油酸囊泡层状液晶作为模板电化学合成银纳米颗粒

在油酸囊泡的层状液晶中利用电化学沉积法成功地制备了银纳米颗粒。并用扫描隧道显微镜(STM)和透射电子显微镜(TEM)对银纳米颗粒进行了表征，发现银纳米颗粒能够均匀地分散在油酸囊泡中，并且油酸囊泡能够有效地阻止产生的银纳米颗粒发生聚集反应。此外，我们还提出了银纳米颗粒形成的机理。     

Size characterization and quantification of silver nanoparticles by asymmetric flow field-flow fractionation coupled with inductively coupled plasma mass spectrometry

A method for determining the size of silver nanoparticles and their quantification by asymmetric flow field-flow fractionation coupled with inductively coupled plasma mass spectrometry (ICP-MS) is proposed and was tested in consumer products. Experimental conditions were studied in detail to avoid aggregation processes or alteration of the original size distributions. Additionally, losses from sorption processes onto the channel membrane were minimized for correct quantification of the nanoparticles. Mobile phase composition, injection/focusing, and fractionation conditions were evaluated in terms of their influence on both separation resolution and recovery. The ionic strength, pH, and the presence of ionic and nonionic surfactants had a strong influence on both separation and recovery of the nanoparticles. In general, better results were obtained under those conditions that favored charge repulsions with the membrane. Recovery values of 83 ± 8% and 93 ± 4% with respect to the content of silver nanoparticles were achieved for the consumer products studied. Silver nanoparticle standards were used for size calibration of the channel. The results were compared with those obtained by photon correlation spectroscopy and images taken by transmission electron microscopy. The quantification of silver nanoparticles was performed by direct injection of ionic silver standard solutions into the ICP-MS system, integration of the corresponding peaks, and interpolation of the fractogram area. A limit of detection of 5.6 μg L^-1 silver, which corresponds to a number concentration of 1×10¹² L^-1 for nanoparticles of 10 nm, was achieved for an injection volume of 20 μL.     

Preparation and characterization of nanocomposite ZnO–Ag thin film containing nano-sized Ag particles: influence of preheating,annealing temperature and silver content on characteristics

Nanocomposite ZnO–Ag thin film containing nano-sized Ag particles have been grown on glass substrate by spin-coating technique using zinc acetate dihydrate as starting precursor in 2-propanol as solvent and monoethanolamine as stabilizer. Silver nanoparticles were added in the ZnO sol using silver nitrate dissolved in ethanol-acetonitrile. Their structural, electrical, crystalline size and optical properties were investigated as a function of preheating, annealing temperature and silver content. The results indicated that the crystalline phase was increased with increase of annealing temperature up to 550 °C at optimum preheating temperature of 275 °C. Thermal gravimetric differential thermal analysis results indicated that the decomposition of pure ZnO and nanocomposite ZnO–Ag precursors occurred at 225 and 234 °C, respectively with formation of ZnO wurtzite crystals. The scanning electron microscopy and atomic force microscopy revealed that the surface structure (the porosity and grain size) of the ZnO–Ag thin film (the film thickness is about 379 nm) was changed compared to pure ZnO thin film. The result of transmission electron microscopy showed that Ag particles were about 5 nm and ZnO particles 58 nm with uniform silver nanoclusters. Optical absorption results indicated that optical absorption of ZnO–Ag thin films decreased with increase of annealing temperature. Nanocomposite ZnO–Ag thin films with [Ag] = 0.068 M and [Ag] = 0.110 M showed an intense absorption band, whose maximum signals appear at 430 nm which is not present in pure ZnO thin films. The result of X-ray photoelectron spectroscopy revealed that the binding energy of Ag 3d_5/2 for ZnO–Ag shifts remarkably to the lower binding energy compared to the pure metallic Ag due to the interaction between Ag and ZnO.     

