Preparation of dendritic Ag/Au bimetallic nanostructures and their application in surface-enhanced Raman scattering

Dendritic Ag/Au bimetallic nanostructures have been synthesized via a multi-stage galvanic replacement reaction of Ag dendrites in a chlorauric acid (HAuCl₄) solution at room temperature. After five stages of replacement reaction, one obtains structures with protruding nanocubes; these will mature into many porous structures with a few Ag atoms that are left over dendrites. The morphological and compositional changes which evolved with reaction stages were analyzed by using scanning electron microscopy, transmission electron microscopy, UV-visible spectroscopy, selected area electron diffraction and energy-dispersive X-ray spectrometry. The replacement of Ag with Au was confirmed. A formation mechanism involving the original development of Ag dendrites into porous structures with the growth of Au nanocubes on this underlying structure as the number of reaction stages is proposed. This was confirmed by surface-enhanced Raman scattering (SERS). The dendritic Ag/Au bimetallic nanostructures could be used as efficient SERS active substrates. It was found that the SERS enhancement ability was dependent on the stage of galvanic replacement reaction.     

Two-dimensional monolayers of single-crystalline α-Fe2O3 nanospheres: Preparation, characterization and SERS effect

Two-dimensional (2-D) α-Fe₂O₃ monolayers have been successfully prepared by assembling of single-crystalline α-Fe₂O₃ nanospheres onto the surfaces of quartz slides. Hexamethylene diisocyanate (HDI) has been used as “bridge” to link between quartz surface and single-crystalline α-Fe₂O₃ nanospheres. The resulting monolayers have been characterized by transmission electron microscopy (TEM) and scan electron microscopy (SEM), and the correlated surface-enhanced Raman scattering (SERS) effect has been investigated. It is found that the well ordered monolayers of single-crystalline α-Fe₂O₃ nanospheres can be used as nicer substrates for SERS.     

Preparation of silver nanoparticles dispersed in polyacrylonitrile nanofiber film spun by electrospinning

Ag nanoparticles dispersed in polyacrylonitrile (PAN) nanofiber film spun by electrospinning were in situ prepared by reduction of silver ions in N₂H₅OH aqueous solution. The Ag/PAN nanocomposite film was characterized by UV absorption spectroscopy, transmission electron microscopy (TEM) and surface-enhanced Raman scattering (SERS) spectroscopy. UV spectrum and TEM image show that silver nanoparticles with average diameter of 10 nm were obtained and dispersed homogeneously in PAN nanofibers. SERS spectrum indicates that the structure of PAN has been changed after Ag nanoparticles are dispersed in PAN.     

The fabrication of SnSe/Ag nanoparticles on TiO2 nanotubes

SnSe and silver (Ag) nanoparticles were sequentially deposited on TiO₂ nanotube (NT) by pulsed electrochemical deposition and polyol chemistry process, respectively. The morphological observation under scanning electron microscope (SEM) showed that the average size of SnSe was about 30 nm and the Ag was about 5 nm. Transmission electron microscopy (TEM) combined with selected area electron diffraction (SAED) examination indicated that Ag nanoparticles exhibited a well-defined crystallinity. However, SnSe nanoparticles were amorphous and they turned to crystalline after being annealed at 300 °C in the atmosphere. The photocatalytic behavior of SnSe/Ag-TiO₂ NT was evaluated by UV–vis diffuse reflectance spectra (DRS). The results showed that the deposition of SnSe and Ag nanoparticles increased light absorption intensity in the wavelength range of visible light, which implied that the SnSe/Ag-TiO₂ NT is a promising ternary hybrid material in photocatalysis.     

Hydrothermal synthesis of single-crystal BaTiO3 dendrites

In this paper, we report a simple hydrothermal method without any surfactants, for the first time, to synthesize single-crystal BaTiO₃ dendrites. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). The KOH concentration was found to be vital to the final formation of BaTiO₃ dendrites. An obvious morphology evolution from sphere-like shape to dendrite was observed when KOH concentration was decreased from 1 M to 0.1 M. It is rational to expect that dendritic structures of other perovskite oxides may also be synthesized by this simple method.     

