Rapid synthesis, characterization and optical properties of TiO2 coated ZnO nanocomposite particles by a novel microwave irradiation method

A novel and rapid microwave method was used to prepare TiO₂ coated ZnO nanocomposite particles. The resulted particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Results show that ZnO nanoparticles were coated with 6-10 nm amorphous TiO₂ layers. In addition, zeta potential analysis demonstrated the presence of TiO₂ layer on the surface of ZnO nanoparticles. Photoluminescence (PL) spectroscopy and UV-visible spectroscopy were used to investigate the optical properties of the nanoparticles. Compared to uncoated ZnO nanoparticles, the TiO₂ coated ZnO nanoparticles showed enhanced UV emission. The UV-visible diffuse reflectance study revealed the significant UV shielding characteristics of the nanocomposite particles. Moreover, amorphous TiO₂ coating effectively reduced the photocatalytic activity of ZnO nanoparticles as evidenced by the photodegradation of Orange G with uncoated and TiO₂ coated ZnO nanoparticles under UV radiation.     

Preparation of Mn2SnO4 nanoparticles as the anode material for lithium secondary battery

The ultrafine Mn₂SnO₄ nanoparticles with diameters of 5-10 nm have been prepared by thermal decomposition of precursor MnSn(OH)₆. The MnSn(OH)₆ nanoparticles precursor was synthesized by a hydrothermal microemulsion method. X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy and electron diffraction have been employed to characterize the crystal structures and morphologies of the as-prepared samples. High-resolution transmission electron microscopy observations revealed that the as-synthesized nanoparticles were single crystals. The thermal characterization was studied by differential thermal analysis and thermogravimetry analysis measurements. Electrochemical test showed that the Mn₂SnO₄ nanoparticles exhibited a high initial charge-discharge capacity of 1320 mAh/g.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Synthesis and characterization of ZnO/SiO2 core/shell nanocomposites and hollow SiO2 nanostructures

In this paper, we prepared the ZnO nanoparticles by a simple hydrothermal method and fabricated the ZnO/SiO₂ core/shell nanostructures through a sol-gel chemistry process successfully. The hollow SiO₂ nanostructures were obtained by selective removal of the ZnO cores. The structure, morphology and composition of the products were determined by the techniques of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). The results indicated that the ZnO nanoparticles were sphere-like shape with the average size of 60 nm and belonged to hexagonal wurtzite crystal structure. With the coating of SiO₂, the vibration modes of Si-O-Si and Si-OH were found. Furthermore, the measurement results of optical properties showed that spectra of bare ZnO nanoparticles and ZnO/SiO₂ core/shell nanocomposites exhibited similar emission features, including a blue emission peak and an orange emission band.     

Preparation N-F-codoped TiO2 nanorod array by liquid phase deposition as visible light photocatalyst

An efficient method for the preparation of N-F-codoped visible light active TiO₂ nanorod arrays is reported. In the process, simultaneous nitrogen and fluorine doped TiO₂ nanorod arrays on the glass substrates were achieved by liquid phase deposition method using ZnO nanorod arrays as templates with different calcination temperature. The as-prepared samples were characterized by Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectra measurements. It was found that calcination temperature is an important factor influencing the microstructure and the amount of N and F in TiO₂ nanorod arrays samples. The visible light photocatalytic properties were investigated using methylene blue (MB) dye as a model system. The results showed that N-F-codoped TiO₂ nanorod arrays sample calcined at 450 °C demonstrated the best visible light activity in all samples, much higher than that of TiO₂ nanoparticles and P25 particles films.     