Sol–gel and impregnated prepared silver TiO<Subscript>2</Subscript> semiconductors as photocatalysts for the UV decomposition of 2,4-<Emphasis Type="SmallCaps">d</Emphasis>: a comparative study of the preparation method

UV-photocatalytic oxidation of 2,4-dichlorophenoxyacetic acid (2,4-d) was studied on Silver–TiO₂ semiconductors prepared by co-gelling silver acetylacetonate and titanium butoxide (TiO₂–Ag) or by incipient impregnation with silver acetylacetonate (0.5 wt% Ag) of bare TiO₂ sol–gel and TiO₂–P25 supports. The comparative study shows that only a slight modification on the specific surface area was obtained on the TiO₂–Ag sample (60 m²/g) as compared to the TiO₂ sol–gel bare support (65 m²/g). XRD patterns of the samples show anatase as the crystalline phase present in the sol–gel TiO₂ preparations. By means of HRTEM and HAADF-STEM electron microscopy techniques, silver nanoparticles (<12.0 nm) were identified which are very small to be detected by XRD. The photocatalytic oxidation of the herbicide 2,4-d used as a model of contaminant show for the kinetic parameter t_1/2 values of 45 min for the TiO₂–Ag sample, while for the impregnated Ag/TiO₂ and Ag/P25 nanomaterials t_1/2 was 124 and 66 min, respectively. The higher photoactivity of the TiO₂–Ag photocatalyst is attributed to a combined effect of the silver nanoparticles in interaction with the titania semiconductor.     

Soft-templating synthesis and adsorption properties of mesoporous carbons with embedded silver nanoparticles

Mesoporous carbons containing silver nanoparticles have been successfully synthesized under acidic conditions by employing resorcinol and formaldehyde as carbon precursors and triblock copolymer EO₁₀₁PO₅₆EO₁₀₁ (Lutrol F127) as a soft template. Silver nanoparticles of ∼90 nm were added to the synthesis mixture to achieve 10 wt% and 20 wt% of Ag loading in the carbon. Also, tetraethyl orthosilicate (TEOS) was introduced to the system in order to improve adsorption properties of the silver-carbon composites and to reinforce its structure. The resulting carbons with incorporated silver nanoparticles featured high surface areas, large total pore volumes and primary mesopores in the range between ∼6–7 nm.     

Reduction of silver nitrate by polyaniline nanotubes to produce silver-polyaniline composites

Polyaniline (PANI) nanotubes were prepared by oxidation of aniline in 0.4 M acetic acid. They were subsequently used as a reductant of silver nitrate in 1 M nitric acid, water or 1 M ammonium hydroxide at various molar ratios of silver nitrate to PANI. The resulting PANI-silver composites contained silver nanoparticles of 40–60 nm size along with macroscopic silver flakes. Under these experimental conditions, silver was always produced outside the PANI nanotubes. Changes in the molecular structure of PANI were analyzed by FTIR spectroscopy. Silver content in the composites was determined as a residue by thermogravimetric analysis, and confirmed by density measurements. The highest conductivity of a composite, 68.5 S cm⁻¹, was obtained at the nitrate to PANI molar ratio of 0.67 in water. Also, the best reaction yield was obtained in water. Reductions performed in an acidic medium gave products with conductivity of 10⁻⁴–10⁻² S cm⁻¹, whereas the reaction in alkaline solution yielded non-conducting products.     

Studies on Silver Accumulation and Nanoparticle Synthesis By <Emphasis Type="Italic">Cochliobolus lunatus</Emphasis>

