Dendronization of gold and CdSe/cdS (core-shell) quantum dots with tomalia type, thiol core, functionalized poly(amidoamine) (PAMAM) dendrons

Poly(amidoamine) (PAMAM) dendrimers containing disulfide cores (i.e., cystamine) and possessing carboxylic acid or hydroxyl terminal groups were reduced with dithiothreitol (DTT) to yield single site, thiol core, functionalized PAMAM dendron reagents. These thiol functionalized dendron reagents were used to surface modify (dendronize) both gold nanoparticles, as well as CdSe/CdS (core-shell) quantum dots (QDs). Dendronization involved self-assembly of the focal point thiol functional dendrons at the metal interface of both gold and CdSe/CdS QDs by ligand exchange of protective surfactants used for their synthesis. The synthesis, characterization and preliminary luminescence studies of these new dendritic hybrids are reported.     

Formation and spectroscopic characterization of mono-dispersed CdSe nanocrystals

In this article, mono-dispersed hexagonal structure CdSe nanocrystals with polyhedron shape were prepared by an open solvent thermal reaction. They show a discrete excitonic transition structure in the absorption spectra and the minimal photoluminescence （PL） peak full-width at half-maximum of 19nm. The PL quantum yield is about 60%. Transmission electron micrographs, high-resolution transmission electron micrographs, x-ray powder diffraction patterns, UV-vis absorption spectra and PL spectra were obtained for the as-prepared CdSe nanocrystals. The size of the CdSe nanocrystals can be tuned by changing the reaction temperature or time. Due to the improved synthesis method, a different growth mechanism of the CdSe nanocrystals is discussed.     

Laser pyrolysis synthesis and characterization of luminescent silicon nanocrystals

Quantum dots of silicon are very attractive materials due to their photoluminescence (PL) emission that can be very strong at room temperature in the visible range under UV illumination. Weighable batches are demanded for several applications in opto-electronic, photovoltaic, medicine, and so on. Laser pyrolysis of silane in a flow reactor is an efficient method to synthesize silicon nanocrystals, but up to now the production rate for the smallest particles was very low. We present here results of a work aimed to overcome this limitation. Optimization of the laser pyrolysis process has been performed through an elaborate study of the synthesis parameters. Weighable batches of very small silicon particles were obtained in a controlled and reproducible way, with production rate in the 0.1–1 g/h. High-resolution electron microscopy and specific surface measurements show that the particles were true silicon nanocrystals in the 4–9 nm range. We have then studied their PL properties. For this purpose, we have paid a particular attention to the surface passivation, an essential step to obtain efficient PL. Various ways were explored: natural oxidation under air and dispersion in liquids. We show that after natural oxidation, the PL properties are, as expected, in agreement with the quantum confinement model. Strong PL is also obtained by dispersion in solvents, but the interpretation is less straightforward in this case, and as discussed in the paper, needs further investigation.     

Synthesis and characterization of nanocomposites films with graphene oxide and reduced graphene oxide nanosheets

Graphene oxide (GO) and reduced graphene oxide (CRGO), as a graphene derivatives, possess unique properties and a high aspect ratio, indicating great potential in nanocomposite fields. The present work reports the fabrication of the nanocomposite films by a simple and environmentally friendly process using aqueous solution and optimized time sonication for better exfoliation of the graphene sheets within Poly(Vinyl alcohol) (PVA) as matrix. The films were characterized using high-resolution TEM (HRTEM), X-ray diffraction (XRD), Microtensile testing, Differential scanning calorimetry (DSC) and Thermogravimetric analysis (TGA). The TEM images revealed a successfully exfoliation of the GO/CRGO nanosheets. XRD combined with TGA and DSC measurements showed an improvement in the thermal stability and tunable thermal properties. In addition, the Young's modulus and tensile yield strength of the composite films containing 1 wt% GO were obtained to be 4.92 GPa and 66 MPa respectively. These excellent reinforcement effects were achieved by the strong interaction between the components.     

