Gold nanoparticles–graphene hybrids as active catalysts for Suzuki reaction

Graphene was successfully modified with gold nanoparticles in a facile route by reducing chloroauric acid in the presence of sodium dodecyl sulfate, which is used as both a surfactant and reducing agent. The gold nanoparticles–graphene hybrids were characterized by high-resolution transmission electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, X-ray diffraction and energy X-ray spectroscopy. We demonstrate for the first time that the gold nanoparticles–graphene hybrids can act as efficient catalysts for the Suzuki reaction in water under aerobic conditions. The catalytic activity of gold nanoparticles–graphene hybrids was influenced by the size of the gold nanoparticles.     

Coriander leaf mediated biosynthesis of gold nanoparticles

Extracellular biological synthesis of gold nanoparticles was achieved by a simple biological procedure using coriander extract as the reducing agent. The aqueous gold ions when exposed to coriander leaf extract are reduced and resulted in the biosynthesis of gold nanoparticles in the size range from 6.75-57.91 nm. The gold nanoparticles were characterized by UV-Vis spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), fourier transform infra-red spectroscopy (FT-IR) and transmission electron microscopy (TEM). This eco-friendly approach for the synthesis of nanoparticles is simple, amenable for large scale commercial production and technical applications.     

Ag_2S纳米粒子的合成与表征

以油酸钠为表面活性剂、硝酸银和硫脲为反应物,在甲苯-水两相界面处合成了Ag_2S纳米粒子。采用紫外-可见吸收光谱(UV-Vis)、透射电子显微镜(TEM)和广角X射线衍射(WAXD)等方法对Ag_2S纳米粒子的光学性质、形貌及晶体结构进行了表征。结果表明,通过改变甲苯-水两相界面反应体系的条件,可以得到粒子尺寸窄分布的Ag_2S纳米粒子;WAXD测定表明所合成的Ag_2S纳米粒子具有单斜结构。     

Modeling of Silver Nanoparticle Synthesis in Ternary Reverse Microemulsion of Cyclohexane/Water/SDS

In the present study, a simple mathematical model has been developed for synthesis of silver nanoparticles. The silver nanoparticles have been synthesized in ternary reverse microemulsion of cyclohexane/water/sodium dodecyl sulfate (SDS). The silver nanoparticles were produced by reaction between silver nitrate in the water droplet core of one microemulsion and hydrazine as reducing agent in the water droplet core of another microemulsion. The dynamic behavior of process was modeled on mass balance equations which were solved using the finite difference method. The kinetic parameters of the critical number size (N _crit ), rate order of nucleation, and growth constants were estimated by minimizing the difference between the average particle size predicted by model and those obtained by experiments. The UV-Vis absorption spectra, transmission electron microscopy (TEM), x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), and dynamic light scattering (DLS) were used to analyze the structure and particle size distribution of silver nanoparticles.     

Novel phase-transfer preparation of monodisperse silver and gold nanoparticles at room temperature

In a novel water-cyclohexane two-phase system, the aqueous formaldehyde is transferred to cyclohexane phase via reaction with dodecylamine to form reductive intermediates in cyclohexane; the intermediates are capable of reducing silver or gold ions in aqueous solution to form dodecylamine protected silver and gold nanoparticles in cyclohexane solution at room temperature. The prepared silver and gold nanoparticles are examined by transmission electron microscopy (TEM), UV-Visible spectroscopy (UV-vis), X-photon electron spectroscopy (XPS) and Fourier transfer infrared spectroscopy (FT-IR). It is found that these nanoparticles are monodisperse in size of less than 10 nm and have good stability in cyclohexane due to the adsorbed dodecylamine on nanoparticle surface. Moreover, the synthesis mechanism is revealed via gas chromatography (GC), gas chromatography-mass spectroscopy (GC-MS), nuclear magnetic resonance (NMR) analyses of the solutions during the preparation process.     

A facile method to prepare size-tunable silver nanoparticles and its antibacterial mechanism

The antibacterial effect of silver nanoparticles (denoted as Ag NPs) is closely related to size. This could partly explain why size controllable synthesis of Ag NPs for bactericidal application is drawing much attention. Thus, we establish a facile and mild route to prepare size-tunable Ag NPs with highly uniform morphologies and narrow size distributions. The as-prepared Ag NPs with averaged sizes of 2, 12 and 32?nm were characterized by transmission electron microscopy (TEM), ultraviolet–visible absorption spectroscopy (UV–vis), X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The antimicrobial effect of the as-prepared Ag NPs with different particles size was assessed by broth dilution and disk diffusion as well as measurement of optical density (OD₆₀₀). Moreover, their antibacterial mechanism was discussed in relation to morphology observation of microorganism by scanning electron microscopy (SEM) and to concentration detection of Ag⁺ by stripping voltammetry. It was found that the parameters such as reactant molar ratio, reaction time, dropping speed, and most of all, pH of the reactant solutions, have significant influences on size-regulation of Ag NPs. The as-prepared Ag NPs exhibit excellent antibacterial properties, and their antimicrobial activities increase with decreasing particles size. Besides, two kinds of mechanisms, i.e., contact action and release of Ag⁺, are responsible for the antimicrobial effect of Ag NPs.     