Development of reliable and eco-friendly processes for synthesis of metallic nanoparticles is an important step in the field of application of nanotechnology. Biological systems provide a useful option to achieve this objective. In this study, potent fungal strain was selectively isolated from soil samples on silver supplemented medium, followed by silver tolerance (100–1,000 ppm) test. The isolated fungus was subjected to morphological, 18S rRNA gene sequencing and phylogenic studies and confirmed as Cochliobolus lunatus. The silver accumulation and nanoparticle formation potential of wet cell mass of C. lunatus was investigated. The accumulation and nanoparticle formation by wet fungal cell mass with respect to pH change was also studied. The desorbing assay was used to recover accumulated silver from cell mass. C. lunatus was found to produce optimum biomass (0.94 g%) at 635 ppm of silver. Atomic absorption spectroscopy study showed that at optimum pH (6.5 ± 0.2), cell mass accumulates 55.6% of 100 ppm silver. SEM and FTIR studies revealed that the cell wall of C. lunatus is the site of silver sorption, and certain organic groups such as carbonyl, carboxyl, and secondary amines in the fungal cell wall have an important role in biosorption of silver in nanoform. XRD determined the FCC crystalline nature of silver nanoparticles. TEM analysis established the shape of the silver nanoparticles to be spherical with the presence of very small-sized nanoparticles. Average size of silver nanoparticles (14 nm) was confirmed by particle sizing system. This study reports the synthesis and accumulation of silver nanoparticles through reduction of Ag⁺ ions by the wet cell mass of fungus C. lunatus.     

Preparation of silver nanoparticles in aqueous solutions in the presence of carbonate ions as stabilizers

Silver nanoparticles are prepared by reducing Ag⁺ ions with sodium borohydride in aqueous solutions containing carbonate ions (5 × 10⁻⁵−1 × 10⁻² mol l⁻¹). It is established that carbonate ions represent an efficient stabilizer that provides nanoparticles with electrostatic protection via the formation of an electrical double layer. The maximum stability of a silver dispersion is observed at a carbonate ion concentration of 1 × 10⁻³ mol l⁻¹. The average size of silver nanoparticles is 10.0 ± 2.5 nm. The formation kinetics of silver nanoparticles is described by an equation for a first-order reaction with a rate constant of 2.3 × 10⁻³ s⁻¹ (±20%).     

Glucosamine-functionalized silver glyconanoparticles: characterization and antibacterial activity

We report the analytical and in vitro antibacterial activity of glucosamine-functionalized silver glyconanoparticles. Morphological characterization ensured the surface topography and particle size distribution of both silver and glucosamine–silver nanoparticles. Surface plasmon resonance of both types of nanoparticle was determined from UV–visible spectroscopy using four different sample concentrations (10–40 μL). The resulting functionalized glyconanoparticles show maximum absorbance with a red shift of 30 ± 5 nm (390–400 nm) from their initial absorbance (425–430 nm). FT-Raman and ¹H-NMR spectroscopic measurement confirmed the surface functionalization of glucosamine on the silver surface through the carbonyl group of a secondary amide linkage (–NH–CO–), elucidated by the conjugation of N-hydroxysuccinimide (NHS)-terminated silver nanoparticles and the amino group of glucosamine. Antimicrobial experiments with well-characterized silver nanoparticles (AgNPs) and glucosamine-functionalized silver nanoparticles (GlcN-AgNPs) demonstrate that GlcN-AgNPs have similar and enhanced minimum inhibitory concentration (MIC) against eight gram-negative and eight gram-positive bacteria compared with AgNPs. MIC data shows that Klebsiella pneumoniae (ATCC 700603) and Bacillus cereus isolate express high levels of inhibition, with the quantity and magnitude of inhibition being higher in the presence of GlcN-AgNPs.     

Phyto-Functionalized Silver Nanoparticles Derived from Conifer Bark Extracts and Evaluation of Their Antimicrobial and Cytogenotoxic Effects

