水热合成法制备银-氧化锡复合粉体备

采用水热合成法,以亚硫酸钠为还原剂,用硝酸银、氨水和锡酸钠为原料制备银-氧化锡复合粉体,对制备的粉体进行X射线衍射、扫描电镜和能谱分析。结果表明:采用水热合成法可以制备出银-氧化锡颗粒,颗粒近似球形,粒径约为400 nm;该粉体由银和氧化锡两种物相组成,银的衍射峰非常明显,银元素和锡元素在粉体中均匀分布,可以推断银和氧化锡的分布是均匀的。     

Silver nanorods using HEC as a template by γ-irradiation technique and absorption dose that changed their nanosize and morphology

Silver (Ag) nanorods with average diameters of 20 nm and lengths up to 250 nm were successfully prepared in large scale using hydroxyethyl cellulose (HEC) as a template reducing silver nitrate by γ-irradiation. When we changed the irradiation time to get a different absorption dose at the same dose rate, we can find that the silver nanorods have been transferred into a larger size and another morphology. The particle size and morphology can be changed by choosing different absorption doses under the same dose rate. The products were characterized by transmission electron microscopy (TEM), electron diffraction (ED) analysis, field-emission scanning electron microscopy (FESEM), X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS).     

Shape- and size-selective electrochemical synthesis of dispersed silver(I) oxide colloids

Silver(I) oxide (Ag2O) micro- and nanoparticles were electrochemically synthesized by anodizing a sacrificial silver wire in a basic aqueous sulfate solution. Ag2O particles were released from the silver electrode surface during synthesis producing a visible sol "stream". The composition of these particles was established using selected area electron diffraction, X-ray diffraction, and X-ray photoelectron spectroscopy. The shape of Ag2O crystallites could be adjusted using the potential of the silver wire generator electrode. The generation of a dispersed Ag2O sol and the observed shape selectivity are both explained by a two-step mechanism involving the anodic dissolution of silver metal, Ag0 --> Ag+(aq) + 1e-, followed by the precipitation of Ag2O particles, 2Ag+ + 2OH- --> Ag2O(s) + H2O. Within 100 mV of the voltage threshold for particle growth, cubic particles with a depression in each face ("hopper crystals") were produced. The application of more positive voltages resulted in the generation of 8-fold symmetric "flower"-shaped particles formed as a consequence of fast growth in the <111> crystallographic direction. The diameter of flower particles was adjustable from 250 nm to 1.8 microm using the growth duration at constant potential.     

超声诱导单分散银胶体的制备及表征

为了研究制备工艺条件对单分散银胶体稳定性的影响,在超声场作用下,以聚乙烯吡咯烷酮(PVP)为保护剂,硝酸银为前驱物,经硼氢化钾还原制备了稳定的单分散银胶体.考察了保护剂和还原剂用量、超声时间和超声功率等因素对银胶体稳定性的影响,利用透射电镜、选区电子衍射和分光光度等技术对制备的银胶体进行了表征.结果表明:银纳米粒子为面心立方(FCC)结构;PVP与AgNO3质量比为1:1时,PVP可有效保护银粒子,获得单分散的球形颗粒;AgNO3与KBH4摩尔比为1:2时,可制得单分散的类球形银纳米颗粒,直径约为20nm;超声50min制得的银胶体主要以单分散的球形纳米颗粒形式存在,粒径在10～20 nm范围内,稳定性好.     

Large-scale fabrication of Ag nanoparticles in PVP nanofibres and net-like silver nanofibre films by electrospinning

Heat treatment of various compositions of AgNO(3)-doped polyvinylpyrrolidone (PVP) composite nanofibres fabricated by electrospinning produced two kinds of silver species: (i) Ag nanoparticles dispersed in PVP nanofibres, when the loading of AgNO(3) was 5?wt%, and (ii)?a net-like silver nanofibre film when the loading of AgNO(3) was five times greater than that of PVP in the composite nanofibres. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible absorption spectroscopy, FT-IR spectra, powder x-ray diffraction (XRD) and x-ray photoelectron spectroscopy (XPS) were used to characterize the silver nanoparticles and nanofibres. The formation mechanisms are discussed based on the redox reaction between AgNO(3) and PVP during heat treatment; essentially, the weight ratios of AgNO(3) to PVP determined the types of morphologies, from Ag nanoparticles to silver nanofibre film. The present results may find some potential application in the design of new composite materials in the dielectric and electronics areas.     

