Effect of synthesis route on the morphologies of silver nanostructures by galvanic displacement reaction

The present study is concerned with the preparation of Ag nanostructures by reduction of AgNO₃ with zinc foil by galvanic displacement reaction. The results confirm that the synthesis route has a direct influence on the morphologies of Ag nanostructures. In addition, the effect of synthesis conditions, including the concentration of AgNO₃ aqueous solutions and reaction time, are investigated. X-ray diffraction (XRD), filed emission scanning electron microscope (SEM) and UV-vis spectra are used to characterize the obtained products. A reasonable formation process of Ag nanostructures is proposed based on the characterization results.     

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.     

Structural and cathodoluminescence assessment of transition metal oxide nanostructures grown by thermal deposition methods

Nanostructures of two transition metal oxides, WO₃ and α-Fe₂O₃, have been grown by a thermal deposition method without a catalyst and characterized by x-ray diffraction, scanning electron microscopy (SEM), high-resolution transmission electron microscopy and cathodoluminescence (CL) in the SEM. WO₃ micro and nanorods exhibit CL emission two orders of magnitude higher than CL intensity from the untreated oxide. α-Fe₂O₃ nanostructures with different morphologies (wires, belts, rods, urchins) were grown at different temperatures on Fe substrates. CL spectra of these nanostructures show emission bands related to charge transfer and ligand field transitions.     

Visible-light photocatalytic degradation of methylene blue with laser-induced Ag/ZnO nanoparticles

The preparation of Ag doped ZnO nanoparticles conducted through the method of laser-induction is presented in this work. The Ag/ZnO nanoparticles attained from various weight percentages of added AgNO₃ relative to ZnO were applied under visible-light irradiation for evaluating the heterogeneous photocatalytic degradations of methylene blue (MB) solutions. It was shown that the catalytic behavior of Ag/ZnO nanoparticles in the visible-light range is notably improved through the Ag deposition onto ZnO nanoparticles by the method of laser-induction with a maximum effectiveness of 92% degradation. The properties of the nanoparticles were characterized by the employments of UV-vis spectroscopy (UV-vis), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), and selected-area electron diffraction (SAED).     

Efficient one-pot synthesis of Ag nanoparticles loaded on N-doped multiphase TiO2 hollow nanorod arrays with enhanced photocatalytic activity

The simultaneous Ag loaded and N-doped TiO₂ hollow nanorod arrays with various contents of silver (Ag/N-THNAs) were successfully synthesized on glass substrates by one-pot liquid phase deposition (LPD) method using ZnO nanorod arrays as template. The catalysts were characterized by Raman spectrum, field-emission scanning electron microscopy (FESEM), high-resolution transmission electron microscope (HRTEM), ultraviolet-vis (UV-vis) absorption spectrum and X-ray photoelectron spectroscopy (XPS). The results suggest that AgNO₃ additive in the precursor solutions not only can promote the anatase-to-rutile phase transition, but also influence the amount of N doping in the samples. The photocatalytic activity of all the samples was evaluated by photodegradation of methylene blue (MB) in aqueous solution. The sample exhibited the highest photocatalytic activity under UV light illumination when the AgNO₃ concentration in the precursor solution was 0.03 M, due to Ag nanoparticles acting as electron sinks; When the AgNO₃ concentration was 0.07 M, the sample performed best under visible light illumination, attributed to the synergetic effects of Ag loading, N doping, and the multiphase structure (anatase/rutile).     

Synthesis of dendritic silver nanostructures by means of ultrasonic irradiation

In this paper, a simple and effective route for the synthesis of silver dendritic nanostructures by means of ultrasonic irradiation has been developed. Well-defined silver dendritic nanostructures were obtained by sonicating the aqueous solution of 0.04 mol/L silver nitrate with 4.0 mol/L isopropanol as reducing agent and 0.01 mol/L PEG400 as disperser for 2 h. The effects of the irradiation time, the concentration of Ag⁺ and the molar ratio of PEG to AgNO₃ on the morphology of silver nanostructures were discussed. The structures of the obtained samples were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED) and X-ray powder diffraction (XRD), and the chemical composition of the dendrites was examined by energy-dispersive X-ray spectrum (EDS).     

Preparation and photocatalytic property of α-Fe2O3 hollow core/shell hierarchical nanostructures

We report the preparation of a novel kind of α-Fe₂O₃ hollow core/shell hierarchical nanostructures self-assembled by nanosheets. A green precursor powder is first prepared using nontoxic and inexpensive FeCl₃ and urea in ethylene glycol by a surfactant-free solvothermal method at 160 °C for 15 h. The α-Fe₂O₃ hollow core/shell hierarchical nanostructures are obtained by the thermal treatment of the green precursor powder. The as-prepared α-Fe₂O₃ hollow core/shell hierarchical nanostructures are porous, and exhibit a good photocatalytic activity for the degradation of phenol. The samples are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM).     

