Controlled synthesis of cuprous oxide nanospheres and copper sulfide hollow nanospheres

Uniform Cu₂O nanospheres have been successfully synthesized by reducing CuSO₄ with ascorbic acid in sucrose solution at room temperature. The diameter of the Cu₂O nanospheres can be tuned from 90 to 280 nm by adding different amounts of sucrose in the solution. Furthermore, CuS hollow nanospheres with different diameters have been obtained based on the Kirkendall effect using the as-prepared Cu₂O nanospheres as sacrificial templates. Cu₂O/Cu_7.2S₄ core/shell nanospheres and Cu_7.2S₄ hollow nanospheres are obtained as the intermediate products at different stages of the conversion process. Through the post-treatment of sodium citrate solution, Cu_7.2S₄ hollow nanospheres can be changed into CuS hollow nanospheres. The products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field-emission scanning electron microscopy (FESEM). Optical properties of the products have also been studied.     

Facile synthesis and electrochemical properties of hierarchical MnO2 submicrospheres and LiMn2O4 microspheres

Hierarchical MnO₂ submicrospheres have been successfully synthesized by a wet chemical method. The as-prepared products were characterized by means of XRD, SEM, FTIR, TG, and TEM. With the as-prepared MnO₂ submicrospheres as precursors, LiMn₂O₄ microspheres were conveniently prepared by a simple solid-state reaction between MnO₂ and LiOH at a temperature as low as 600 °C. Electrochemical properties of the as-prepared MnO₂ submicrospheres and LiMn₂O₄ microspheres as cathode materials in lithium ion cells were investigated by galvanostatic charge/discharge tests.     

Synthesis and optical properties of CuS nanoplate-based architectures by a solvothermal method

The controlled synthesis of copper sulfide (CuS) nanoplate-based architectures in different solvents has been realized at low cost by simply reaction of Cu(NO₃)₂·3H₂O and S under solvothermal conditions without the use of any template. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectrometer and fluorescence measurement were used to characterize the products. The products were all in hexagonal phase with high crystallinity and the morphology was significantly influenced by the solvents. The CuS products synthesized in dimethylformamide (DMF) were nanoplates and the samples prepared in ethanol were flower-like morphology composed of large numbers of nanoplates, but those synthesized in ethylene glycol (EG) were CuS architectures with high symmetry made up of several nanoplates arranged in a certain mode. The optical properties were investigated and the growth mechanisms of these CuS crystals were also proposed.     

Low-density core-shell composite hollow microspheres with tunable magnetic properties

Low-density (about 0.9 g/cm³) composite core-shell hollow microspheres with tunable magnetic properties were fabricated by Ni-Fe-P deposition on hollow glass microspheres (HGM) with modified electroless plating process. The effects of mole ratio of Fe²⁺/Ni²⁺, concentration of the reducer and pH value of the solution on the magnetic properties of the products were investigated. In conclusion, the increase in the mole ratio of Fe²⁺/Ni²⁺ and pH value of the solution could improve the soft magnetic properties of composite microspheres remarkably, while the increase in the concentration of NaH₂PO₂ had the opposite effect. The as-obtained metallic shells were amorphous and the crystallization got better with increased annealing temperature after plating. In addition, the saturation intensity of the composite microspheres was enhanced monotonically by increasing the annealing temperature. This work provided a facile and effective strategy to fabricate core-shell composite hollow microspheres with tailored magnetic properties.     

Fabrication of novel Cu microspheres assembled with nanoparticles by a solvothermal reduction route

Copper microspheres assembled with nanoparticles have been synthesized by a simple solvothermal route at 160 °C for 24 h. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometer (EDX), transmission electron microscopy (TEM) and electron diffraction (ED) techniques. The results show that the diameters of the microspheres range from 2 to 4 μm. The formation mechanism of the morphology control over the copper microspheres assembled by nanoparticles was investigated; the use of polyvinylpyrrolidone (PVP) as the surfactant and the choice of N,N-dimethylformamide (DMF) as the reducing agent were found to be important for the final generation of copper microspheres.     