Surface-enhanced Raman scattering substrate of silver nanoparticles depositing on AAO template fabricated by magnetron sputtering

In this report, we describe a fabrication process of low-cost and highly sensitive SERS substrates by using a simple anodizing setup and a low-energy magnetron sputtering method. The structure of the SERS substrates consists of silver nanoparticles deposited on a layer of anodic aluminum oxide (AAO) template. The fabricated SERS substrates are investigated by a scanning electron microscope (SEM), a transmission electron microscope (TEM), and a confocal Raman spectroscope. We have verified from the surface morphology that the fabricated SERS substrates consist of high-density round-shape silver nanoparticles where their size distribution ranges from 10 to 30 nm on the top and the bottom of nanopores. The surface-enhanced Raman scattering activities of these nanostructures are demonstrated using methylene blue (MB) as probing molecules. The detection limit of 10⁻⁸ M can be achieved from this SERS substrate.     

Photochemical synthesis and characterization of Ag/TiO2 nanotube composites

TiO₂ nanotubes were fabricated by a hydrothermal method. Silver nanoparticles with diameters around 3–5 nm were loaded onto the surface of TiO₂ nanotubes via a deposition approach followed by a photochemical reduction process under ultraviolet irradiation. Transmission electron microscopy (TEM), N₂ adsorption measurements, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis diffuse reflectance spectroscopy (UV-vis), and fluorescence spectroscopy (FL) were applied to characterize the as-prepared Ag/TiO₂ nanotube composites. The photocatalytic activity of the as-prepared materials was investigated by photodegrading of methyl orange. The results showed that silver particles were in zero oxidation state and highly dispersed on the surface of TiO₂ nanotubes when the concentration of Ag⁺ was low. The presence of metallic silver can help the electron-hole separation by attracting photoelectrons. The Ag/TiO₂ nanotube composites with a suitable amount of silver showed a further improvement on the photocatalytic activity for degradation of methyl orange in water.     

Microstructures of high-Jc melt-textured YBa2Cu3O7?x/Ag superconductors

Silver has been previously added to the melt-textured YBa₂Cu₃O_7–x in order to increase the critical current density (J _c ) of these materials. However, the effect of this addition on theJ _c is presently unclear. The purpose of this study is to investigate the effect of silver on both critical current density and the microstructure of the melt-textured YBa₂Cu₃O_7–x superconductors by means of X-ray diffraction, optical polarized microscopy, and transmission electron microscopy (TEM). TheJ _c of the MTG YBCO/Ag samples is more than 10⁴A/cm² under the 5 kOe magnetic field. It has been shown that as the concentration of silver increases, the fraction of the 211 phase dispersed within the 123 matrix decreases. Therefore, theJ _c slightly decreases. These results, together with the effect of the 211 phase, dislocations, and other structure defects on flux pinning, are described in this paper.     

Surface-enhanced Raman scattering substrate of silver nanoparticles depositing on AAO template fabricated by magnetron sputtering

In this report, we describe a fabrication process of low-cost and highly sensitive SERS substrates by using a simple anodizing setup and a low-energy magnetron sputtering method. The structure of the SERS substrates consists of silver nanoparticles deposited on a layer of anodic aluminum oxide (AAO) template. The fabricated SERS substrates are investigated by a scanning electron microscope (SEM), a transmission electron microscope (TEM), and a confocal Raman spectroscope. We have verified from the surface morphology that the fabricated SERS substrates consist of high-density round-shape silver nanoparticles where their size distribution ranges from 10 to 30 nm on the top and the bottom of nanopores. The surface-enhanced Raman scattering activities of these nanostructures are demonstrated using methylene blue (MB) as probing molecules. The detection limit of 10⁻⁸ M can be achieved from this SERS substrate.     

Synthesis and characterisation of SnO2 nano-single crystals as anode materials for lithium-ion batteries

Rutile structure SnO₂ nano-single crystals have been synthesized using tin (IV) chloride as precursor by the modified hydrothermal method. Controllable morphology and size of SnO₂ could be obtained by adjusting the concentration of the hydrochloric acid. The SnO₂ nanoparticles were characterised by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and electrochemical methods. The SnO₂ nanoparticles as anode materials in lithium-ion batteries exhibit high lithium storage capacities. The reversible capacities are more than 630 mA h g^− 1.     

The role of Ag particles deposited on TiO2 or Al2O3 self-organized nanoporous layers in their behavior as SERS-active and biomedical substrates

In this paper, we present recent results of investigations of hybrid materials consisting of nanoporous oxides layers loaded with Ag nanoparticles: Ag/TiO₂-n/Ti and Ag/Al₂O₃-n/Al (where “n-“stands for nanotubes), which could be used as active SERS substrates or as bioactive materials in medicine (implants). Simple electrochemical, chemical and physical methods appear suitable for fabricating such hybrid materials having different functional properties.     

