PbTe nanostructures: Microwave-assisted synthesis by using lead Schiff-base precursor,characterization and formation mechanism

Pure cubic phase lead telluride (PbTe) nanostructures have been produced by using a Schiff-base complex as a precursor in the presence of microwave irradiation. The Schiff base used as ligand was derived from salicylaldehyde and ethylenediamine. The Schiff-base complex was marked as [Pb(salen)]. In addition, the effect of the irradiation time and the type of reducing agent on the morphology and purity of the final products was investigated. The as-synthesized PbTe nanostructures were characterized extensively by techniques like X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The microwave formation mechanism of the PbTe nanostructures was studied by XRD patterns of the products. Although it was found that both ionic and atomic mechanisms could take place for the preparation of PbTe, the main steps were according to the atomic reaction process, which could occur between elemental Pb and Te.     

A Systematic Study of ZnO/CuO Core/Shell Nanostructures Pegylated by Microwave Assistant Reverse Micelles (RM) Method

In this work we synthesized ZnO/CuO nanostructures pegylated by simple and fast microwave method assistant reverse micelles, Reverse micelles protocol creates many advantages in stability, particle size control, morphology, density, loading level, distribution, uniformity, charge and purification. Based on the statistical results ZnO/CuO nanostructures placed in the hydrophilic substrate. The effect of microwave and concentration of surfactant on the surface area, pore diameter and pore volume of the final product was systematically studied using Taguchi technique. ZnO/CuO core/shell pegylated nanostructures, indicating a ZnO as core and CuO as shell and continuous micelles chains around this structures. Products were characterized by UV–Vis spectra, X-ray diffraction, scanning electron microscopy, Dynamic light scattering, Energy-dispersive X-ray spectroscopy, transmission electron microscopy and nitrogen adsorption (i.e. Brunauer–Emmett–Teller surface area analysis).     

树枝状钯纳米结构的控制合成及硝基苯加氢反应的催化活性

以氯钯酸为前驱体, 苯甲醇为还原剂和溶剂, 十六烷基吡咯烷酮(PVP)为稳定剂, 在微波辐射下制备了分散均匀、形貌均一的树枝状钯纳米结构. 产物用透射电子显微镜(TEM), X射线粉末衍射(XRD), X射线光电子能谱(XPS)进行了表征, 表明所制备的Pd纳米颗粒呈树枝状, 形貌单一, 分散均匀, 是由许多近似圆形的小颗粒自组装而成的二级结构. 对树枝状钯催化硝基苯加氢反应进行探究, 表明树枝状钯的催化活性比市售的钯碳催化剂的催化活性高.     

Self-assembly and branching of sucrose stabilized silver nanoparticles by microwave assisted synthesis: From nanoparticles to branched nanowires structures

Silver nanostructures were synthesized under microwave irradiation from a solution of silver nitrate and sucrose, with any other reducing or capping agent. The size and morphology of nanostructures changed continuously during the irradiation time. The obtained nanostructures at the different irradiation time were characterized by X-Ray diffraction, UV–vis spectroscopy, scanning and transmission electron microscopy and selected area diffraction pattern. It was evidenced that initially Ag nanoparticles were formed, which, as reaction time elapsed, self-assembled and fused with each other to yield nanowires and further branched nanowires. The formation of the silver branched nanostructures can be explained as a process of initial reduction–nucleation–adsorption–growth–branching growth.     

Effect of titania structure on the properties of its supported copper oxide catalysts

A facile and rapid microwave irradiation method was explored for the synthesis of bismuth phosphate (BiPO(4)) nanostructures with various morphologies and phases in different solvents. The BiPO(4) products were characterized by powder X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), UV-vis diffuse reflection spectroscopy (DRS). The effect of the solvents on the formation of the BiPO(4) nanostructures was discussed on the basis of experimental results. The different BiPO(4) nanostructures exhibited different optical properties, BET surface areas and photocatalytic activities on the degradation of methyl orange (MO) under UV and visible light irradiation. The experimental results suggested that the photocatalytic activity was closely relative with the crystalline phase and band gap of BiPO(4). Hexagonal BiPO(4) nanoparticles with narrow band gap showed the highest photocatalytic performance.     