天然石墨-纳米银/聚氨酯导电复合薄膜的制备及性能

采用热处理还原银盐原位引入银粒子的方法, 成功制备了天然石墨-纳米银/聚氨酯(C-Ag/PU)导电复合薄膜。并通过透射电镜(TEM)、 扫描电镜(SEM)观察了该复合薄膜的微观结构, 用X射线衍射仪(XRD)跟踪了银的还原和银粒子的生长过程, 探讨了加热温度和加热时间对银还原过程的影响, 研究了纳米银的生成和聚集对C/PU复合体系导电性能的影响。结果表明, 随着热处理的进行, 银粒子不断地生成和聚集, 最终以纳米尺寸(约10nm)均匀分散在聚合物基体中。纳米银粒子在天然石墨粒子之间起到了桥梁的作用, 改善了复合体系的导电通路, 显著提高了复合体系的导电性。      

Fabrication and chemical etching of Ag/C nanocables

In this paper, Ag/C nanocables were synthesized via a one-step simple hydrothermal route by using glucose as reducing agent and carbon source, AgNO3 as silver source. The products are characterized in detail by multiform techniques: X-ray diffraction, energy-dispersive X-ray analysis, scanning electron microscopy, transmission electron microscopy. The results show that the obtained products are coaxial nanocables with lengths of several micrometers, about 200-500 nm in diameter, and a surrounding sheath about 80-100 nm in thickness. Different products including carbonaceous nanotubes and nanocables with fragmentary Ag core were obtained by adjusting time of chemical etching.     

Synthetic control of large-area, ordered silver nanowires with different diameters

Silver (Ag) nanowires with different diameters (28, 38, 55, 80, 200 nm) have been successfully fabricated into the anodic alumina membranes (AAMs) by direct-current electrochemical deposition technique. X-ray diffraction and selected area electron diffraction analysis show that the as-synthesized samples have preferred (220) orientation independent of the nanowire diameters. Transmission electron microscopy and field-emission scanning electron microscopy investigation reveal that the large-area and highly ordered Ag nanowire arrays with smooth surface and uniform diameter are synthesized, and they have the high aspect ratio. The formation mechanism of the silver nanowires is also discussed. The nanowire arrays with different diameters may have potential applications in the future nanodevices.     

Microwave-assisted rapid synthesis of anisotropic Ag nanoparticles by solid state transformation

Anisotropic silver nanoparticles (NPs) have been synthesized rapidly using microwave irradiation by the decomposition of silver oxalate in a glycol medium using polyvinyl pyrolidone (PVP) as the capping agent. The obtained Ag nanoparticles have been characterized by UV-visible spectroscopy, powder x-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) studies. Anisotropic Ag nanoparticles of average size around 30?nm have been observed in the case of microwave irradiation for 75?s whereas spherical particles of a size around 5-6?nm are formed for 60?s of irradiation. The texture coefficient and particle size calculated from XRD patterns of anisotropic nanoparticles reveal the preferential orientation of (111) facets in the Ag sample. Ethylene glycol is found to be a more suitable medium than diethylene glycol. A plausible mechanism has been proposed for the formation of anisotropic Ag nanoparticles from silver oxalate.     

活性碳纤维载银工艺及其表面银颗粒的形态特征

以自制粘胶基活性碳纤维（ＡＣＦ）为载体，通过真空浸渍和真空热分解的方法在其表面沉积银，制得了载银活性碳纤维（ＡＣＦ（Ａｇ）。研究了载银工艺参数对ＡＣＦ（Ａｇ）的银含量、表面银颗粒大小、分布及形态的影响规律，提出了银颗粒的形核与长大机制；此外，还分析了银颗粒与ＡＣＦ结合力的影响因素。     

海藻酸钠光化学还原法制备纳米银

以海藻酸钠为还原剂和稳定剂,经紫外光照射 AgNO3溶液在室温下制备出纳米银。通过紫外吸收光谱(UV-Vis)、X 射线衍射(XRD)、红外光谱(FTIR)、透射电镜(TEM)、抑菌实验等对纳米银进行表征。结果表明,照射时间、海藻酸钠和 AgNO3浓度对纳米银生成均有影响。在 AgNO3浓度为1 mmol/L,海藻酸钠浓度为0.5%,反应时间为2 h 时能够生成理想的纳米银。此时生成的银纳米粒子为球形,粒径分布均匀,粒径大小在1~5 nm 之间,对大肠杆菌和金黄色葡萄球菌均有较强的抑菌性。     

Polyurethane–silver fibers prepared by infiltration and reduction of silver nitrate

Silver-incorporating polyurethane fibers were prepared by infiltration of silver nitrate on electrospun polyurethane fibers and reduction with sodium borohydride. They were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and energy-dispersive X-ray system. The Ag nanoparticles prepared by reduction of silver nitrate showed nano-sized crystals of 4–10 nm in diameter. However, larger aggregated Ag particles of 50–200 nm were also found to be dispersed in the polyurethane matrix when Ag particles were formed in electrospun fibers by the infiltration–reduction process of silver nitrate. As a result, infiltration method of silver nitrate into the electrospun fibers was significantly effective to produce silver-incorporating fibers due to a high specific surface area of fibers.     