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.     

Simultaneous synthesis of TiO2 microrods in situ decorated with Ag nanoparticles and their bactericidal efficiency

In this study, we report a simple and cost-effective method for in situ decoration of Ag NPs onto nanoporous TiO₂ microrods by one medium (ethylene glycol) that can produce two different morphologies. In order to investigate the morphology, phase composition, crystalline structure, and chemical state (valency) of samples before and after annealing in air at different temperatures, field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were performed. The present results show that the size, morphology and crystallinity of both Ag NPs and TiO₂ microrod substrate depend on the post-annealing treatment temperatures. The annealed Ag–TiO₂ NP/microrod composites show large inhibition zones against E. coli bacteria. The obtained Ag–TiO₂ composites have the potential for use as a novel antibacterial material and in water treatment applications.     

Structural transformation of MoO<Subscript>3</Subscript> nanobelts into MoS<Subscript>2</Subscript> nanotubes

The structural transformation of MoO₃ nanobelts into MoS₂ nanotubes using a simple sulfur source has been reported. This transformation has been extensively investigated using electron microscopic and spectroscopic techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), electron diffraction (ED), and energy-dispersive X-ray analysis (SEM-EDAX and TEM-EDX). The method described in this report will serve as a generic route for the transformation of other oxide nanostructures into the chalcogenide nanostructures.     

Formation of silver nanoclusters in transparent polyimides by Ag-K ion-exchange process

Silver nanoclusters embedded in two transparent fluorinated polyimides, 4,4'-hexafluoroisopropylidene diphthalic anhydride – 2,3,5,6-tetramethyl paraphenylene diamine (6FDA-DAD) and 3,3',4,4' – biphenyltetracarboxylic acid dianhydride – 1,1-bis(4-aminophenyl)-1-phenyl-2,2,2-trifluoroethane (BPDA-3F), have been produced by surface modification with KOH aqueous solution followed by K-assisted Ag doping and thermal reduction in hydrogen atmosphere. The reaction rate of the nucleophilic hydrolysis in KOH, studied by Fourier transform infrared spectroscopy (FT-IR) and Rutherford backscattering spectrometry (RBS), depends on the polyimide chemical structure. After ion-exchange in AgNO₃ solution and subsequent annealing, the polyimide structure recovery was monitored by FT-IR whereas the characteristic surface plasmon absorption band of silver nanoparticles was evidenced by optical absorption measurements. The structure of silver nanoclusters as related to size and size distribution in the different polyimide matrices was thoroughly investigated by Transmission electron microscopy (TEM) and X-ray diffraction (XRD). The collected data evidenced a uniform distribution of Ag clusters of nanometric size after thermal treatment at 300 ^○C in both polyimides. For the same ion-exchange treatment parameters and annealing temperature, XRD analyses evidenced the presence of crystallites with similar sizes.     

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.     

Controllable synthesis of PbI2 nanocrystals via a surfactant-assisted hydrothermal route

PbI₂ nanostructures were successfully prepared via a surfactant-assisted hydrothermal method at a low temperature of 100°C for 8 h. Polyvinyl pyrrolidone (PVP) and cetyltrimethylammonium bromide (CTAB) were used as surfactants. The resulting products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV–vis spectroscopy. It was found that the formation of PbI₂ nanostructures with various morphologies could be well controlled by the adjustment of the pH of the synthesis solution, selection of suitable surfactant, and the amount of the desired surfactant. UV–vis absorption results showed an apparent shift of the band gap energy of the PbI₂ nanoparticles relative to that of the bulk.     

Growth mechanism and photoluminescence of the SnO2 nanotwists on thin film and the SnO2 short nanowires on nanorods

SnO2 nanotwists on thin film and SnO2 short nanowires on nanorods have been grown on single silicon substrates by using Au-Ag alloying catalyst assisted carbothermal evaporation of SnO2 and active carbon powders.The morphology and the structure of the prepared nanostructures are determined on the basis of field-emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),selected area electronic diffraction(SAED),high-resolution transmission electron microscopy(HRTEM),x-ray diffraction(XRD),Raman and photoluminescence(PL) spectra analysis.The new peaks at 356,450,and 489 nm in the measured PL spectra of two kinds of SnO2 nanostructures are observed,implying that more luminescence centres exist in these SnO2 nanostructures due to nanocrystals and defects.The growth mechanism of these nanostructures belongs to the vapour-liquid-solid(VLS) mechanism.     