Synthesis and characterization of chemically anchored adenosine with PHEMA grafted gold nanoparticles

The synthesis of chemically anchored adenosine with biocompatible poly(2-hydroxylethyl methacrylate) grafted gold nanoparticles (Ado-i-PHEMA-g-AuNPs) was realized by employing a simple strategy. Disulfide-containing poly(2-hydroxylethyl methacrylate) (DT-PHEMA) was initially synthesized by atom transfer radical polymerization (ATRP). The formation of DT-PHEMA was confirmed by ¹H-NMR and FT-IR. The molecular weight and molecular weight distribution were found to be 9.6 kg/mol and 1.40 from GPC analysis. DT-PHEMA was subsequently used for the synthesis of PHEMA-g-AuNPs by a grafting to protocol. The grafting of DT-PHEMA on the surface of AuNPs was confirmed by FT-IR, TGA, XPS, and EDX analyses. The particle size of the PHEMA-g-AuNPs was found to be ca. 5.0 nm from HR-TEM analysis. Boronic acid was used for functionalization of PHEMA-g-AuNPs, which was then subjected for covalent immobilization with adenosine via strong interaction between free hydroxyl groups of adenosine and boronic acid. Characterization and properties of the Ado-i-PHEMA-g-AuNPs were investigated by taking advantage from FT-IR, XPS, EDX, and UV-visible spectroscopy. The Ado-i-PHEMA-g-AuNPs nanocomposite exhibits a surface plasmon resonance peak at 586 nm which is red shifted from AuNPs (521 nm), indicating significant changes of surface property upon PHEMA-adenosine immobilization onto the surface of AuNPs.     

Phase transitions and kinetic properties of gold nanoparticles confined between two-layer graphene nanosheets

The thermodynamic and kinetic behaviors of gold nanoparticles confined between two-layer graphene nanosheets (two-layer-GNSs) are examined and investigated during heating and cooling processes via molecular dynamics (MD) simulation technique. An EAM potential is applied to represent the gold–gold interactions while a Lennard–Jones (L–J) potential is used to describe the gold–GNS interactions. The MD melting temperature of 1345 K for bulk gold is close to the experimental value (1337 K), confirming that the EAM potential used to describe gold–gold interactions is reliable. On the other hand, the melting temperatures of gold clusters supported on graphite bilayer are corrected to the corresponding experimental values by adjusting the ε_Au–C value. Therefore, the subsequent results from current work are reliable. The gold nanoparticles confined within two-layer GNSs exhibit face center cubic structures, which is similar to those of free gold clusters and bulk gold. The melting points, heats of fusion, and heat capacities of the confined gold nanoparticles are predicted based on the plots of total energies against temperature. The density distribution perpendicular to GNS suggests that the freezing of confined gold nanoparticles starts from outermost layers. The confined gold clusters exhibit layering phenomenon even in liquid state. The transition of order–disorder in each layer is an essential characteristic in structure for the freezing phase transition of the confined gold clusters. Additionally, some vital kinetic data are obtained in terms of classical nucleation theory.     

单原子层FeS半导体纳米片及其光催化还原二氧化碳应用

采用简单的溶剂热法制备了厚度约为1.16 nm单层超薄FeS纳米片,其具有涵盖从近紫外至近红外的太阳光谱波段的优异光学吸收性能和干净均一的表面,显微图像显示其具有超薄的片状结构,晶面结构清晰,物相测定证实合成的超薄FeS纳米片为单硫铁矿相,物性测定及理论计算显示超薄FeS纳米片具有半导体的电子能带结构,电子迁移率高,全光谱光催化CO₂还原到CO的产率约为260μmol·g^-1·h^-1,且具有很好的光催化稳定性,该研究为地球储量丰富的铁基材料应用于能源转化领域提供了可行的方向.     

Preparation and characterisation of CoS2 nanomaterial in aqueous cationic surfactant medium of cetyltrimethylammonium bromide (CTAB)

Cobalt disulfide is an important nanomaterial in the field of material chemistry due to its interesting catalytic and electromagnetic properties. We herein report the simple solution phase preparation of nanoparticles of cobalt disulfide in micellar medium of cationic surfactant cetyltrimethylammonium bromide (CTAB) and also by way of capping with thiophenol. The product has been characterized using spectroscopic and electron microscopic and magnetic moment measurements. The presence of disulfide bond is clearly evident from the 480 cm⁻¹ peak in the infrared spectrum. The thiol passivated particles prepared in aqueous and ethanol medium has been found to have different compositions as observed from the ESIMS study.     