pH effect on the aggregation of silver nanoparticles synthesized by chemical reduction

Silver colloidal nanoparticles were prepared according to the chemical reduction method in which the ascorbic acid was used as a reducing agent and sodium citrate as a stabilizing agent. The absorption spectra of all prepared samples obtained using the UV-Vis spectrophotometer showed a surface plasmon peak at a wavelength of about 420 nm. The size of the silver nanoparticles was controlled by changing the pH values of the reaction system. At high pH, smaller size silver nanoparticles were obtained compared to low pH values. This difference can be attributed to the difference in the reduction rate of the precursor. In addition to the inverse proportionality between the size and the pH value it is clear that increasing the pH value enables us to obtain spherical nanoparticles while at low pH, rods and triangular particle shapes were formed. Poor balance between nucleation and growth processes could be the cause of this result.     

Synthesis and characterization of nano-gold composite using Cylindrocladium floridanum and its heterogeneous catalysis in the degradation of 4-nitrophenol

Greener synthesis of nanogold-biocomposite by fungus, Cylindrocladium floridanum was reported in this study. Results revealed that when cultured in static condition for a period of 7d, the fungus accumulated gold nanoparticles on the surface of the mycelia. Bionanocomposites with Au nanocrystals were characterized by UV-Vis spectroscopy, XRD, SEM, EDX and high-resolution TEM. The SPR band of UV-Vis spectrum at 540 nm confirmed the presence of gold nanoparticles on the surface of the fungal mycelia. The fcc (111)-oriented crystalline nature of particles was identified by XRD pattern. The synthesized particles are spherical in shape as evidenced by TEM image. The biocomposites with Au nanoparticles function as an efficient heterogeneous catalyst in the degradation of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP), in the presence of reducing agent, sodium borohydride which was reflected by UV-Vis spectra of the catalytic reaction kinetics. The reduction of 4-nitrophenol follows pseudo-first-order kinetic model with the reaction rate constant of 2.67 × 10(-2)min(-1) with 5.07 × 10(-6)mol/dm(3) of gold at ca. 25 nm. The rate of the reaction was increased by increasing the concentration of gold nanoparticles from 2.54 × 10(-6) to 12.67 × 10(-6)mol/dm(3) (～ 25 nm) and with reduced size from 53.2 to 18.9 nm respectively. This is the first report on fungal-matrixed gold(0) nanocomposites heterogeneously catalyzing the reduction of the toxic organic pollutant, 4-nitrophenol that enable the recovery and recycling of AuNPs catalysts.     

Biological synthesis of gold and silver nanoparticles mediated by the bacteria Bacillus subtilis

Biological synthesis of gold and silver nanoparticles was carried out using the bacteria Bacillus subtilis. The reduction processes of chloroaurate and silver ions by B. subtilis were found to be different. Gold nanoparticles were synthesized both intra- and extracellularly, while silver nanoparticles were exclusively formed extracellularly. The gold nanoparticles were formed after 1 day of addition of chloroaurate ions, while the silver nanoparticles were formed after 7 days. The nanoparticles were characterized by X-ray diffraction, UV-vis spectra and transmission electron spectroscopy. X-ray diffraction revealed the formation of face-centered cubic (fcc) crystalline gold nanoparticles in the supernatant, broth solution and bacterial pellet. Silver nanoparticles also exhibited diffraction peaks corresponding to fcc metallic silver. UV-vis spectra showed surface plasmon vibrations for gold and silver nanoparticles centered at 530 and 456 nm, respectively. TEM micrographs depicted the formation of gold nanoparticles intra- and extracellularly, which had an average size of 7.6 +/- 1.8 and 7.3 +/- 2.3 nm, respectively, while silver nanoparticles were exclusively formed extracellularly, with an average size of 6.1 +/- 1.6 nm. The bacterial proteins were analyzed by sodium dodecyl sulfonate-polyacrylamide electrophoresis (SDS-PAGE) before and after the addition of metal ion solutions. We believe that proteins of a molecular weight between 25 and 66 kDa could be responsible for chloroaurate ions reduction, while the formation of silver nanoparticles can be attributed to proteins of a molecular weight between 66 and 116 kDa. We also believe that the nanoparticles were stabilized by the surface-active molecules i.e., surfactin or other biomolecules released into the solution by B. subtilis.     