Hydrothermal synthesis and characterization of nanocrystalline Zn-Mn spinel

Hydrothermal method had been used to successfully synthesize the nanocrystalline spinel zinc manganese oxide (ZnMn₂O₄) directly from Zn(CH₃COO)₂·2H₂O, NaOH, Mn(NO₃)₂ and H₂O₂ at 170 °C for the reaction time of 48 h. The effects of the synthesis conditions, such as the Zn/Mn molar ratio, the reaction temperature, the reaction time, the zinc source and the concentrations of NaOH and H₂O₂, on the formation of the Zn-Mn spinel were investigated. The products were characterized by means of X-ray diffraction (XRD), inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The results indicated that the compositions of the Zn-Mn spinel with the tetragonal structure were Zn_1.14Mn_1.86O₄. Scanning electron microscope (SEM) and transmission electron microscopy (TEM) images showed that the products at 170 °C were with square-shaped nanocrystalline spinel with the particle size of about 20-50 nm. The thermal behaviors of the products were investigated by thermogravimetric analysis (TG).     

Study of flowerlike CeO2 microspheres used as catalyst supports for CO oxidation reaction

Porous flowerlike CeO₂ microspheres were synthesized via a novel hydrothermal method and were used as supports for the oxidation of CO. After loaded with Au or CuO, it exhibited an excellent low-temperature catalytic activity toward CO oxidation reaction. Especially, for the Au-loaded flowerlike CeO₂ microsphere catalyst, CO gas started its conversion into CO₂ above 80% at room temperature. The possible reasons for the superior catalytic activity of flowerlike CeO₂ microsphere catalysts were discussed.     

Preparation and characterization of SnO nanowhiskers

In this paper, some single-crystalline Stannous oxide (SnO) nanowhiskers were successfully prepared by a wet method using SnCl₂·2H₂O as raw material and cetyltrimethylammoniumbromide (CTAB) as surfactant. The morphologies, purity and sizes of the products were characterized by transmission electron microscopy, powder X-ray diffractmetry and standard selected area electron diffraction. The results showed that the diameter and the length of the particles were 10-30 and 200-400 nm, respectively. The influence of some reaction parameters, including the pressure, the temperature, the surfactant and the reaction duration, on the formation, morphology and particle size of SnO crystallite is discussed.     

t-Se microspheres with holes: Hydrothermal synthesis and growth mechanism

In the present paper, novel t-Se microspheres with holes were successfully prepared via a facile solution-phase approach at 150 °C for 20 h, employing SeO₂ and glucose as reagents, poly(vinylpyrrolidone) (PVP) as the surfactant. The phase and morphology of the product were characterized by means of powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The conversion from α-Se to t-Se was investigated by a series of experiments and a possible formation process was suggested based on the experimental results.     

Polishing behavior of PS/CeO2 hybrid microspheres with controlled shell thickness on silicon dioxide CMP

Organic-inorganic composite microspheres with PS as a core and CeO₂ nanoparticles as a shell were synthesized by in situ decomposition reaction of Ce(NO₃)₃ on the surfaces of PS microspheres prepared through soap-free emulsion polymerization. The shell thickness of the composite microspheres could be turned by varying the concentration of Ce(NO₃)₃ in the reaction solution. The whole process required neither surface treatment for PS microspheres nor additional surfactant or stabilizer. The as-synthesized PS/CeO₂ composite microsphere samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Oxide chemical mechanical polishing (CMP) performance of the PS/CeO₂ composite abrasives with different shell thickness was characterized by atomic force microscopy (AFM). The results indicated that the as-prepared core-shell structured composite microspheres (220-260 nm in diameter) possessed thin shell (10-30 nm) composed of CeO₂ nanoparticles (particle diameter of 5-10 nm), and the final CeO₂ contents of the composite microspheres ranged from 10 to 50 wt%. A possible mechanism for the formation of PS/CeO₂ composite microspheres was discussed also. The CMP test results confirmed that the novel core-shell structured composite abrasives are useful to improve oxide CMP performance. In addition, there is an obvious effect of shell thickness of the composite abrasives on oxide CMP performance.     