Synthesis, characterization, and ion-exchange properties of colloidal zeolite nanocrystals

Here, we present physical–chemical properties of Linde type A (LTA) zeolite crystals synthesized via conventional hydrothermal and microwave heating methods. Both heating methods produced LTA crystals that were sub-micron in size, highly negatively charged, super-hydrophilic, and stable when dispersed in water. However, microwave heating produced relatively narrow crystal size distributions, required much shorter heating times, and did not significantly change composition, crystallinity, or surface chemistry. Moreover, microwave heating allowed systematic variation of crystal size by varying heating temperature and time during the crystallization reaction, thus producing a continuous gradient of crystal sizes ranging from about 90 to 300 nm. In ion-exchange studies, colloidal zeolites exhibited excellent sorption kinetics and capacity for divalent metal ions, suggesting their potential for use in water softening, scale inhibition, and scavenging of toxic metal ions from water.     

Investigation of the surface properties of gold nanowire arrays

Gold nanowire arrays with diameters ranging from 45 to 200 nm were obtained via electrochemical deposition within the ion-track templates. The morphology of gold nanowires was imaged by scanning electron microscopy (SEM). The surface properties were investigated by surface plasmon resonance (SPR) and X-ray photoelectron spectroscopy (XPS). The SPR peaks were observed as the gold nanowire arrays embedded in the templates and their intensity decreased after the sample exposed to the air for a certain time due to the formation of chemisorbed oxygen on nanowire surface. The positive binding energy shifts in Au core level was found when the gold nanowire arrays embodied in template and the initial- and finial-state effects were introduced to explain this phenomenon.     

Synthesis and characterization of PbS nanorods and nanowires

 A surfactant assisted solvotermal approach for the controllable synthesis of PbS nanowires and nanorods is applied. The synthesis is based on decomposition of lead thiocyanate in boiling benzyl alcohol with Cetyl trimethyl ammonium bromide used as a surfactant. Nanowires of PbS (about 2–3 μm with an average diameter of 30–50 nm) and nanorods (200–300 nm in length with an axial ratio of 4–5) were synthesised. The nanostructures were characterized by high resolution transmission electron microscopy (HR-TEM), scanning electron microscopy (SEM), selected area electron diffraction (SAED) and X-ray diffraction analysis. The experimental results indicate that the reaction duration and concentration of surfactant play key roles in determining the final morphologies of PbS blocks building and also in their crystallinity. A possible mechanism for creation of PbS nanowires and nanorods is discussed.     

Synthesis and characterization of brightly photoluminescent CdTe nanocrystals

A new synthesis procedure for the preparation of spherical shaped CdTe nanocrystals (NCs) is presented, exhibiting bright luminescence with exceptionally high quantum efficiency (up to 85%). The growth of these NCs occurs in a non-coordinating solvent, octadecene, with the addition of oleic acid/tri-octylphosphine stabilizers, CdO as a precursor for the Cd monomers and additional Cd metal particles as a supplementary Cd reservoir source. The dependence of the crystalline quality and the optical properties of the CdTe NCs, on the initial Cd:Te precursors’ molar ratio, and the reaction duration were investigated. It was demonstrated that the NCs’ properties improved significantly as the initial Cd:Te molar ratios are increased. The obtained NCs’ properties were correlated with measurements of the Cd⁰ concentration in Cd metal particles, CdTe NCs and in Cd monomer solutions.     

Synthesis,characterization, and toxicity of hollow gold nanoshells

Hollow gold nanoshells (HGN) with a diameter of 50–70 nm and tunable optical properties within the near-infrared region were synthesized from a substitution reaction using a sacrificial template, in which the morphological properties of the HGN were affected by the synthesis conditions. Using EDX line scan, the composition of the structure was determined to verify if the sacrificial template is completely consumed or residues remain after the chemical synthesis, obtaining that the final HGN structure contains about 11% of the remaining silver that showed no significant effect on the cell viability of a hNS1 cell line, but resulted as toxic on a C6 glioma cell line at high concentrations. The photothermal properties were evaluated using a NIR laser, which despite its low power showed the conversion of light into heat. This study was conducted to evaluate the potential of these nanostructures as therapeutic agents with an emphasis on toxicity.     

Thiolated poly(ε-caprolactone) macroligand with vacant coordination sites on gold substrate: Synthesis and surface characterization

Surface-confined telechelic poly(ε-caprolactone) macroligand with two distinct functional groups per polymeric chain has been synthesized and characterized. The molecular microstructure of the macroligand with regard to the properties of the end-capped functionalities and with those on surface substrate has been studied by solution and surface analytical methods (i.e., X-ray photoelectron spectroscopy (XPS), grazing angle reflectance-Fourier transform IR spectroscopy (GA-FTIR), water contact angle measurements, and atomic force microscopy (AFM)) to elucidate the structure and properties of such multifunctional polymer on gold (1 1 1) substrate.     