In-situ preparation of binary-phase silver nanoparticles at a high Ag+ concentration

Stable and monodisperse silver nanoparticles (NPs) have been synthesized using high metal salt concentration (up to 0.735 M) through a simple but novel technique. It is based on one-step procedure that uses glycerol for reducing Ag+ in the presence of o-phenylenediamine (o-PDA) resulting the nanoparticles are in two forms (one water-soluble, the other a precipitated). The water-soluble phase contains NPs that have a bimodal size distribution (2-3 and 5-6 nm); the other comprises precipitated NPs, having a unimodal size distribution (2-3 nm). The water-soluble NPs are covalently bonded to the aromatic amine molecules to form isolated units, while the precipitated nanoparticles are embedded in the networks formed by cross-linking between COOH groups of hydroxypyruvic acid (oxidized form of glycerol) and NH2 groups of o-PDA molecules. We used transmission electron microscopy (TEM), UV-Vis spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) to characterize the silver products obtained.     

合成工艺对水相合成金纳米颗粒的影响

分别采用柠檬酸三钠和硼氢化钠为还原剂在水相中还原氯金酸制备了稳定的金纳米溶胶。通过透射电子显微镜、激光粒度分析仪、紫外-可见分光光度计对所制备的金纳米颗粒的形貌、结构、粒度分布以及光学特性进行表征,研究了还原剂用量、加热反应时间、反应温度、pH值对水相制备金纳米颗粒的影响。结果表明通过调节合成工艺,可以实现金纳米颗粒的可控生长,制备出平均粒径在5～70nm粒度分布均匀的球形金纳米颗粒。     

室温条件下纳米银的温和制备和形貌调控

目的 探究室温条件下不同还原剂以及其他实验助剂在化学还原纳米银过程中对其颗粒粒径、尺寸分布和形貌的影响。方法 以抗坏血酸为还原剂,聚乙烯吡咯烷酮（PVP）为分散剂,柠檬酸钠为保护剂和第2还原剂,选择葡萄糖和硼氢化钠作对照,在室温下通过化学还原的方法来制备纳米银颗粒。通过马尔文激光粒度仪、紫外–可见光谱（UV–vis）、透射电镜（TEM）等对所制备纳米银进行表征。结果 采用抗坏血酸作为还原剂时,通过调控抗坏血酸体积（0.2 mL）,固定柠檬酸钠和PVP体积分别为0.5、0.6 mL,制备出粒径较小（平均粒径为56 nm）且尺寸分布较均一的球形纳米银;采用葡萄糖和硼氢化钠作还原剂时纳米银颗粒尺寸过大（平均粒径分别为216nm和189nm）。结论 采用抗坏血酸作为还原剂,调控柠檬酸钠、PVP等实验参数在最佳范围,更容易制备出球形度好、粒径小的均匀纳米银溶液。     

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。     

Nanoparticles-aided silver front contact paste for crystalline silicon solar cells

High-dispersive spherical silver nanoparticles were prepared by solvothemal process, using ethylene glycol as solvent and reducing agent. The silver nanoparticles were characterized by X-ray diffraction and FESEM to analyze the size, shape and morphology. X-Ray diffraction (XRD) pattern indicated that the silver nanoparticles were well-crystallized with no crystallographic impurities. The average size calculated by Debye–scherrer’s fomula was 48 nm, which well agreed with the result of FESEM. From the FESEM, it was demonstrated that the silver nanoparticles were high-dispersive and spherical in shape. Thick silver films were prepared by screen-printing using the front contact silver paste containing the as-prepared silver nanoparticles. The experimental results indicated that the silver nanoparticles were favor to sintering of micro-size silver particles, and contributed to improve the photovoltaic performances of crystalline silicon solar cells.     

Structure and Properties of Chemically-reduced Functionalized Graphene Oxide Platelets

Green reduction of graphene oxide(GO) functionalized with 3-aminopropyltriethoxysilane and 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride/N-hydroxysuccinimide was performed by using ascorbic acid and sodium bisulfite.The obtained materials were characterized by thermo-gravimetric analysis,transmission electron microscopy.X-ray diffraction,UV-Vis,Fourier transform infrared and Raman spectroscopy techniques.The results indicated a strong dependence of the materials properties such as deoxygenation degree,absorption peak shift,crystallite size and functionalization degree on the functionalization approach and reducing agent.     