Immobilization of silver nanoparticles on silica microspheres

The silver nanoparticles (Ag NPs) have been immobilized onto silica microspheres through the adsorption and subsequent reduction of Ag⁺ ions on the surfaces of the silica microspheres. The neat silica microspheres that acted as the core materials were prepared through sol–gel processing; their surfaces were then functionalized using 3-mercaptopropyltrimethoxysilane (MPTMS). The major aims of this study were to immobilize differently sized Ag particles onto the silica microspheres and to understand the mechanism of formation of the Ag nano-coatings through the self-assembly/adsorption behavior of Ag NPs/Ag⁺ ions on the silica spheres. The obtained Ag NP/silica microsphere conglomerates were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and energy-dispersive spectroscopy (EDS). Their electromagnetic wave shielding effectiveness were also tested and studied. The average particle size of the obtained Ag NPs on the silica microsphere was found that could be controllable (from 2.9 to 51.5 nm) by adjusting the ratio of MPTMS/TEOS and the amount of AgNO₃.     

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).     

Controlled synthesis of BaWO4 hierarchical nanostructures by exploiting oriented attachment in the solution of H2O and C2H5OH

Shape-controlled synthesis of BaWO₄ hierarchical nanostructures has been successfully achieved by exploiting oriented attachment in a mixture of water and ethanol. A controlled change in the volume ratio of C₂H₅OH and H₂O or the concentration of initial reagents has resulted in the synthesis of products of various morphologies, such as shuttle-like, ellipsoid-like, and flower-like ones. The obtained products are characterized by field emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray powder diffraction, and Fourier transform infrared spectroscopy. The altered nucleation and growth rates of primary particles that assembled to the final hierarchical nanostructures through oriented attachment are the main cause of the evolution of their morphologies. The room-temperature photoluminescent intensities of the products strongly depend on their morphology.     

A novel method for synthesis of colloidal silver nanoparticles by arc discharge in liquid

This paper presents a novel, inexpensive and one-step approach for synthesis of silver nanoparticles (Ag NPs) using arc discharge between titanium electrodes in AgNO₃ solution. The resulting nanoparticles were characterized using UV–Vis spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Silver nanoparticles of 18 nm diameter were formed during reduction of AgNO₃ in plasma discharge zone. Optical absorption spectroscopy of as prepared samples at 15 A arc current in AgNO₃ solution shows a surface plasmon resonance around 410 nm. It was found that sodium citrate acts as a stabilizer and surface capping agent of the colloidal nanoparticles. SEM images exhibit the increase of reduced nanoparticles in 6 min arc duration compared with 1 min arc duration. TEM image of the sample prepared at 6 min arc duration shows narrow size distribution with 18 nm mean particle size. Antibacterial activities of silver nanoparticles were investigated at the presence of Escherichia coli (E-coli) bacteria.     

Effect of Ag doping on the crystallization and phase transition of TiO2 nanoparticles

TiO₂ nanoparticles doped with different Ag contents were prepared by a modified sol–gel method, using titanium tetraisopropoxide and silver nitrate as precursors and 2-propanol as solvent. Silver was incorporated into the TiO₂ matrix via decomposition of AgNO₃ during thermal treatment in different atmospheres. Effects of Ag doping on the crystallization and phase transition of the TiO₂ nanoparticles were studied using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD), and Raman spectroscopy techniques. While air annealing incorporates silver into TiO₂ matrix in silver oxide form, annealing in nitrogen incorporates metallic silver into TiO₂. Formation of silver oxide increases the thermal stability of the TiO₂ particles. Silver oxide affects the crystallization process of TiO₂ particles and the temperature of transition form anatase to rutile. On the other hand, presence of metallic silver in the samples annealed in nitrogen atmosphere decreases the temperature of phase transition of TiO₂ nanoparticles.     

Influence of bases on hydrothermal synthesis of titanate nanostructures

A hydrothermal treatment of titanium dioxide (TiO₂) with various bases (i.e., LiOH, NaOH, KOH, and NH₄OH) was used to prepare materials with unique morphologies, relatively small crystallite sizes, and large specific surface areas. The experimental results show that the formation of TiO₂ is largely dependent on the type, strength and concentration of a base. The effect of the nature of the base used and the concentration of the base on the formation of nanostructures were investigated using X-ray diffraction, Raman spectroscopy, transmission and scanning electron microscopy, as well as surface area measurements. Sodium hydroxide (NaOH) and potassium hydroxide (KOH) were both used to transform the morphology of starting TiO₂ material.