Silver nanoparticles synthesized using plant extracts as reducing and capping agents showed various biological activities. In the present study, colloidal silver nanoparticle solutions were produced from the aqueous extracts of Picea abies and Pinus nigra bark. The phenolic profile of bark extracts was analyzed by liquid chromatography coupled to mass spectrometry. The synthesis of silver nanoparticles was monitored using UV-Vis spectroscopy by measuring the Surface Plasmon Resonance band. Silver nanoparticles were characterized by attenuated total reflection Fourier transform infrared spectroscopy, Raman spectroscopy, dynamic light scattering, scanning electron microscopy, energy dispersive X-ray and transmission electron microscopy analyses. The antimicrobial and cytogenotoxic effects of silver nanoparticles were evaluated by disk diffusion and Allium cepa assays, respectively. Picea abies and Pinus nigra bark extract derived silver nanoparticles were spherical (mean hydrodynamic diameters of 78.48 and 77.66 nm, respectively) and well dispersed, having a narrow particle size distribution (polydispersity index values of 0.334 and 0.224, respectively) and good stability (zeta potential values of −10.8 and −14.6 mV, respectively). Silver nanoparticles showed stronger antibacterial, antifungal, and antimitotic effects than the bark extracts used for their synthesis. Silver nanoparticles obtained in the present study are promising candidates for the development of novel formulations with various therapeutic applications.     

A new,simple, green,and one-pot four-component synthesis of bare and poly(α,γ,<Emphasis Type="SmallCaps">l</Emphasis>-glutamic acid)-capped silver nanoparticles

A simple and green chemical method has been developed to synthesize stable bare and capped silver nanoparticles based on the reduction of silver ions by glucose and capping by poly(α,γ,l-glutamic acid) (PGA). The use of ammonia during synthesis was avoided. PGA has had a dual role in the synthesis and was used as a capping agent to make the silver nanoparticle more biocompatible and to protect the nanoparticles from agglomerating in the liquid medium. The synthesized PGA-capped silver nanoparticles in the size range 5–45 nm were stable over long periods of time, without signs of precipitation. Morphological examination has shown that the silver nanoparticles had a nearly spherical, multiply twinned structure. The effects of the reaction temperature and the reaction time during the synthesis were investigated too. The biocompatibility of the PGA-capped silver nanoparticles is discussed in terms of in vitro toxicity with human intestinal Caco-2 cells. The samples were characterized by UV–Visible spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, and zeta potential measurements.     

Thermal,physicochemical and microstructural studies of binary organic eutectic systems

Solid–liquid phase equilibrium data of three binary organic systems, namely, 3-hydroxybenzaldehyde (HB)—4-bromo-2-nitroanilne (BNA), benzoin (BN)—resorcinol (RC) and urea (U)—1,3-dinitrobenzene (DNB), were studied by the thaw–melt method. While the former two systems show the formation of simple eutectic, the third system shows the formation of a monotectic and a eutectic with a large immiscibility region where two immiscible liquid phases are in equilibrium with a liquid of single phase. Growth kinetics of the pure components, the monotectic and the eutectics, studied by measuring the rate of movement (v) of solid–liquid interface in a thin U-tube at different undercoolings (ΔT) suggests the applicability of the Hillig–Turnbull’s equation: v = u (ΔT) ⁿ , where v and n are the constants depending on the nature of the materials involved. The thermal properties of materials such as heat of mixing, entropy of fusion, roughness parameter, interfacial energy, and excess thermodynamic functions were computed from the enthalpy of fusion values, determined by differential scanning calorimeter (Mettler DSC-4000) system. The role of solid–liquid interfacial energy on morphologic change of monotectic growth has also been discussed. The microstructures of monotectic and eutectics were taken which showed lamellar and federal features.     

Synthesis on an ultra large scale of nearly monodispersed γ-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles with La(III) doping through a sol–gel route assisted by propylene oxide

Nearly monodispersed La³⁺ doped γ-Fe₂O₃ nanoparticles were synthesized on an ultra-large scale of about 60 g in a single reaction by a low temperature sol–gel route. The nanoparticles were obtained by the reaction of FeCl₂ and La(NO₃)₃ in ethanol solution with propylene oxide to form the sol, followed by the boiling of the sol solution. The La³⁺ doping promotes the phase transformation temperature of γ-Fe₂O₃ nanoparticles from 350 to 650 °C by the La³⁺ doping induced enhancement of phase transformation activation energy. This large scale synthesis strategy offers important advantages over other conventional routes for the preparation of undoped and doped γ-Fe₂O₃ nanoparticles. These guarantee the promising application of this route in the industrial production.     

