单晶ZnO六棱锥的PEG400辅助热分解合成及其光致发光性能(英文)

将由Zn(CH3COO)2·2H2O和Na2CO3通过室温研磨反应获得的前驱体在PEG400存在下于240°C热分解获得大量的ZnO六棱锥产物。用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和高分辨透射电子显微镜(HRTEM)表征产物的晶体结构和形貌。进一步的实验结果表明:PEG400在ZnO六棱锥形成过程中发挥着重要作用,单六棱锥和双六棱锥的结构差异来自于热分解反应。光致发光谱(PL)测试表明:ZnO六棱锥在386nm处展示强的近带隙发射,在550nm处展示较弱的绿光发射。435cm-1处的拉曼振动表明ZnO六棱锥具有良好的晶体质量。     

Microwave-assisted synthesis of CePO<Subscript>4</Subscript> nanorod phosphor with violet emission

Monoclinic and hexagonal CePO4 nanoparticles and nanorods were successfully synthesized from Ce(NO3) 3·6H2O and Na3PO4·12H2O solu-tions at pH 1-5 by a 180 W microwave radiation for 60 min.The products were characterized by X-ray diffraction(XRD) ,Fourier transform infrared(FTIR) spectroscopy,and scanning electron microscopy(SEM) .XRD patterns revealed that the products are hexagonal CePO4 structures at pH 2-5,and monoclinic CePO4 structures at pH 1.SEM characterization shows that these products were nanoparticles,short nanorods,and long nanorods,controlled by the pH of the precursor solutions.Optical properties of the nanorods were also investigated by ultraviolet-visible(UV-vis) and photoluminescence(PL) spectroscopy.     

Hydrothermal synthesis and optical properties of Ni doped ZnO hexagonal nanodiscs

Single crystalline Ni-doped ZnO hexagonal nanodiscs are successfully synthesized. Zinc acetate, nickel nitrate, sodium hydroxide and poly (vinyl pyrrolidone) (PVP) were mixed together and transferred to a 100 ml Teflon-lined stainless steel autoclave which kept at 150 °C for 24 h. The morphology and microstructure were determined by field emission scanning electron microscopy (FE-SEM), X-ray diffraction transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and photoluminescence (PL) spectroscopy. The investigation confirmed that the products were of the wurtzite structure of ZnO. The doped hexagonal nanodiscs have edge length 30 nm and thickness of 45 nm. EDX result showed that the amount of Ni in the product is about 12%. Photoluminescence of these doped hexagonal nanodiscs exhibits a blue shift and weak ultraviolet (UV) emission peak, compared with pure ZnO, which may be induced by the Ni-doping. The growth mechanism of the doped hexagonal nanodiscs was also discussed.     

Morphology and phase evolvement of Yb/Er co-doped NaYF4 microtubes prepared with YF3 submicrospindles as precursor

Hexagonal phase NaYF₄ microtubes co-doped with Yb³⁺ and Er³⁺ were synthesized through a hydrothermal process with YF₃ submicrospindles as precursor. The X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM) were utilized to characterize the structure and morphology of the as-prepared products. XRD results show that pure cubic NaYF₄ crystals can be obtained when reaction time is 2 h. While the product is mixture of cubic and hexagonal phase NaYF₄ when reaction time is from 7 to 20 h. Continuing to increase the reaction time to 24 h, the pure hexagonal NaYF₄ crystals were formed. The FE-SEM and TEM results show that the morphology of pure cubic NaYF₄ is spherical clusters composed of spherical nanoparticles with average diameter of about 100 nm and the pure hexagonal NaYF₄ crystals have tubular structure with out diameter of about 0.3-0.5 μm, inner diameter of about 0.5-1 μm and length ranging from 3 to 12 μm. The luminescence properties of Yb³⁺/Er³⁺ co-doped cubic and hexagonal phase NaYF₄ microcrystals were also studied. Under 980-nm excitation, the upconversion luminescence (UCL) intensity of hexagonal phase NaYF₄ microtubes is much stronger than that of cubic phase clusters. Moreover, both red and green upconversion are ascribed to the two-photon process. Therefore, hexagonal phase NaYF₄ microtubes with high UCL efficiency may have a potential application in photonic device.     

Synthesis of lanthanum hydroxide and lanthanum oxide nanoparticles by sonochemical method

In this work lanthanum hydroxide nanoparticles were synthesized by sonochemical method. La₂O₃ nanoparticles were obtained after calcination of the La(OH)₃ nanoparticles precursor in air at 600 °C for 2 h. The effect of some parameters such as concentration of precursors, pulse time of sonication, time of sonication, and addition of PEG as surfactant on the morphology and the particle size were studied. The as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrum (XPS) and Fourier transform infrared (FT-IR) spectra.     