A facile and environmentally friendly chemical route for the synthesis of metastable VO2 nanobelts

Metastable VO₂ nanobelts, designated as VO₂ (B), were successfully fabricated by a facile hydrothermal route in the presence of V₂O₅ and glucose. The samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM), selected area electronic diffraction (SAED), high-resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM) techniques. The main synthesis parameters such as temperature, reaction time and molar ratio of the starting materials have been also discussed. The results showed that pure B phase VO₂ nanobelts with high crystallinity can be prepared easily at 180 °C in 24 h at the molar ratio of V₂O₅:glucose=1:1. Typically, the belt-like products were 0.6-1.2 μm long, 80-150 nm wide and 20-30 nm thick. It is noted that the whole process is free of any harmful reducing reagents and surfactants, and valuable gluconic acid can be formed as the main by-product. From an economic and environmental point of view, the present approach is particularly fit for the synthesis of VO₂ (B) nanobelts on a large scale.     

Shape-controlled synthesis of CuS nanocrystallites via a facile hydrothermal route

Without the use of any extra surfactant, template or other additive, shape-controlled synthesis of sphere-, urchin- and tube-like CuS nanocrystallites has been realized just via hydrothermal treatment of different amounts of CuSO₄·5H₂O and equimolar Na₂S₂O₃·5H₂O in water at 150 °C for 12 h. The possible mechanism for the formation of the various nanostructures of CuS in this system was discussed.     

Solvothermal preparation and characterization of nanocrystalline Bi2Te3 powder with different morphology

Bi₂Te₃-based alloys are currently best-known, technological important thermoelectric materials near room temperature. In this paper, nanocrystalline Bi₂Te₃ with different morphologies was synthesized by a solvothermal process based on the reaction between BiCl₃, Te, and KBH₄ in N,N-dimethylformamide at 100-180 °C. KBH₄ was used as a reducing agent. The products were characterized by X-ray diffraction and transmission electron microscopy (TEM). The particle morphologies and size are dependent on the reaction temperature and time. A possible formation mechanism is proposed.     

Synthesis of quasi-1D cuprous oxide nanostructure and its structural characterizations

A wealth of superfine polycrystalline cuprous oxide (Cu₂O) nanowires have been synthesized with hydrazine hydrated (N₂H₄·H₂O), act as the reducing agent, and Cu(OH)₂ nanowires, act as a soft template and surfactant, at room temperature. Two methods were employed for the synthesis of these nanowires, i.e. with and without capping agent (polyethylene glycol Mw 8000). Techniques of powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) pattern, electron diffraction X-ray (EDX) spectroscopy, and UV-visible (UV-vis) spectroscopy have been used to characterize the morphology, structure, crystallinity, purity, and composition of nanowires. The average diameters of Cu₂O nanowires, prepared with and without capping agent, were observed to be 8-10 and 12-15 nm and lengths of several microns, respectively. It is found that capping agent (PEG) confines the dimensions of synthesized nanowires. In addition, the observed optical band gap of products show blue-shift effect compared to the bulk Cu₂O (E_g=2.17 eV), which ascribe it as a promising material for the conversion between solar energy and electrical or chemical energy.     