Method for effective immobilization of Ag nanoparticles/graphene oxide composites on single-stranded DNA modified gold electrode for enzymeless H2O2 detection

In this paper, we report a new method for effective immobilization of Ag nanoparticles (AgNPs) decorated graphene oxide (AgNP/GO) composites onto thiolated single-stranded DNA decorated Au electrode (AuE) surface. The novel immobilization method is based on the coordination interactions and π–π stacking interactions between DNA bases and AgNP/GO composites. The morphologies of the AgNP/GO nanocomposites are characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). It is found that the AgNP/GO-decorated AuE exhibits remarkable catalytic performance for H₂O₂ reduction. This H₂O₂ sensor has a fast amperometric response time of less than 5 s. The linear range is estimated to be from 0.1 mM to 20 mM (r = 0.998) and the detection limit is estimated to be 1.9 μM at a signal-to-noise ratio of 3, respectively.     

Silver effect on the structure of SiO2-CaO-P2O5 ternary system

In this study are reported results obtained from the structural, morphological and textural investigations of 56SiO₂?(40-x)CaO·4P₂O₅·xAg₂O system, where 0 ≤ x ≤ 10 mol%. The samples obtained by sol-gel method were annealed and then characterized by X-ray diffraction (XRD), differential thermal analysis (DTA), thermal gravimetric analysis (TGA), vibrational spectroscopy (Raman, FTIR), N₂-adsorption measurements, and transmission electron microscopy (TEM). XRD patterns of the investigated samples exhibit tricalcium phosphate (TCP) nanostructured phase and show the existence of metallic silver as dispersed phase. The presence of apatite-like phase is underlined by the recorded Raman and especially FT-IR spectra. TEM pictures indicate the presence of silver nanoparticles of almost spherical shapes and various sizes inside the matrix, depending on the Ag₂O content. Regarding the textural properties, it was observed both a decrease of the specific surface area as well as a progressive change of the mesoporous characteristics with the silver addition, the latter behavior recommending the potential use of these samples for applications, where the morphology control is required.     

Synthesis and electrocatalytic property of mono-dispersed Ag/Fe3O4 composite micro-sphere

One-step reaction was designed to synthesize mono-dispersed Ag/Fe₃O₄ micro-sphere with different Ag content via a facile and easily controlled hydrothermal method without use of any surfactant. The phases and composition analysis of the as-prepared samples were characterized by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. The morphology of the samples was observed by transmission electron microscopy (TEM) and field-emission scanning electron microscopy (FE-SEM). The results revealed that the Ag/Fe₃O₄ composite samples with different Ag content were micro-spheres with almost the identical size of 175 nm or so in diameter. The electrocatalytic activity of the resultant samples modified on a glassy carbon electrode (GCE) for p-nitrophenol reduction in a basic solution was investigated. The results indicated that all the samples exhibited enhanced electrocatalytic activity for p-nitrophenol reduction, and the sample with 3% Ag exhibited the highest electrocatalytic one.     

Preparation of Ag2S–Graphene nanocomposite from a single source precursor and its surface-enhanced Raman scattering and photoluminescent activity

Ag₂S–Graphene nanocomposite was prepared via a relatively facile hydrothermal method, using a single-source molecular (silver diethyldithiocarbamate [Ag(DDTC)]) as precursor and graphene sheets as a support material. The composite was characterized by X-ray power diffraction, X-ray photoelectron spectroscopy, Field-emission scanning electron microscope, transmission electron microscopy, Fourier transform infrared, Raman spectra and fluorescence spectroscopy. The experimental results show that the Ag₂S–Graphene nanocomposite displays surface-enhanced Raman scattering (SERS) activity for graphene oxide and reveals relatively better fluorescence property compared with pure Ag₂S.     

Synthesis and characterization of L-histidine capped silver nanoparticles

L-histidine capped Ag nanoparticles have been synthesized by a hydrothermal method. Spherical Ag nanoparticles with average diameter ranging from 9 to 21 nm can be obtained by tuning the reaction pH and the reactant ratio. The topography, surface and internal structures of the histidine capped Ag nanoparticles have been characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM), dynamic light scattering, X-ray photoelectron spectroscopy (XPS), X-ray Diffraction (XRD), Raman spectroscopy and UV–vis absorption spectroscopy. Surface enhanced Raman scattering (SERS) results revealed that the Ag colloid in present study have a structure that the imidazole moiety of histidine is bound on the Ag surface and COO^? group is exposed outward. The as-synthesized Ag colloidal solution was very stable and can be stored at room temperature at least one month. In addition, it was found that the solution color of Ag colloid can change from yellow to reddish-brown by addition of the NiCl₂ solution, which may have potential application for Ni²⁺ detection.     