A simple thermal decomposition-nitridation route to nanocrystalline boron nitride (BN) from a single N and B source precursor

Nanocrystalline boron nitride (BN) was synthesized via a simple thermal decomposition-nitridation route by the reaction of hydrated ammonium tetraborate (NH₄HB₄O₇·3H₂O) and metallic magnesium powders in an autoclave at 650 °C. The crystal phase, morphology, grain size, and chemical composition of the as-prepared products were characterized in detail by X-ray powder diffraction (XRD), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). The products were also studied by FT-IR and the thermogravimetric analysis (TGA). Results revealed that the as-synthesized nanocrystalline were h-BN, and they had diameters within 100 nm. They had good thermal stability and oxidation resistance in high temperature.     

Microwave-assisted solid-state decomposition of La[Co(CN)6]·5H2O precursor: A simple and fast route for the synthesis of single-phase perovskite-type LaCoO3 nanoparticles

Pure and single-phase nanoparticles of perovskite-type LaCoO₃ were prepared via microwave-assisted solid-state decomposition of La[Co(CN)₆]·5H₂O precursor in the presence of CuO powder as a strong microwave absorber within a very short reaction time of 10 min. Product was characterized by X-ray diffraction (XRD), Fourier-transformed infrared spectroscopy (FT-IR), Raman spectroscopy, UV–visible spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) and surface area measurement. The method is simple, fast and energy efficient and resulted in fine particles (10–30 nm) with high specific surface area and narrow size distribution. This hybrid microwave heating route is promising for the synthesis of other mixed oxide and related compounds.     

Nanosphericals and nanobundles of ZnO: Synthesis and characterization

ZnO nanosphericals and nanobundles well dispersion have been synthesized using [(N,N′-bis(salicylaldehydo)ethylenediamine)zinc(II)]; [Zn(salen)] as precursor via two methods. Nanosphericals of ZnO has been prepared via thermal decomposition of [Zn(salen)] in the presence of oleylamine at 290 °C for 90 min. Also nanobundle of ZnO has been synthesized via thermolysis of [Zn(salen)] in the air at 500 °C for 5 h. The as-synthesized products were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and scanning electronic microscopy (SEM). The room temperature photoluminescence (PL) spectra of both nanostructures are dominated by the green emission attributed to the oxygen vacancy (V_O) related donor-acceptor transition. Presence of several infrared (IR) inactive vibrational modes in the Fourier transform infrared (FT-IR) absorption spectra of the samples indicates a breakdown of translational symmetry in the nanostructures induced by native defects.     

Growth and photocatalytic activity of ZnO nanosheets stabilized by Ag nanoparticles

The Ag nanoparticles-stabilized ZnO nanosheets were prepared using a liquid-liquid two-phase method with (n-Dodecyl)trimethylammonium bromide (DTAB) as a phase transfer agent at the room temperature. The silver nanoparticles which are conductors with the character of attracting energy can make the ZnO sheets stabilize under the higher energy electrons. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectroscopy and fluorescence. The results demonstrate that the silver nanoparticles load on the surface of ZnO sheets and make the ZnO sheets stabilize. Furthermore, the formation mechanism of ZnO sheets stabilized by silver nanoparticles was also proposed and discussed in detail. Moreover, the photocatalysis test shows that the ZnO sheets stabilized by silver nanoparticles exhibit a higher photocatalytic activity than the pure ZnO nanosheets, thereby implying that the Ag/ZnO interfaces promote the separation of photogenerated electron-hole pairs and enhance the photocatalytic activity.     

A facile method to prepare MoS2 with nanolameller-like morphology

MoS₂ nanolamellers were synthesized by a one-step oxidation-reduction reaction in solution, in which the (NH₄)₂MoS₄ and H₂C₂O₄·2H₂O were used as reactants and then calcined at 800 °C under N₂ for 1 h. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The diameter and nanoplate thickness of the obtained MoS₂ nanolamellers were approximately 80 nm and 20-30 nm, respectively. These novel structures of nanolamellers had potential applications in solid lubricants.     