Microstructure and microchemistry of silicon particles formed during electrical-discharge machining

The structure and morphology of particles representing the byproduct of electrical-discharge machining (EDM) were analyzed using transmission electron microscopy (TEM). The EDM process involved high-efficiency and high-accuracy fine boring of a single-crystal silicon ingot by high-frequency electrical spark discharges. As the silver electrode advanced, spark-discharge-melted or vaporized small particles of the silicon workpiece were produced and the particles were flushed away and collected in deionized water. Standard TEM and analytical electron microscopy (AEM) observations were carried out. Bright-field (BF) images, diffraction, and energy-dispersive X-ray spectrometry (EDXS) data were obtained to completely characterize the EDM particles. BF images indicated the presence of large silicon particles decorated by smaller silver particles originating from the electrode as the byproducts of the EDM processing. Analysis of the particle-size distribution resulted in an average silicon particle size of about 500 nm decorated by smaller silver particles of an average size of about 65 nm. EDXS spectra depicted individual silicon and silver particles with characteristic peaks that identify the elements present. Selected-area electron diffraction (SAED) pattern confirmed the presence of crystalline silicon. Finally, a set of SAED patterns, EDXS profiles, and TEM images is included that fully describe the particles' chemistry, structure, and morphology, respectively.     

包覆型铜-银双金属粉的制备

为了提高铜粉的抗氧化性能,在超细铜粉表面包覆一层具有优良导电性和抗氧化的银,以乙酰丙酮(Acac)为Cu2+的螯合剂,采用置换反应法制备与原超细铜粉粒度相同的包覆型铜-银双金属粉.采用X射线衍射仪(XRD)、煅烧后增重等手段分析包覆型铜-银双金属粉的抗氧化性能,并用扫描电子显微镜(SEM)表征了其表面形貌.结果表明,乙...     

Dielectric and optical properties of CaCu3Ti4O12 thin films containing Ag nanoparticles

Simple sol-gel techniques are used to prepare thin films of a high dielectric constant perovskite CaCu₃Ti₄O₁₂, containing different amounts of metallic silver nanoparticles. The formations of the silver nanoparticles are verified by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and optical absorption studies. The dielectric properties are found to be significantly affected by the presence of the silver nanoparticles. A maximum in the dielectric constant is observed at an intermediate metal particle concentration. This is explained in terms of the polarization at the particle-dielectric interface and the internal barrier layer capacitor effect. The optical absorption spectrum is compared with Mie theory in electrodynamics for the optical absorption of small particles to extract the particle size of the silver particle. Non-uniform distributions of Ag particles through the thickness of the thin films are reported.     

Microstructure and optical properties of Si–Ag nanocomposite films prepared by co-sputtering

Novel composite thin films consisting of nanosized Ag particles embedded in an amorphous Si matrix were made with Ag contents from 0 at% to 61 at% by radio frequency co-sputtering of Si and Ag. The microstructure and optical properties of the films were characterized by conventional and high resolution transmission electron microscopy and spectrometry in the wavelength range from 200 to 1500 nm. It was found that the films consist of nanosized Ag particles (2.8–6.0 nm) particle and their clusters embedded in an amorphous Si matrix. The optical absorption spectra of the films up to 40 at% Ag exhibit characteristics similar to the amorphous semiconductor Si. At higher Ag contents two absorption maxima at 350 nm and 700 nm appear. Effective medium theories were examined to predict the optical properties of the films and it was found that the predictions from the Sheng Ping theory with a modified dielectric function of bulk Ag (taking into account the mean free path limitation of Ag particle boundaries) qualitatively agree with the measured absorption spectra. The two absorption maxima are accounted for as interfacial plasma resonance absorption associated with the silver particle/silicon matrix interfaces.     

Silver/dendrimer nanocomposites as biomarkers: fabrication, characterization, in vitro toxicity, and intracellular detection