Solvothermal synthesis of In(OH)3 nanorods and their conversion to In2O3

In this work, we demonstrate that monodisperse indium hydroxide (In(OH)₃) nanorods constructed with parallel wire-like subunits have been fabricated via a acrylamide-assisted synthesis route without any template. NH₃ from the hydrolysis of acrylamide acts as the OH⁻ provider. The structure and morphology of as-prepared products have been characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and thermogravimetric analysis (TG). A detailed mechanism has been proposed on the basis of time-dependent experimental results. Furthermore, by annealing In(OH)₃ precursors at 500 °C for 3 h in air, In₂O₃ samples were obtained with the designed morphology.     

Facile synthesis of MnO2/CNT nanocomposite and its electrochemical performance for supercapacitors

A nanocomposite of manganese dioxide coated on the carbon nanotubes (MnO₂/CNTs) was synthesized by a facile direct redox reaction between potassium permanganate and carbon nanotubes without any other oxidant or reductant addition. The morphology, microstructure and crystalline form of this MnO₂/CNT nanocomposite were characterized by scanning electron microscopy (SEM), transition electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The electrochemical properties are characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and galvanostatic charge/discharge (GCD). The results show that the facile prepared MnO₂/CNTs nanocomposite shows specific capacitance of 162.2 F g⁻¹ at the current density of 0.2 A g⁻¹ and excellent charge/discharge property with 90% of its specific capacitance kept after 2000 cycles at the current density of 5 A g⁻¹.     

Solvothermal synthesis of sheet-like Co3O4 and Ag/Co3O4 nanocomposites and their electrocatalysis performances

Precursors of Co₃O₄ and Ag/Co₃O₄ composites with sheet-like shape were synthesized with assistance of ethylene glycol via a solvothermal process. The final samples were obtained by calcining each precursor at 400 °C. The as-prepared samples were identified and characterized by thermogravimetric analysis (TG) and differential thermal gravimetric (DTG) analysis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FE-SEM). The Co₃O₄ and Ag/Co₃O₄ composite nanosheets were used as electrocatalysts modified on a glassy carbon electrode for p-nitrophenol and H₂O₂ reduction respectively in a basic solution. The electrocatalytic results showed that p-nitrophenol could be reduced by pure Co₃O₄ at a large peak current but a rather higher peak potential, and could be reduced effectively by Ag/Co₃O₄ composites at lower potential. Ag/Co₃O₄ composites with 6% Ag displayed the highest electrocatalytic activity for H₂O₂ reduction at the largest peak current and a lower peak potential. The reduction peak potentials of H₂O₂ all reduced a great deal using Ag/Co₃O₄ composite.     

Facile synthesis of Ag nanoparticles supported on TiO2 inverse opal with enhanced visible-light photocatalytic activity

TiO₂ inverse opal films loaded with silver nanoparticles (ATIO) were synthesized on glass substrates. TiO₂ inverse opal (TIO) films were prepared via a sol-gel process using self-assembly of SiO₂ colloidal crystal template and a facile wet chemical route featuring an AgNO₃ precursor solution to fabricate silver nanoparticles on the TIO films. The inverse opal structure and Ag deposition physically and chemically modify titania, respectively. The catalysts were characterized by Raman spectroscopy, field-emission scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), UV-vis absorption spectra, X-ray photoelectron spectroscopy and photoluminescence spectroscopy. The HRTEM results show that Ag nanoparticles measuring 5-10 nm were evenly distributed on TIO. Both the UV- and visible-light photocatalytic activities of the samples were evaluated by analyzing the degradation of methylene blue (MB) in aqueous solution. The results reveal that the apparent reaction rate constant (k_app) of MB degradation of the sample ATIO under UV-light irradiation is approximately 1.5 times that of the conventional Ag-loaded TiO₂ film (ATF) without an ordered porous structure at an AgNO₃ concentration of 5 mM in the precursor solution. At an AgNO₃ concentration of 10 mM, the sample exhibits a k_app value approximately 4.2 times that of ATF under visible-light irradiation. This enhanced visible-light photocatalytic performance can be attributed to the synergistic effect of optimized Ag nanoparticle deposition and an ordered macroporous TIO structure. Repeated cycling tests revealed that the samples showed stable photocatalytic activity, even after six repeated cycles.