Glycolthermal synthesis and characterization of hexagonal CdS round microparticles in flower-like clusters

Hexagonal CdS round microparticles in flower-like clusters were synthesized by glycolthermal reactions of CdCl₂ and thiourea as cadmium and sulphur sources in 1,2-propylene glycol (PG) at 100-200 °C for 10-30 h. Phase and morphology were detected using X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM, TEM). The products were pure phase of hexagonal wurtzite CdS. The quantitative elemental analysis of Cd:S ratio was detected using energy dispersive X-ray (EDX) analyzer. Raman spectrometer revealed the presence of fundamental and overtone modes at 296 and 595 cm⁻¹, corresponding to the strong 1LO and weak 2LO modes, respectively. Photonic properties were investigated using UV-visible and photoluminescence (PL) spectroscopy. They showed the same absorption at 493-498 nm, and emission at 431 nm due to the excitonic recombination process. A possible formation mechanism was also proposed, according to experimental results.     

Controlling the particle size of nanobrookite TiO2 thin films

In this study, pure nanobrookite TiO₂ thin films were successfully deposited on glass substrates with the spin-coating method using titanium butoxide and acetic acid. The particle size of TiO₂ films was controlled by the water:AcAc volume ratio. This study shows that it is possible to obtain single oriented pure brookite films. The structural and optical properties of the nanobrookite TiO₂ thin films were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), ultraviolet-visible spectroscopy (UV-vis), scanning electron microscopy (SEM), spectrophotometer (NKD), and Fourier transform infrared spectrometer (FTIR).     

Synthesis and Characterization of the Antibacterial Activity of Zinc Oxide Nanoparticles against Salmonella typhi

Metal oxides can be used as a series of new and effective anti-bacterial agents.In this study,four concentrations of ZnO nanoparticles(0.2,0.5,0.7 and 1.0 mol/L) were synthesized using a low-temperature sol-gel method annealed at400 and 550 °C.The products were characterized by X-ray diffraction(XRD),transmission electron microscopy(TEM)and Fourier transform infrared spectroscopy(FTER).XRD results show the hexagonal wurtzite structure of the nanoparticles with the grain size in the range of 38-43 nm.TEM micrographs exhibit a polyhedral form of the synthesized nanoparticles.The antimicrobial activity of different concentrations of nanoparticles against Salmonella typhi PTCC 1609 was determined by disk diffusion and agar dilution method at five concentrations of 10,5,2.5,1.25 and 0.625 mg/mL.Analysis shows that the prepared ZnO nanoparticles have a very effective antimicrobial activity against Salmonella typhi.This activity increases by reducing the size of nanoparticles and increasing their content in the bacterial growth medium.     

Preparation and characterization of carbonyl iron soft magnetic composites with magnesioferrite insulating coating layer

Spherical carbonyl iron (Fe) powders were coated with magnesioferrite (MgFe₂O₄) insulating coating layer and then mixed with epoxy-modified silicone resin (ESR). Soft magnetic composites (SMCs) were fabricated by compaction of the coated powders and annealing treatment. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffractometry (XRD) and X-ray photoelectron spectroscopy (XPS) revealed that the MgFe₂O₄ layer was coated on the surface of the iron powders. The magnetic properties of SMCs were determined using a vibrating sample magnetometer and an auto testing system for magnetic materials. The results showed that the SMCs prepared at 800 MPa and 550 °C exhibited a significant core loss of 167.5 W/kg at 100 kHz and 50 mT.     

Corrosion performance and mechanical properties of sputter-deposited MgY and MgGd alloys

Films of MgY and MgGd alloys were deposited on silicon wafers by magnetron sputtering. The microstructure, crystal structure and mechanical properties were evaluated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and tensile testing. Corrosion was evaluated for immersion in 3.5% NaCl solution saturated with Mg(OH)₂. TEM, SEM and XRD indicated that the alloys were single phase. There was no significant change of corrosion rate with alloy content. The strength increased with alloying content, and ductility decreased concomitantly. Strengthening was consistent with solid solution strengthening or short-range order.     

Characterisation of the coke formed during metal dusting of iron in CO-H2-H2O gas mixtures

Carbon deposits formed on the surface of iron samples during carburisation at 700 °C in a gas mixture of 75%CO-24.81%H₂-0.19%H₂O were characterised by using scanning electron microscopy (SEM), X-ray diffraction (XRD), Mössbauer spectroscopy and transmission electron microscopy (TEM). Cross-section observation of the iron sample by light optical microscopy revealed the formation of cementite after only 10 min reaction, together with a thin layer of graphite. After 4 h reaction, a thick coke layer was formed on top of the cementite surface. SEM surface observation indicated the formation of filamentous carbon in the coke layer. Further analysis of the coke by XRD and Mössbauer showed the presence of mainly Fe₃C and small amount of Fe₂C but no metallic iron in the carbon deposit. TEM analysis of the coke detected very convoluted filaments with iron-containing particles at the tip or along their length. These particles were identified to be cementite by selected area diffraction. Carbon deposits produced at the same temperature but with other gas compositions were also analysed by using XRD. It was found that with a low content of CO, e.g. 5%, both α-Fe and Fe₃C were detected in the coke. Increasing CO content to more than 30%, iron carbide was the only iron-containing phase.     