Preparation and characterization of SnS nanocrystals by a triethanolamine-assisted diethylene glycol solution synthesis

Stoichiometric, phase-controllable SnS nanocrystals (NCs) were prepared by a solution chemical synthesis using triethanolamine-assisted diethylene glycol solvent, tin(II) chloride and thioacetamide as precursors at injection temperature of 180-220 °C. The influences of triethanolamine adding amounts, injection temperature, refluxing time on crystal phase, growth morphology and optical property of the synthesized SnS NCs were investigated. The results showed that both orthorhombic (OR) and zinc-blende (ZB) phase of SnS NCs could be formed by altering triethanolamine amounts.     

Calculation of curvature dependent surface plasmon resonance in gold nanospheroid and nanoshell

In this paper, theoretical calculations based on dipole-limit are performed to investigate the effects of curvature on the surface plasmon resonance (SPR) properties of nanometer size gold spheroid and shell. By comparing the aspect ratio with the shell thickness, we demonstrated that the curvature radius is a common better factor that can be used to predict the SPR wavelength and shift fashion. For nanospheroid, increasing the ratio of curvature radius corresponding to the climaxes leads to an increase in the ratio of SPR wavelength, whereas increasing the ratio of curvature radius of outer and inner surface in nanoshell leads to an decrease in the ratio of SPR wavelength. As a morphologic factor, curvature radius plays an important role in affecting the distribution of electron density, and consequently controlling the SPR frequency.     

磁控溅射法制备金团簇纳米颗粒及性能表征

 采用磁控溅射法制备金团簇纳米颗粒,用透射电镜(TEM)、X射线衍射(XRD)、紫外可见光分光光度计(UV-Vis)和X射线光电子能谱(XPS)等分析手段对其表征,研究了金团簇纳米颗粒的形貌、颗粒度、结构、光吸收性质及物质成份。研究结果表明：制备的金团簇纳米颗粒呈球形,平均粒径在10 nm左右,粒径分布均匀,无团聚、氧化现象,颗粒的结构为面心立方。在519 nm处出现团簇颗粒的表面等离子共振吸收峰,测试得到Au(4f_7/2)和Au(4f_5/2)电子的结合能分别为83.3 eV和86.9 eV,并且没有出现金的氧化产物。     

Synthesis and characterization of hexagonal nano-sized nickel selenide by simple hydrothermal method assisted by CTAB

Nano-sized nickel selenide powders have been successfully synthesized via an improved hydrothermal route based on the reaction between NiCl₂·6H₂O, SeCl₄ and hydrazine (N₂H₄·H₂O) in water, in present of cetyltrimethyl ammonium bromide (CTAB) as surfactant, at various conditions. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and X-ray energy dispersive spectroscopy analysis. Effects of temperature, reaction time and reductant agent on the morphology, the particle sizes and the phase of the final products have been investigated. It was found that the phase and morphology of the products could be greatly influenced by these parameters. The synthesis procedure is simple and uses less toxic reagents than the previously reported methods. Photoluminescence (PL) was used to study the optical properties of NiSe samples.     

Synthesis and optical characterization of vertically grown ZnO nanowires in high crystallinity through vapor-liquid-solid growth mechanism

The gas-phase growth and optical characteristics of 1-dimensional ZnO nanostructure have been investigated. The ZnO nanowires (NWs) were grown vertically on Au coated silicon substrates by vapor-liquid-solid (VLS) growth mechanism using chemical vapor deposition (CVD). The ZnO NWs were grown in the crystal direction of [0 0 0 1]. The ZnO NWs exhibit the uniform size of less than 100 nm in diameter and up to 5 μm in length. Photoluminescence (PL) spectrum of ZnO NWs shows the strong band-edge emission at ∼380 nm (∼3.27 eV) without significant deep-level defect emission. The exciton lifetime of ZnO NWs was measured to be approximately 150 ± 10 ps.     

Fe(Ⅲ)-苯基荧光酮-溴化十六烷基三甲胺显色反应的研究与应用

本文研究了在溴化十六烷基三甲胺存在下，苯基荧光酮与铁的显色反应。试验结果表明，显色的适宜酸度为pH等于7.3至10．5，配合物的摩尔吸光系数为1．09×105L·mol-1·cm-1，铁量在0－6μg·25mL-1范围内符合比耳定律。用于试样中铁的测定，灵敏度高，且简便可靠。