Synthesis and characterization of nickel sulfide nanoparticles via cyclic microwave radiation

In current study, nanoparticles of NiS were synthesized by applying microwave radiation. The effect of concentration of sulfur source, reaction time, and power of microwave irradiation on the treatment process was investigated. The morphology, structure, and composition of the as-synthesized nanostructures have been confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Optical properties of as-prepared sample were investigated by photoluminescence spectroscopy; the emission peak is at 555.04 nm and shows the blue shift.     

微波热解法制备Cu/Cu2O纳米材料

在二乙二醇溶剂体系中利用微波介电加热分解醋酸铜前体,进一步还原得到Cu2O和Cu纳米粒子以及Cu/Cu2O核壳结构。 采用X射线衍射、透射电子显微镜、扫描电子显微镜和紫外吸收光谱测试技术对产物的形貌、结构和组成进行了研究,结果表明,得到的Cu/Cu2O核壳结构直径为500 nm左右。 对比实验研究了不同聚合度乙二醇系列溶剂、反应时间以及表面活性剂或配位剂对产物形貌、组成的影响,表明低聚合度乙二醇和长的反应时间有利于醋酸铜还原形成铜。     

Direct synthesis of gallium oxide tubes,nanowires, and nanopaintbrushes

We demonstrate bulk synthesis of highly crystalline beta-gallium oxide tubes, nanowires, and nanopaintbrushes using molten gallium and microwave plasma containing a mixture of monatomic oxygen and hydrogen. Gallium oxide nanowires were 20-100 nm thick and tens to hundreds of micrometers long. Transmission electron microscopy (TEM) revealed the nanowires to be highly crystalline and devoid of any structural defects. Results showed that multiple nucleation and growth of gallium oxide nanostructures could easily occur directly out of molten gallium exposed to an appropriate composition of hydrogen and oxygen in the gas phase. These gallium oxide nanostructures should be of particular interest for optoelectronic devices and catalytic applications.     

Synthesis and Characterization of CdS Nanoparticles via Cyclic Microwave from Cadmium Oxalate

The present study reports synthesis and characterization of CdS nanoparticles prepared by cyclic microwave route with the use of [Cd(C₂O₄)·3H₂O] powder as a precursor. The products, with an average size ~15 nm, were characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray microanalysis, thermogravimetric analysis, transmission electron microscopy and Fourier transform infrared spectroscopy. Optical property of obtained product was investigated by photoluminescence spectroscopy. The prepared nanostructures displayed a very strong luminescence at 528 nm (2.34 eV) at room temperature.     

Microwave-assisted method for preparation of Sb-doped ZnO nanostructures and their photocatalytic activity

Nanostructures of Sb-doped ZnO with 0.00, 0.03, 0.06, 0.10 and 0.15 mol fractions of Sb⁺³ ions were prepared by a one-pot method in water under microwave irradiation for 5 min. Powder X-ray diffraction studies display that the nanostructures are excellently crystallized in the form of Wurtzite hexagonal crystalline phase and doping Sb⁺³ ions does not change structure of ZnO. Moreover, size of the nanostructures decreases with increasing mole fraction of Sb⁺³ ions. Scanning electron microscopy and transmission electron microscopy images show that morphology and size of the nanostructures are changing with mole fraction of the dopant. In Fourier transform infrared spectra, intensity of the characteristic peak corresponding to Sb–O bond gradually increases with mole fraction of Sb⁺³ ions. UV–vis diffuse reflectance spectra of the nanostructures are similar to each other and they have a maximum of about 357 nm. Photocatalytic activity of the nanostructures was investigated by degradation of methylene blue under UV irradiation. For the nanostructures with 0.10 mol fraction of Sb⁺³ ions, the degradation rate constant increases nearly two times relative to pure ZnO. In addition, influence of various operational parameters on the degradation activity was investigated and the results were discussed.     

A Simple Microwave Method for Synthesis of CdS Nanoparticles

In this work a surfactant-free microwave method for preparation of CdS nanoparticles is reported. The effect of different parameters i.e. time and irradiation power, sulfur source and solvent on the morphology and the samples particle size have been investigated. The synthesized nanostructures were characterized by X-ray diffraction, energy-dispersive X-ray analysis, scanning electron microscopy, Fourier transform infrared, photoluminescence and ultraviolet–visible spectroscopy.     