Mn behaviors in Mn-implanted ZnO

The behavior of Mn when doped into ZnO by ion implantation was investigated by scanning transmission electron microscopy, electron energy loss spectroscopy and energy dispersive X-ray spectroscopy. Unlike the previously reported case of Co/Ni-implanted ZnO (where Co/Ni nanocrystals were observed), Mn implantation has been found to induce an O deficiency in ZnO, which results in the formation of hexagonal Zn nanocrystals when the implantation dose is sufficient. Further annealing of the high-dose Mn-implanted ZnO promotes the formation of ZnMn₂O₄ compounds near the surface and a porous structure within the implanted region. The fundamental reasons behind these physical phenomena are discussed.     

X-ray diffraction analysis of a severely plastically deformed aluminum alloy

The crystallite size, lattice microstrain, lattice parameter, and formation of solid solutions of a nanocrystalline Al₉₃Fe₃Cr₂Ti₂ alloy prepared via mechanical alloying (MA) starting from elemental powders have been investigated using the Rietveld method of X-ray diffraction (XRD) in conjunction with line-broadening analyses through the variance, Warren–Averbach, and Stokes and Wilson methods. Detailed analyses using transmission electron microscopy (TEM), scanning electron microscopy (SEM), and inductively coupled plasma-optical emission spectroscopy (ICP) have also been conducted in order to corroborate the formation of solid solutions and the grain size measurement determined from the XRD analyses. The results from the exhaustive XRD analyses are in excellent agreement with those derived from the investigation of TEM, SEM, and ICP. The lattice microstrains of the nanocrystalline Al solid solution determined from the XRD analyses are isotropic along different crystallographic directions and high, exhibiting the same order of magnitude as the ratio of the tensile strength to the elastic modulus of the Al crystal. Implications resulting from the comparison between the present study and the simplified XRD analyses are discussed.     

Controlled synthesis of TiO2 mesoporous microspheres via chemical vapor deposition

Anatase titanium dioxide (TiO₂) mesoporous microspheres with core-shell and hollow structure were successfully prepared on a large scale by a one-step template-free chemical vapor deposition method. The effects of various reaction conditions on the morphology, composition and structure of the products were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET) technique and photoluminescence (PL) method. The results indicate that the product near the source was composed of core-shell structure TiO₂ microspheres with diameters from 3 to 5 μm. With increasing the distance between the source materials and the substrate, the hollow TiO₂ spheres with 1-2 μm dominant the products. A localized Ostwald ripening can be use to explain the formation of core-shell and hollow structures, and the size of the initial TiO₂ solid nanoparticles plays an important role in determining the evacuation manner of the solid in the ripening-induced hollowing process. The surface area of TiO₂ hollow microspheres determined by the adsorption isotherms was measured to be 74.67 m²/g. X-ray photoelectron spectroscopy (XPS) analysis revealed that the O-H peaks of hollow structures have a chemical shift compared with the core-shell structures. The optical property of the products was also discussed.     

Decorating Mg/Fe oxide nanotubes with nitrogen-doped carbon nanotubes

Mg/Fe oxide nanotubes decorated with nitrogen-doped carbon nanotubes (CN_x) were fabricated by catalytic chemical vapor deposition of ethylenediamine on the outer surface of oxide nanotubes. Mg/Fe oxide nanotubes were prepared using a 3:1 molar precursor solution of Mg(NO₃)₂ and Fe(NO₃)₃ and anodic aluminum oxide as the substrate. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and vibrating sample magnetometer (VSM). The XRD pattern shows that the oxide nanotubes are made up of MgO and Fe₂O₃. TEM and SEM observations indicate the oxide nanotubes are arrayed roughly parallel to each other, and the outer surface of oxide nanotubes are decorated with CN_x. XPS results show the nitrogen-doped level in CN_x is about 7.3 at.%. Magnetic measurements with VSM demonstrate the saturated magnetization, remanence and coercivity of oxide nanotubes are obvious improved after being decorated with CN_x.