银纳米晶体的制备与表征

在聚乙烯吡咯烷酮存在的条件下,用水合肼还原硝酸银,通过控制反应条件成功制备出了粒径均一、有良好分散性的银纳米微粒,并以此为种子,利用种子诱导生长,在十六烷基三甲基溴化铵的棒状胶束环境中制备出了银纳米棒和纳米线.并用X射线衍射、透射电子显微镜、傅立叶红外光谱和紫外-可见光谱等手段对产品的形貌、结构进行了表征.     

用双还原法制备三角形银纳米片及其光学性能

在硼氢化钠和柠檬酸三钠共存的体系中还原硝酸银, 以聚乙烯吡咯烷酮(PVP)为表面活性剂和保护剂, 水浴加热制备得到三角形银纳米片, 用X射线衍射(XRD)、透射电子显微镜(TEM)、紫外-可见(UV-Vis)吸收光谱、表面增强拉曼散射(SERS)光谱对其进行了表征. 结果表明: 三角形银纳米片产物为立方相金属银, 边长为(100±40) nm, 厚度为(10±5) nm; 产物表现出与球形银纳米粒子完全不同的吸收光谱; 柠檬酸根在银晶核不同晶面的选择吸附、PVP的包覆作用及Ag(111)晶面的层错对产物的形成起决定作用; 与球形纳米颗粒相比, 三角形银纳米片膜对吡啶(Py)分子有显著的SERS活性.     

Microwave-assisted synthesis of high aspect ratio ruthenium nanorods

<正>Poly(N-vinyl-2-pyrrolidone)(PVP)-stabilized ruthenium nanorods with high aspect ratio by refluxing ruthenium(Ⅲ) chloride in n-propanol have been successfully prepared by means of a facile and rapid microwave heating for the first time.The structure and morphology of the obtained products were characterized by transmission electron microscopy(TEM),select area electron diffraction(SAED),ultraviolet-visible spectrophotometry(UV-vis),X-ray photoelectron spectroscopy(XPS) and Fourier transform spectroscopy(FT-IR).XPS analysis reveals that the nanorods were in the metallic state.TEM images showed that ruthenium nanorods had an obvious one-dimensional structure with the aspect ratio ranged from 5 to 40 nm and length up to 600 nm.SAED patterns indicated that the nanorods were single-crystalline with a hexagonal structure.     

Polymer-controlled synthesis of Fe3O4 single-crystal nanorods

In this study, we describe a simple approach to preparing single-crystal Fe3O4 nanorods in the presence of poly(vinylpyrrolidone) (PVP). The morphologies of the nanorods are characterized by transmission electron microscopy (TEM), which indicates that these nanorods are formed by nucleation and growth process in situ in aqueous solution. A superconducting quantum interference device (SQUID) magnetometer characteristic of the as-synthesized Fe3O4 nanorods shows superparamagnetic properties.     

General, room-temperature method for the synthesis of isolated as well as arrays of single-crystalline ABO4-type nanorods

Single-crystalline BaWO(4) and BaCrO(4) nanorods of reproducible shape and of varying sizes have been controllably prepared using a simple, room-temperature approach, based on the use of porous alumina template membranes. Aligned BaWO(4) and BaCrO(4) nanorod arrays can be obtained by dissolving the template. Our facile technique, which is analogous to biomineralization, offers a promising and generalized methodology to prepare other types of free-standing ABO(4) nanorods and their corresponding nanorod arrays. Extensive characterization of these samples has been performed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDS), selected area electron diffraction (SAED), Raman spectroscopy, FT-infrared spectroscopy (FT-IR), and X-ray diffraction (XRD).     

Characterization of h-WO3 nanorods synthesized by hydrothermal process

Hexagonal tungsten oxide nanorods have been synthesized by hydrothermal strategy using Na₂WO₄·2H₂O as tungsten source, aniline and sulfate sodium as structure-directing templates. Techniques X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy have been used to characterize the structure, morphology and composition of the nanorods. The h-WO₃ nanorods are up to 5 μm in length, and 50–70 nm in diameter.     