Facile synthesis of monodispersed α-Fe2O3 microspheres through template-free hydrothermal route

Monodisperse α-Fe₂O₃ microspheres have been selectively synthesized through a facile hydrothermal method without the assistance of any surfactant, employing FeCl₃·6H₂O and NH₄NaHPO₄ as initial materials. The products were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. α-Fe₂O₃ microspheres with average size about 250 nm were constructed by single crystalline nanoparticles with average diameter about 15 nm. The investigation on the evolution formation revealed that growth temperature was critical to control the assembly of the fresh formed nanocrystallites, and the microsphere formation was proved to be the Ostwald ripening process by tracking the structures of the products at different growth temperature. α-Fe₂O₃ microspheres showed a weak ferromagnetic behavior with a remanent magnetization of 0.208 emu g⁻¹ and a coercivity of 1,034.27 Oe at room temperature.     

Self-assembly of CuS nanoparticles to solid,hollow, spherical and tubular structures in a simple aqueous-phase reaction

We report fabrication of CuS particles with solid, hollow, spherical and tubular structures in a simple aqueous system under microwave irradiation, employing CuSO₄ and Na₂S₂O₃ as the starting materials without assistance of any surfactant or template. Energy-dispersive X-ray analysis and an X-ray powder diffraction pattern proved that the product is hexagonal CuS phase. The morphologies of the product were observed by scanning electron microscopy and transmission electron microscopy. Some factors affecting the morphologies of the product are discussed. PACS 81.05.Hd; 81.07.Bc; 81.16.Be; 81.16.Dn; 81.20.Ka     

Controlled growth of uniform nanoflakes-built pyrite FeS<Subscript>2</Subscript> microspheres and their electrochemical properties

Nanoflakes-built pyrite FeS₂ microspheres were synthesized through a simple solvothermal process in mixed solvents of N, N-dimethytformamide and ethylene glycol without using any surfactant. Both the composition of the solvents and urea were key factors for the formation of the uniform products. It was found that the flake-like intermediate products transformed into FeS₂ nanoflakes in situ in the early stage and Ostwald ripening growth mechanism would contribute to the uniformity of the final products. Electrochemical studies revealed that the nanoflakes-built pyrite FeS₂ microspheres exhibited large lithium storage capacities. This method can be easily controlled and is expected to be extendable to the fabrication of other metal chalcogenides with controlled shape and structure.     

Reactions of chlorine and related molecules with graphite intercalation compounds

K-graphite intercalation compounds (GICs), metal chloride-GICs and reduced products of CuCl₂-GICs were allowed to react with chlorine. Decomposition of K-GICs took place through the reaction with chlorine. The extent of the decomposition was found to be dependent not on the gas pressure of the chlorine but on the stage number of the starting GIC. Metal chloride-GICs were unreactive with chlorine, whereas chlorine could react with copper particles generated in the interlayer of graphite through the reduction of CuCl₂-GICs. The reaction products were CuCl and CuCl₂; the former exists as crystals in the interlayer, and the latter can form CuCl₂-GICs. Also reported on are reactions of GICs with chlorobenzene, benzoyl bromide and iodine monochloride.     

Pyrolysis synthesis of magnetic - and -MnO2 nanostructures and the polymorph discrimination

The concentration of the Mn(NO₃)₂ solution has significant influence on the morphologies and the phases of the MnO₂ products. A large number of ε- MnO₂ nanowires were prepared via a simple pyrolysis under lower reaction concentration. The nanowires have lengths up to tens of micrometers and diameters in the range of 20–100 nm. The β- MnO₂ nanobundles and nanoflowers were prepared by increasing the concentration of Mn(NO₃)₂ solution. The superparamagnetism of ε- MnO₂ nanowires and paramagnetism of β- MnO₂ nanoflowers indicate their potential applications in magnetic materials.     

Microwave-assisted synthesis of Fe3O4 nanorods and nanowires in an ionic liquid

Without using inert gas to prevent the oxidation of Fe²⁺, Fe₃O₄ nanorods and nanowires have been successfully synthesized via a microwave-assisted ionic liquid method (MAIL). Compared to the traditional methods, the whole reaction process can be carried out more easily and faster. Our result shows that temperature and time of microwave heat played important roles in the formation of Fe₃O₄ with different morphologies. These products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), thermogravimetric analysis (TG) and FT-IR spectra.