Nanosilver resonance scattering spectral method for determination of hydroxyl radical and its application

Silver nanoparticles were prepared under a microwave high-pressure condition using citric acid sodium as a reducer while the excess citrate was removed under high speed centrifugation. There is a resonance scattering (RS) peak at 470 nm for silver nanoparticles. In a pH 4.0 HAc-NaAc buffer solution, hydroxyl radicals from the Fenton reaction can oxidize silver nanoparticles to Ag , resulting in the RS intensity decreasing. The decreased RS intensity at 470 nm (△I 470 nm) is linear with respect to the concentration of H2O2 (C) in the range of 0.27-7.56 μmol/L with a detection limit of 0.23 μmol/L. Its regression equation is △I 470 nm = 24.3 C 13.8 with a correlation coefficient of 0.9959. This method was applied to screening the antioxidants with satisfactory results.     

Stripping chronopotentiometric analysis of cysteine on nano-silver coat polyquercetin–MWCNT modified platinum electrode

Silver nanoparticles coat polyquercetin (Qu) and multi-walled carbon nanotube (MWCNT) complex films were prepared using an electrochemical coupling strategy on platinum electrode (Ag/Qu/MWCNT/Ch/Pt). The new composite material was characterized by means of field emission scanning electron microscopy, X-ray photoelectron spectroscopy spectra, X-ray diffraction, and electrochemical techniques, which confirmed that polyquercetin plays an important role to obtain a great deal of uniformly dispersed silver nanoparticles and MWCNT complex film with a diameter of 10 ± 6 nm. The resulting Ag/Qu/MWCNT/Ch/Pt electrode shows a significant electrocatalysis for the redox of cysteine (CysH). The stripping chronopotentiometric analysis of CysH has been successfully used with a satisfying effect. A linear range of 1 × 10⁻¹⁰ to 9 × 10⁻⁸ M was obtained with a detection limit of 3 × 10⁻¹¹ M (3σ) and sensitivity of 35 μA/nM. The films were also robust, surviving up to 100 consecutive cyclic voltammograms and sonication.     

Synthesis and characterisation of silver nanoparticles in viscous solvents and its transfer into non-polar solvents

Room temperature synthesis of silver nanoparticles has been successfully achieved by adding NaOH acting as an accelerator for the reduction of silver ions in ethylene glycol and glycerol without adding any external reducing agent. Highly monodisperse silver particles are obtained in the presence of various stabilisers such as PVP, SiO₂ and SDS. Nanoparticles with a mean diameter of 25 nm and a mean deviation of 2 nm could be obtained under experimental conditions. The silver nanoparticles so obtained could be easily transferred to chloroform containing CTAB, giving rise to CTAB stabilised silver nanoparticles having sizes of around 25 nm. The newly found role of OH⁻ stabilisation was used to formulate a mechanism for the formation of silver nanoparticles in ethylene glycol and glycerol. In this mechanism, silver nanoparticles are stabilised in ethylene glycol by the adsorbed OH⁻ ions.     

Biosynthesis of Silver Nanoparticles by <Emphasis Type="Italic">Geotricum</Emphasis> sp.

Nanoparticles are usually 1–100 nm in each spatial dimension considered as building blocks of the next generation of optoelectronics, electronics, and various chemical and biochemical sensors. In the synthesis of nanoparticles use of microorganisms emerges as an eco-friendly and exciting approach that reduce waste products (ultimately leading to atomically precise molecular manufacturing with zero waste); the use of nanomaterials as catalysts for greater efficiency in current manufacturing processes by minimizing or eliminating the use of toxic materials (green chemistry principles); the use of nanomaterials and nanodevices to reduce pollution (e.g. water and air filters); and the use of nanomaterials for more efficient alternative energy production (e.g. solar and fuel cells). Fungi have many advantages for nanoparticle synthesis compared with other organisms. In this study, Geotricum sp. found to successfully produce Ag nanoparticles. Geotricum sp. was grown in SDA (Sabro Dextrose Agar) medium at 25 ± 1 °C for 96 h. The mycelia were used to convert silver nitrate solution into nano-silver. Silver nanoparticles were synthesized using these fungi (Geotricum sp.) extracellularly. UV–VIS spectroscopy, Atomic Force Microscopy (AFM) and Scanning Electron Microscopy images shows the nanoparticle formation in the medium. Energy-dispersive X-ray spectroscopy (EDX) also confirmed that silver nanoparticles in the range of 30–50 nm were synthesized extracellularly. FTIR analyses confirmed the presence of amide (I) and (II) bands of protein as capping and stabilizing agent on the surface of nanoparticles.     