Microwave plasma growth and high spatial resolution cathodoluminescent spectrum of tetrapod ZnO nanostructures

A novel microwave plasma assisted by tube furnace heating system is designed to grow tetrapod ZnO nanostructures. Under optimal reaction conditions, Zn powder is oxidated to form the tetrapod ZnO with straight and uniform four legs (nanorods), bearing diameters ranging from 10 to 25 nm and lengths up to 160 nm. High-resolution transmission electron microscopy analyses reveals that the tetrapod ZnO nanostructures are perfect crystalloid. High spatial resolution cathodoluminescent spectrum for individual tetrapod ZnO nanostructure shows only a strong ultraviolet emission at 385 nm.     

微波诱导燃烧法合成类花状ZnO纳米材料及其晶体结构、荧光性质研究

以硝酸锌[Zn(NO3)2.6H2O]和尿素[CO(NH2)2]作前驱体,通过微波诱导燃烧技术可控合成具有不同形貌的ZnO纳米晶体,并用热重分析和差热分析进行了研究。对各种生长条件:微波功率,辐射时间和尿素/Zn2+物质的量的比对ZnO纳米晶体形貌的影响作了分析。结果表明:尿素/Zn2+物质的量的比对ZnO纳米材料的形貌具有显著影响。X衍射图表明合成的ZnO纳米结构呈六角形。傅里叶变换红外光谱图中400~500 cm-1处明显的峰为Zn-O的振动峰。ZnO纳米结构的发光光谱在366 nm的带边发射,因缺陷又由许多可见光发射峰组成。用扫描电子显微镜、透射电子显微镜、选区电子衍射研究了花状ZnO纳米结构的增长机理。本方法仅需几分钟就获得的了ZnO纳米结构。     

桑葚状CaF_2纳米材料的合成及CaF_2:Yb~(3+)的光学性质

通过一步水热法合成了分散性良好、尺寸均一的桑葚状CaF2纳米材料.采用X射线粉末衍射(XRD)、场发射扫描电子显微镜(FESEM)和透射电子显微镜(TEM)对产物的结构、形貌及尺寸进行了表征,发现CaF2纳米材料是由尺寸约为50 nm的纳米粒子构成.通过对不同反应阶段产物的分析提出了其形成机理.研究了Yb3+掺杂CaF2纳米材料的近红外发光性质.     

pH sensitive swelling and releasing behavior of nano-gels based on polyaspartamide graft copolymers

Dendritic and porous Ag-Pd alloy nanostructures were successfully fabricated on the surface of silicon substrate using the co-reduction method and galvanic replacement reaction, respectively. The molar compositions of Ag and Pd in the alloy could be modulated by controlling the molar ratios of metal precursors and reaction time. The Ag-Pd alloy nanostructures were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX), and X-ray diffraction (XRD). The morphology and phase of Au-Pd alloy nanostructures were discussed as a function of molar ratios of metal precursors and reaction time. In addition, the morphology and composition-dependent surface-enhanced Raman scattering (SERS) of the as-synthesized Ag-Pd alloy nanostructures were investigated. The SERS enhancement factor was estimated and SERS mapping was performed to prove the homogeneity of these substrates. The results indicate that as-synthesized dendritic and porous Ag-Pd alloy nanostructures are good candidates for SERS spectroscopy.     

不同形貌ZnO纳米结构的电子显微分析

控制实验合成条件,利用溶胶-凝胶法和化学溶液生长法制备出不同形貌的ZnO纳米结构。采用X射线衍射仪(XRD)、扫描电子显微镜( SEM) 以及透射电子显微镜(TEM)等多种测试手段对ZnO纳米结构的微观形态及晶相进行了分析。结果表明:3种ZnO纳米结构形貌虽不同,但均具有Z nO六方纤锌矿晶相结构。ZnO纳米棒和花状ZnO纳米结构为单晶,生长方向均沿(0001)方向。ZnO纳米球则为多晶。     

A completely green approach to the synthesis of dendritic silver nanostructures starting from white grape pomace as a potential nanofactory