Electrochemical synthesis of ZnO nanorods/porous silicon composites and their gas-sensing properties at room temperature

The zinc oxide (ZnO) nanorods with different aspect ratio (length/diameter) were grown directly on the porous silicon (PS) substrate through electrochemical synthesis. The obtained ZnO nanorods/PS products were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and gas-sensing test. Comparative study shows that the addition of nonionic polymer polyvinylpyrrolidone (PVP) into oxygenated zinc chloride electrolyte can modulate the crystal growth and the aspect ratio of ZnO nanorods from electrodeposition, thus, influence the gas-sensing properties of ZnO nanorods/PS composites. With appropriate amount of PVP in the electrolyte, the product possessing high-density and large aspect ratio ZnO nanorods has an obvious improvement of the NO₂-sensing performances with high sensitivity, fast response-recovery characteristic, and good repeatability and selectivity. The gas-sensing mechanism was discussed in the paper. The result indicated that the heterojunction effect of ZnO nanorods and PS may be responsible for the excellent gas-sensing properties.     

葡萄糖辅助合成碲化铅纳米棒及其表征

采用简单的葡萄糖辅助溶剂热合成法制备了碲化铅纳米棒。 利用X射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)、高分辨率透射电子显微镜(HRTEM)、能谱仪(EDS)等技术手段进行材料结构和形貌表征。 结果表明,产物是纯的立方相PbTe,纳米棒的直径约为50 nm,长500 nm左右。 研究了反应过程的影响因素及碲化铅纳米棒的形成机制。 产物的形貌受葡萄糖的量、反应时间、反应温度和聚乙烯吡咯烷酮(PVP)质量的控制,分析了形成这种结构的原因。     

Studies on the micropolarities of bmimBF4/TX-100/toluene ionic liquid microemulsions and their behaviors characterized by UV-visible spectroscopy

Ionic liquids (ILs), 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF4), were substituted for polar water and formed nonaqueous microemulsions with toluene by the aid of nonionic surfactant TX-100. The phase behavior of the ternary system was investigated, and microregions of bmimBF4-in-toluene (IL/O), bicontinuous, and toluene-in-bmimBF4 (O/IL) were identified by traditional electrical conductivity measurements. Dynamic light scattering (DLS) revealed the formation of the IL microemulsions. The micropolarities of the IL/O microemulsions were investigated by the UV-vis spectroscopy using the methyl orange (MO) and methylene blue (MB) as absorption probes. The results indicated that the polarity of the IL/O microemulsion increased only before the IL pools were formed, whereas a relatively fixed polar microenvironment was obtained in the IL pools of the microemulsions. Moreover, UV-vis spectroscopy has also shown that ionic salt compounds such as Ni(NO3)2, CoCl2, CuCl2, and biochemical reagent riboflavin could be solubilized into the IL/O microemulsion droplets, indicating that the IL/O microemulsions have potential application in the production of metallic or semiconductor nanomaterials, and in biological extractions or as solvents for enzymatic reactions. The IL/O microemulsions may have some expected effects due to the unique features of ILs and microemulsions.     

水溶性银纳米颗粒的制备及抗菌性能

采用液相还原法, 以单宁酸为还原剂, 聚乙烯吡咯烷酮(PVP)为修饰剂制备出了水溶性的表面修饰Ag纳米颗粒. 通过X 射线粉末衍射仪(XRD)、透射电子显微镜(TEM)、紫外-可见吸收分光光度计(UV-Vis)、傅里叶变换红外(FTIR)光谱仪等对所得样品的形貌和结构进行了表征. 采用肉汤稀释法测试了样品的抗菌性能, 考察了样品在水相中的分散稳定性, 提出了PVP修饰Ag纳米颗粒的形成机理. 结果表明所制备的样品具有Ag的面心立方晶体结构, 平均粒径为15-17 nm. 样品在水相中能长时间稳定分散; 对埃希氏大肠杆菌(E. coli)、金黄色葡萄球菌(S. aureus)具有明显的抗菌作用. 操作简便、条件温和的制备方法易于在工业规模上放大; 试剂无毒, 使得所制备的PVP修饰Ag纳米颗粒作为抗菌剂具有良好的应用前景.     