We have synthesized water-soluble, biocompatible, fluorescent, and stable silver/dendrimer nanocomposites that exhibit a potential for in vitro cell labeling. Amino-, hydroxyl-, and carboxyl-terminated ethylenediamine core generation 5 poly(amidoamine) dendrimers were utilized to prepare aqueous silver(I)-dendrimer complexes (with the molar ratio of 25 Ag+ per dendrimer) at the biologic pH of 7.4. Conversion of silver(I)-dendrimer complexes into dendrimer nanocomposites was achieved by irradiating the solutions with UV light to reduce the bound Ag+ cations to zerovalent Ag0 atoms, which were simultaneously trapped in the dendrimer network, resulting in the formation of {(Ag0)25-PAMAM_E5.NH2}, {(Ag0)25-PAMAM_E5.NGly}, and {(Ag0)25-PAMAM_E5.NSAH} dendrimer nanocomposites (DNC), respectively. The silver-DNCs were characterized by means of UV-vis, fluorescence spectroscopy, dynamic light-scattering, zeta potential measurements, high-resolution transmission electron microscopy, X-ray energy dispersive spectroscopy, and selected area electron diffraction. The cytotoxicity of dendrimers and related silver nanocomposites was evaluated using an XTT colorimetric assay of cellular viability. The cellular uptake of nanoparticles was examined by transmission electron and confocal microscopy. Results indicate that {(Ag0)25-PAMAM_E5.NH2}, {(Ag0-)25-PAMAM_E5.NGly}, and {(Ag0)25-PAMAM_E5.NSAH} form primarily single particles with diameters between 3 and 7 nm. The dendrimer nanocomposites are fluorescent, and their surface charge, cellular internalization, toxicity, and cell labeling capabilities are determined by the surface functionalities of dendrimer templates. The {(Ag0)25-PAMAM_E5.NH2} and {(Ag0)25-PAMAM_E5.NSAH} nanocomposites exhibit potential application as cell biomarkers.     

Diospyros assimilis root extract assisted biosynthesised silver nanoparticles and their evaluation of antimicrobial activity

The current research study focuses on biosynthesis of silver nanoparticles (Ag NPs) for the first time from silver acetate employing methanolic root extract of Diospyros assimilis. The UV–Vis absorption spectrum of biologically synthesised nanoparticles displayed a surface plasmon peak at 428 nm indicating the formation of Ag NPs. The influence of metal ion concentration, reaction time and amount of root extract in forming Ag NPs by microscopic and spectral analysis was thoroughly investigated. Structural analysis from transmission electron microscopy confirmed the nature of metallic silver as face‐centered cubic (FCC) crystalline with an average diameter of 17 nm, which correlates with an average crystallite size (19 nm) calculated from X‐ray diffraction analysis. Further, the work was extended for the preliminary examination of antimicrobial activity of biologically synthesised Ag NPs that displayed promising activity against all the tested pathogenic strains.Inspec keywords: antibacterial activity, nanoparticles, silver, particle size, nanofabrication, nanomedicine, biomedical materials, ultraviolet spectra, visible spectra, optical microscopy, surface plasmon resonance, transmission electron microscopy, crystallites, X‐ray diffraction, microorganismsOther keywords: Diospyros assimilis root extract assisted biosynthesised silver nanoparticles, antimicrobial activity, silver acetate, methanolic root extract, UV‐visible absorption spectrum, biologically synthesised nanoparticles, surface plasmon peak, Ag NPs formation, metal ion concentration, reaction time, microscopic analysis, spectral analysis, structural analysis, transmission electron microscopy, metallic silver, FCC crystalline phase, average crystallite size, X‐ray diffraction analysis, pathogenic strains, Ag     

Silver halide-containing photochromic powders of SiO2 sol–gel glass

In order to develop a photochromic powder, an SiO2-gel based on tetraethoxysilane (TEOS) was doped with AgNO3 or AgNO2. The dried gel pieces were pulverized and treated with aqueous or ethanolic halide solutions for growing silver halide microcrystals. Both the introduction of cuprous compounds such as CuBr, CuCl, Cu2O, Cu(CH3COO)2·H2O or sulphur-containing compounds and the formation of AgBrxCl1-x crystals lead to variations of photochromic properties. X-ray diffraction measurements indicate that the average diameters of silver halide microcrystals are limited to 70–110nm. Ultraviolet–visible spectroscopic investigations show the reversibility of the darkening/fading process. Cu+-containing samples exhibit a remarkable fading even at room temperature.     

Preparation of silver nanoparticles having low melting temperature through a new synthetic process without solvent

This study presents a new synthetic method of silver nanoparticles using a novel polyoxyethylene maleate-based surfactant (PEOM). Unlike conventional process using large amount of a solvent to dissolve silver salts, large amount of silver salts (AgNO3) can be dissolved and stabilized by our surfactant without solvent. Silver salts can be dissociated within PEOM by the formation of charge complex between hydrophilic-COOH segments and Ag+NO3-, resulting in formation of self-assembled microstructures which acting as a nano-reactor and stabilizer. After reduction using NaBH4, uniform sized silver nanoparticles were formed in the hydrophilic domain of PEOM. Silver contents in the colloids were changed by 0.5 approximately 3 wt%. Distribution of silver nanoparticle sizes was investigated by using TEM and XRD. Melting temperature of silver nanoparticles was measured by differential scanning calorimetry, which depends upon the particle size of silver nanoparticles. The lowest melting temperature of 112 degrees was measured from 3.5 nm average-sized silver particles.