A simple, eco-friendly, cost-effective and rapid microwave-assisted method has been developed to synthetize dendritic silver nanostructures, composed of silver nanoparticles (AgNPs), using white grape pomace aqueous extract (WGPE) as both reducing and capping agent. With this aim, WGPE and AgNO₃ (1 mM) were mixed at different ratio, and microwave irradiated at 700 W, for 40 s. To understand the role of bioactive compounds involved in the green synthesis of AgNPs, preliminary chemical characterization, FT-IR analysis and ¹H NMR metabolite profiling of WGPE were carried out. The effects of bioactive extract concentration and stability over time on AgNPs formation were also evaluated. WGPE-mediated silver nanostructures were then characterized by UV–vis, FTIR analyses, and scanning electron microscopy. Interestingly, the formation of dendritic nanostructures, originated from the self-assembly of Ag rounded nanoparticles (average diameter of 33 ± 6 nm), was observed and ascribed to the use of microwave power and the presence of organic components within the used WGPE, inducing an anisotropic crystal growth and promoting a diffusion-limited aggregation mechanism. The bio-dendritic synthetized nanostructures were also evaluated for potential applications in bio-sensing and agricultural fields. Cyclic voltammetry measurements in 0.5 M phosphate + 0.1 M KCl buffer, pH 7.4 showed that green AgNPs possess the electroactive properties typical of AgNPs produced using chemical protocol. The biological activity of synthetized AgNPs was evaluated by in-vitro antifungal activity against F. graminearum. Additionally, a phytotoxicity evaluation of synthetized green nanostructures was carried out on wheat seed germination. Results highlighted the potential of WGPE as green agent for bio-inspired nanomaterial synthesis, and of green Ag nanostructures, which can be used as antifungal agent and in biosensing applications.     

稀土离子掺杂的AgLa(WO4)2枝状纳米材料的合成与上转换发光性质

通过无模板的水热方法合成了AgLa(WO4)2树枝状纳米晶,没有表面活性剂等模板的介入,使反应变得简捷、绿色和经济. 综合利用多种测试手段对所得材料进行了表征,如X-射线粉末衍射,扫描电子显微镜,透射电子显微镜等,并根据实验结果的分析提出了扩散限制生长（DLA,diffusion-limited aggregation）模型. AgLa(WO4)2树枝状纳米晶可以作为稀土离子掺杂的主体材料,这种掺杂稀土离子（Yb3+, Er3+, Tm3+）的纳米晶在980 nm激光激发下展示丰富的上转换发光颜色. 根据上转换光谱详细研究了AgLa(WO4)2:RE3+树枝状纳米晶在980 nm激光激发下的上转换发光性质和发光机理.     

Chemical stability of ZnO nanostructures in simulated physiological environments and its application in determining polar directions

The in vitro chemical stability and etching of ZnO nanostructures in simulated physiological solution (SPS) were studied using electron microscopy. Calcium hydrogen phosphate thin layers were observed to be uniformly deposited on the surfaces of ZnO nanomaterials in SPS. Electron diffraction and high-resolution transmission electron microscopy revealed that the calcium hydrogen phosphate layers were amorphous and had excellent interfacial contact with the nanocrystals. ZnO nanostructures fabricated by thermal evaporation were found to survive much longer in SPS than those fabricated using a hydrothermal solution method. The shapes of the voids formed in the ZnO nanostructures by the etching in SPS can be used to deduce the polar directions of ZnO nanostructures.     

Ag作催化剂制备的GaN的形貌及其性能

用化学气相沉积法(CVD)在Si(100)衬底上以Ag纳米颗粒为催化剂制备了微纳米结构的GaN,原料是熔融态的金属Ga和气态的NH3。采用X射线衍射仪(XRD)、透射电镜(TEM)、X-ray能谱仪(EDS)、场发射扫描电子显微镜(SEM)、光致发光能谱(PL)和霍尔效应测试对样品进行了结构、成分、形貌和发光、电学性能分析。结果表明:生成的自组装GaN为六方纤锌矿的类似小梯子的微纳米单晶结构,且在不同的温度下,GaN的发光性能和电学性能也有所不同,相对于强的紫外发光峰,其它杂质发光峰很微弱,且均呈p型导电。对本实验所得到的GaN微纳米结构的可能形成机理进行了探讨。