Facile fabrication of rutile monolayer films consisting of well crystalline nanorods by following an IL-assisted hydrothermal route

In this study, rutile films consisting of rectangular nanorods were facilely deposited on glass substrates from strongly acid solution of TiCl₄. The highly ordered array of nanorods was realized in presence of ionic liquid (IL) of [Bmim]Br by following a hydrothermal process. In this process, Degussa P25 nanoparticles served as seeds that were pre-deposited on the substrates to facilitate the array of rutile nanorods. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectrum were used to characterize the obtained nanorod films. The measurements showed that the nanorods were rectangular with width of 100-200 nm and length of more than 1 μm, and grew up typically along c-axis to form the arrays against the substrate. The presence of IL was found vital for the formation of rutile nanorods, and the suitable molar ratio of [Bmim]Br to TiCl₄ ranged from 500:1 to 1500:1. The excessive [Bmim]Br may hinder the precipitation of rutile particles.     

反应条件对ZnWO4纳米棒的形貌和光致发光性能的影响

采用水热法合成了ZnWO4纳米棒, 并用扫描电镜(SEM)、透射电镜(TEM)和粉末X射线衍射(XRD)等技术对产物进行了表征. 实验结果表明, 反应溶液的pH值和反应时间是影响ZnWO4纳米棒形成的重要因素. 研究了不同反应条件下制备的ZnWO4纳米晶的光致发光性能.     

Silver nanoparticles stabilized by crosslinked poly(vinyl pyrrolidone) and its application for facilitated olefin transport

Positively polarized silver nanoparticles by poly(vinyl pyrrolidone) (PVP) have been demonstrated for use as stable olefin carriers for facilitated olefin transport membranes. The formation and size of silver nanoparticles stabilized by PVP were monitored using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Nanocomposite membranes consisting of polymer and silver nanoparticles stabilized by PVP exhibited the high separation performance for olefin/paraffin mixtures. X-ray photoelectron spectroscopy (XPS) showed that silver nanoparticles stabilized by PVP exhibited a high positive polarity, resulting in the reversible interaction between the surface of silver nanoparticles and olefin molecules.     

Mesoporous Silica Materials Synthesized via Sol-Gel Methods Modified with Ionic Liquid and Surfactant Molecules

Mesoporous silica materials were synthesized via a sol-gel method employing a room temperature ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, bmimBF4) as a new solvent medium and further modified with surfactant (hexadecyl-trimethyl-ammonium bromide, CTAB) as a pore templating material. The synthesized samples were characterized by the transmission electron microscopy, X-ray diffraction, and N2 adsorption-desorption techniques. The results indicated that the mesoporous silica synthesized by using bmimBF4 and CTAB as mixed templates showed better mesostructural order and smaller pore size, compared with mesoporous silica materials synthesized by using single bmimBF4 as template under the same conditions. This indicates that the presence of surfactant can affect the microstructures of silica prepared by the present synthesis method.     

Pd-Ag合金纳米线的可见光辅助简易合成及其对乙醇的电催化氧化

以硝酸钯和硝酸银为金属前驱体,乙醇和柠檬酸钠作为还原剂,聚乙烯吡咯烷酮作为稳定剂和导向剂,以普通市售白炽灯作为光源,采用简易可见光辅助液相法合成了Pd-Ag合金纳米线。通过FESEM、TEM、HRTEM、PXRD和UV-Vis等技术对样品的形貌、晶体结构和光学性质进行了表征,并通过循环伏安法和计时电流法研究了Pd-Ag合金纳米线修饰玻碳电极对乙醇的电催化氧化。与相同条件下制备的纳米钯材料相比,Pd-Ag合金纳米线具有更好的电催化活性、抗中毒性和稳定性。     

Pd-Ag合金纳米线的可见光辅助简易合成及其对乙醇的电催化氧化

以硝酸钯和硝酸银为金属前驱体,乙醇和柠檬酸钠作为还原剂,聚乙烯吡咯烷酮作为稳定剂和导向剂,以普通市售白炽灯作为光源,采用简易可见光辅助液相法合成了Pd-Ag合金纳米线。通过FESEM、TEM、HRTEM、PXRD和UV-Vis等技术对样品的形貌、晶体结构和光学性质进行了表征,并通过循环伏安法和计时电流法研究了Pd-Ag合金纳米线修饰玻碳电极对乙醇的电催化氧化。与相同条件下制备的纳米钯材料相比,Pd-Ag合金纳米线具有更好的电催化活性、抗中毒性和稳定性。     