Sol–gel synthesis of nanosilver embedded hybrid materials using combined organosilica precursors

A facile sol–gel route to the fabrication of size-controllable nanosilver embedded hybrid materials at room-temperature is presented. The preparation process involves using three kind of organosilica precursors, i.e. tetraethoxysilane, 3-mercaptopropyltrimethoxysilane and polymethylhydrosiloxane, which behaved as framework constructor, complexing agent toward metal ions and in situ reducing agent for Ag⁺ ions, respectively, under alcohol-rich synthesis conditions. The prepared hybrid materials were characterized by Ultraviolet–visible diffuse reflectance spectra, Fourier transform infrared, transmission electron microscopy, X-ray diffraction, nitrogen adsorption–desorption measurements. It was shown that well-dispersed silver nanoparticles (AgNPs) with small particle size were successfully embedded in the hybrid skeleton, and the mean particle size of AgNPs could be controlled at ca. 2–5 nm.     

Silver containing sol–gel derived silica thin films: effect of aluminum incorporation on optical,microstructural and bactericidal properties

Silver containing silica (Ag–SiO₂) thin films with and without aluminum (Al) were prepared on soda-lime-silica glass by spin coating of aqueous sols. The coating sol was formed through mixing tetraethyl orthosilicate [Si(OC₂H₅)₄]/ethanol solution with aqueous silver nitrate (AgNO₃) and aluminum nitrate nonahydrate [(AlNO₃)₃·9H₂O] solutions. The deposited films were calcined in air at 100, 300 and 500 °C for 2 h and characterized using x-ray diffraction, UV-visible and x-ray photoelectron spectroscopy. The effect of Al incorporation and calcination treatment on microstructure and durability of the films, and chemical/physical state of silver in the silica thin film have been reported. The bactericidal activity of the films was also determined against Staphylococcus aureus via disk diffusion assay studies before and after chemical durability tests. The investigations revealed that the optical, bactericidal properties and chemical durability of Ag–SiO₂ films can be improved by Al addition. The Al-modified Ag–SiO₂ thin films do not exhibit any coloring after calcination in the range of 100–500 °C, illustrating that silver is incorporated within the silica gel network in ionic form (Ag⁺). Al incorporation also improved the overall durability and antibacterial endurance of Ag–SiO₂ thin films.     

Biosynthesis of silver nanoparticle using flowers of Calotropis gigantea (L.) W.T. Aiton and activity against pathogenic bacteria

Silver nanoparticles (AgNPs) from silver nitrate solution are carried out using the flower extract of Calotropis gigantea. Silver nanoparticles were characterized by UV–vis spectrophotometer, X-Ray diffractometer (XRD). Reduction of silver ions in the aqueous solution of silver during the reaction was observed by UV–vis spectroscopy. Crystalline nature of synthesized silver nanoparticles was studied by XRD pattern, refraction peak using the Scherrer’s equation. Antibacterial activity of the silver nanoparticles was performed by disc diffusion method against Bacillus subtilis, Pseudomonas putida and Escherichia coli. The antibacterial activity of synthesized silver nanoparticles by flower extract of C. gigantea was found against B. subtilis (10 mm). Synthesised AgNPs has the efficient antibacterial activity against Gram positive bacteria.