enhancement in the Ag:ZnO nanostructures photocatalytic activity under visible light irradiation can be ascribed to the effect of physisorbed noble metal Ag by acting as electron traps in ZnO band gap. A mechanism for photocatalytic degradation of organic pollutant over Ag:ZnO photocatalyst was proposed based on our observations.     

Polyol synthesis of polycrystalline cuprous oxide nanoribbons and their growth chemistry

A facile organic-solution method was developed for the synthesis of two-dimensional cuprous nanostructures. Ribbons as thin as 50 nm were successfully prepared by dissolving CuCl in ethylene glycol before raising the solution temperature to 150°C in air. Transmission electron microscopic studies revealed that the ribbon nanostructures obtained were polycrystalline, with nanocrystals present in the structures mostly less than 25 nm. Selective-area electron diffraction patterns taken from the ribbon nanostructures indicated that the chemical composition of the nanocrystals was Cu₂O, though X-ray photoelectron spectrometric analysis showed that the nanostructures also contained the Cu²⁺ phase. Growth factors including the molecular structure of the solvent and the counter-ion of copper in the precursor that may affect the formation of polycrystalline nanoribbons were examined. More importantly, the detail of chemistry involved in the step-by-step, dimensional growth of copper-based nanostructures in ethylene glycol is presented at the molecular level for the first time using the growth of the Cu₂O nanoribbon as an example. Ethylene glycol chelates Cu²⁺, which is produced from Cu⁺ undergoing disproportionation reactions, to form tetragonally elongated glycolates. A sequence of nucleophilic substitutions then takes place to bond glycolates together to yield stripe-like polymers before the polymers aggregate via van der Waals force into ribbon nanostructures. The Cu⁰ produced from the disproportionation reaction is crystallized out within the polymers and oxidized at elevated temperature by the dissolved O₂ in the solution to form Cu₂O nanocrystals.     

Ultrasonic assisted synthesis,characterization and influence factors of monodispersed dumbbell-like YF3 nanostructures

In the present paper, we reported the successful synthesis of dumbbell-like YF₃ nanostructures with a high yield in a mixed system of water/N,N-dimethylformamide (DMF) under the assistance of ultrasound waves of 40 kHz with the ultrasonic power of 100% (200 W) at 65 °C for 2 h, employing Y₂O₃ (99.99%) and NH₄F as the starting reactants. The product was characterized by means of powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED) pattern and field-emission scanning electron microscopy (SEM). Some factors influencing the morphology of YF₃ nanostructures, including the ultrasonic time and power, the amount of NH₄F, and the ratio of water/DMF, were systematically investigated. Research showed that the morphology of YF₃ could be tuned by the volume ratio of water/DMF. The roles of DMF and the ultrasonic wave in the formation of YF₃ nanostructures were discussed.     

Sonophotocatalytic degradation of trypan blue and vesuvine dyes in the presence of blue light active photocatalyst of Ag3PO4/Bi2S3-HKUST-1-MOF: Central composite optimization and synergistic effect study

An efficient simultaneous sonophotocatalytic degradation of trypan blue (TB) and vesuvine (VS) using Ag₃PO₄/Bi₂S₃-HKUST-1-MOF as a novel visible light active photocatalyst was carried out successfully in a continuous flow-loop reactor equipped to blue LED light. Ag₃PO₄/Bi₂S₃-HKUST-1-MOF with activation ability under blue light illumination was synthesized and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), photoluminescence (PL) and diffuse reflectance spectra (DRS). The effect of operational parameters such as the initial TB and VS concentration (5–45 mg/L), flow rate (30–110 mL/min), irradiation and sonication time (10–30 min), pH (3–11) and photocatalyst dosage (0.15–0.35 g/L) has been investigated and optimized using central composite design (CCD) combined with desirability function (DF). Maximum sonophotodegradation percentage (98.44% and 99.36% for TB and VS, respectively) was found at optimum condition set as: 25 mg/L of each dye, 70 mL/min of solution flow rate, 25 min of irradiation and sonication time, pH 6 and 0.25 g/L of photocatalyst dosage. At optimum conditions, synergistic index value was obtained 2.53 that indicated the hybrid systems including ultrasound irradiation and photocatalysis have higher efficiency compared with sum of the individual processes.