单分散磷酸镧纳米棒的可控制备

采用一步水热法在无模板情况下合成了单一形貌和尺寸均匀的磷酸镧纳米棒,产物分散性好.这种合成方法操作简单、能耗低、合成条件可控,并且重复性很好、可大面积合成.用X射线粉末衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)对磷酸镧的形貌、结构以及相组成进行了分析.结果表明:所合成磷酸镧为单斜相独居石结构;纳米棒直径为15 nm,长度约为几百纳米,具有相当高的纵横比,有望在性能方面得到优化;磷酸镧纳米棒为单晶.对影响磷酸镧纳米棒形成的反应条件如水热温度和水热时间进行了研究,并详细研究了其生长过程.提出了磷酸镧纳米棒的可能生长机制是基于纳米颗粒的定向粘附作用.     

A facile route to growth of γ-MnOOH nanorods and electrochemical capacitance properties

Single crystal nanorods of γ-MnOOH with lengths up to hundreds of nanometers were successfully prepared employing a novel solvothermal process based on the redox reaction between potassium permanganate (KMnO(4)) and N, N-dimethyl ammonium formate (DMF) without extra surfactant or template. The as-prepared products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and Fourier transformed infrared spectroscopy (FTIR). The electrochemical properties of γ-MnOOH nanorods were investigated by cyclic voltammetry and galvanostatic charge-discharge performance measurements. Specific capacitance (C(s)) calculated from the galvanostatic discharge curve was 131.9 F g(-1) for γ-MnOOH nanorods at the current density of 0.5 A g(-1). The electrochemical experiment results demonstrate that γ-MnOOH nanorods should be a good candidate as electrode material for supercapacitor.     

Structural studies of 1-butyl-3-methylimidazolium tetrafluoroborate/TX-100/ p-xylene ionic liquid microemulsions.

The ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF4) forms nonaqueous microemulsions with p-xylene, with the aid of the nonionic surfactant TX-100. The phase behavior of the ternary system is investigated, and three microregions of the microemulsions-ionic liquid-in-oil (IL/O), bicontinuous, and oil-in-ionic liquid (O/IL)-are identified by conductivity measurements, according to percolation theory. On the basis of a phase diagram, a series of IL/O microemulsions are chosen and characterized by dynamic light scattering (DLS). The size of aggregates increases on increasing the amount of added polar component (bmimBF(4)), which is a similar phenomenon to that observed for typical water-in-oil (W/O) microemulsions, suggesting the formation of IL/O microemulsions. The microstructural characteristics of the microemulsions are investigated by FTIR and 1H NMR spectroscopy. The results indicate that the interaction between the electronegative oxygen atoms of the oxyethylene (OE) units in TX-100 and the electropositive imidazolium ring may be the driving force for the solubilization of bmimBF4 into the core of the TX-100 aggregates. In addition, the micropolarity of the microemulsions is investigated by using methyl orange (MO) as a UV/Vis spectroscopic probe. A relatively constant polarity of the microemulsion droplets is obtained in the IL microemulsion. Finally, a plausible structure for the IL/O microemulsion is presented.     

一种在固体基底上制备高度取向氧化锌纳米棒的新方法

采用廉价、低温的方法，在修饰过ZnO纳米粒子膜的ITO基底上成功制备出具有 高长径比、高度取向的ZnO纳米棒阵列，用扫描电子显微镜(SEM)，X射线衍射(XRD) ，高分辨透射电子显微镜(HRTEM)以及拉曼光谱对制备出的ZnO纳米棒的结构和形貌 进行了表征，测试结果表明，ZnO纳米棒是单晶，属于六方晶系，与基底直，上仍 沿(001)晶面择优生长的特征，并且ZnO纳米棒基本上无氧空位的存在，统计结果显 示，水热反应2h后90%以上的ZnO纳米棒直径为120～190nm，长度为4μm