Antimicrobial active silver nanoparticles and silver/polystyrene core-shell nanoparticles prepared in room-temperature ionic liquid

Uniform silver nanoparticles and silver/polystyrene core-shell nanoparticles were successfully synthesized in a room temperature ionic liquid, 1-n-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]·BF₄). [BMIM]·BF₄ plays a protective role to prevent the nanoparticles from aggregation during the preparation process. Transmission electron micrographs confirm that both silver nanoparticles and core-shell nanoparticles are regular spheres with the sizes in the range of 5–15 nm and 15–25 nm, respectively. The X-ray diffraction analysis reveals the face-centered cubic geometry of silver nanoparticles. The as-prepared nanoparticles were also characterized by Fourier transform infrared spectroscopy, Raman spectroscopy, UV–vis diffuse reflectance spectroscopy and X-ray photoelectron spectroscopy. In addition, antimicrobial activities against E. coli and S. aureus were studied and the results show that both silver nanoparticles and core-shell nanoparticles possess excellent antimicrobial activities. The antimicrobial mechanism of the as-prepared nanoparticles was discussed.     

One step synthesis of rutile TiO2 nanoparticles at low temperature

Sphere-like rutile TiO2 nanocrystals have been synthesized by sol-gel method followed by hydrolysis of titanium tetrachloride in deionized water in the presence of ammonium hydroxide as hydrolysis catalyst. The as-prepared TiO2 nanoparticles have single rutile phase with average diameter approximately 26.4 nm. The results show that the temperature has a great influence on the particle size distribution and also crystalline phase (rutile) of TiO2 nanoparticles is consistent with the temperature. Characterization of the as-prepared nanocrystalline powder was carried out by different techniques such as powder X-ray diffraction (XRD), field emission transmission electron microscopy (FE-TEM) and Raman spectroscopy.     

Ammonium bicarbonate reduction route to uniform gold nanoparticles and their applications in catalysis and surface-enhanced Raman scattering

A new protocol for the synthesis of nearly monodisperse gold nanoparticles with controllable size is described. The pathway is based on the reduction of AuCl₄⁻ by ammonium bicarbonate in the presence of sodium stearate under hydrothermal conditions. The particle sizes could be easily tuned by regulating the reaction conditions including precursor concentration, reaction temperature and growth time. A tentative explanation for the reduction and growth mechanism of uniform gold nanoparticles has been proposed. The as-prepared gold particles showed good catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol by excess NaBH₄, and a surface-enhanced Raman scattering (SERS) study suggested that the gold nanoparticles exhibited a high SERS effect on the probe molecule Rhodamine 6G.      

Bio-synthesis of gold and silver nanoparticles from Candida guilliermondii and their antimicrobial effect against pathogenic bacteria

In the present study we investigated the extra cellular synthesis of gold and silver nanoparticles by using the yeast Candida guilliermondii. The formation of noble metal nanoparticles was monitored by the UV-Visible spectroscopy. As prepared gold and silver nanoparticles showed distinct surface plasmon peaks at 530 nm and 425 nm respectively. Phase and morphology of the as synthesized materials were investigated by X-ray diffraction and electron microscopy techniques respectively. XRD patterns confirmed the formation of gold and silver nanoparticles with face centered cubic structures. Bio-TEM images showed the formation of near spherical, well dispersed gold and silver nanoparticles in the size range of 50-70 nm and 10-20 nm respectively. The biosynthesized nanoparticles were tested for their antimicrobial activity against five pathogenic bacterial strains. The highest efficiency for both gold and silver nanoparticles was observed against Staphylococcus aureus. A comparative study was also done to find the effect of chemically synthesized noble metal nanoparticles against the above test strains. Chemically synthesized particles had no antimicrobial activity against any of the pathogenic strains. The results obtained suggest that biosynthesized gold and silver nanoparticles can be used as effective antimicrobial agents against some of the potential harmful pathogenic microorganisms.     

A study on gold nanoparticle synthesis using oleylamine as both reducing agent and protecting ligand

The growth kinetics and mechanism of a gold nanoparticle synthesis using water as a single phase solvent and oleylamine as both reducing agent and monolayer protection agent were studied. FT-IR and 1H NMR spectroscopic analysis revealed a conversion of oleylamine ligands to oleylamides when gold(III) was reduced to gold(I) and gold atoms. During the reaction, it was found by UV-Vis absorption spectroscopy and transmission electron microscopic study that oleylamine ligands formed large complex aggregates with gold salt instantly upon mixing these two agents together. At an elevated temperature of 80 degrees C, the complex decomposed first into very small particles and then the small particles recombined together into larger and thermally stable particles with an average core size around 9-10 nm. The oleylamide ligands formed a protecting monolayer around the nanoparticles through a hydrogen bonding network between the amide groups. The recombination of small particles into larger ones was found to follow a logistic model, as confirmed by a nonlinear regression fitting of the UV-Vis absorption data of the reaction solution with the mathematical model.