Preparation of reduced graphene oxide-NiFe2O4 nanocomposites for the electrocatalytic oxidation of hydrazine

A reduced graphene oxide (RGO)-NiFe₂O₄ nanocomposite was synthesized by a simple one step hydrothermal approach and its application in the electrocatalytic oxidation of hydrazine was demonstrated. The as-synthesized nanocomposite was characterized by X-ray diffraction, Fourier transform infrared spectroscopy, UV–visible spectroscopy, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, Thermogravimetric analysis, Field emission-scanning electron microscopy (FE-SEM), and Transmission electron microscopy (TEM). The FE-SEM and TEM image analyses revealed that the NiFe₂O₄ nanoparticles were uniformly distributed on the RGO sheets with a diameter and length of ∼10 and ∼100 nm, respectively. The XPS analysis confirmed the ionic states of Ni and Fe to be Ni³⁺ and Ni²⁺, and Fe²⁺ and Fe³⁺, respectively. Further, the electrochemical activity of the RGO-NiFe₂O₄ nanocomposite was investigated by studying the oxidation of hydrazine. The RGO-NiFe₂O₄ modified glassy carbon electrode (GCE) showed an outstanding electrocatalytic activity towards the oxidation of hydrazine as compared to the NiFe₂O₄ and RGO modified electrodes. The enhanced electrocatalytic activity is due to the synergistic effect between RGO and NiFe₂O₄. Using amperometry, the lowest detection limit of 200 nM was achieved with the RGO-NiFe₂O₄ modified GCE. Therefore, the RGO-NiFe₂O₄ modified GCE can be used for the electrochemical oxidation of hydrazine.     

Popcorn like morphology and absence of room temperature ferromagnetism in Ni doped SnO<Subscript>2</Subscript> nanoparticles

Ni-doped SnO₂ nanoparticles were synthesized by the microwave oven assisted solvothermal method. The structural characterization was done by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy. The outcomes confirmed that Ni-doped SnO₂ nanoparticles have a pure rutile-type tetragonal phase of SnO₂ structures with a high degree of crystallization and a crystallite size of 10–14 nm. Popcorn like SEM morphology of the nickel doped sample is shown. Optical characterization was done by UV–Vis spectrometer, fluorescence spectroscopy and electron paramagnetic resonance spectroscopy. Magnetic characterization was done by vibrating sample magnetometer (VSM). The VSM measurements revealed that the Ni doped SnO₂ powder samples were diamagnetic at room temperature. This diamagnetic result is in contradiction to earlier published results.     

Preparation of carbon nanotube-neodymium oxide composite and research on its catalytic performance

Carbon Nanotube-Neodymium Oxide (CNT-Nd₂O₃) composite was prepared by using acid treated carbon nanotubes (CNTs) and neodymium nitrate in the presence of sodium dodecyl sulfate and ammonia liquid. Techniques of transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and differential thermal analysis (DTA) are used to characterize the morphology, structure, composition and catalytic property of the CNT-Nd₂O₃ composite. The experimental results show that the Nd₂O₃ nanoparticles, which have an average diameter of about 30-40 nm, are loaded on the surface of carbon nanotube. Compared with pure Nd₂O₃ nanorods, the CNT-Nd₂O₃ composite can catalyze the thermal decomposition of ammonium perchlorate more effectively. The sampling methods of the experimental samples made a difference on the catalytic experiment results, and the best catalytic result was obtained when de-ionized water served as the solvent of ammonium perchlorate.     

Catalytic synthesis of large-scale GaN nanorods

A novel rare earth metal seed was employed as the catalyst for the growth of GaN nanorods. Large-scale GaN nanorods were synthesized successfully through ammoniating Ga₂O₃/Tb films sputtered on Si(1 1 1) substrates. Scanning electron microscopy, X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, and X-ray photoelectron spectroscopy were used to characterize the structure, morphology, and composition of the samples. The results demonstrate that the nanorods are high-quality single-crystal GaN with hexagonal wurtzite structure. The growth mechanism of GaN nanorods is also discussed.     

Luminescence response and CL degradation of combustion synthesized spherical SiO2:Ce nanophosphor

This study was aimed to systematically investigate the luminescence response of SiO₂:Ce³⁺ nanophosphors with different excitation sources. The powders were synthesized by using an urea assisted combustion method. SiO₂:Ce_1m% samples were also annealed at 1000 °C for 1 h in a charcoal environment to reduce incidental Ce⁴⁺ to partial Ce³⁺ ions. High resolution transmission electron microscopy (HRTEM) images of the as synthesized and annealed powder samples confirmed that the particles were spherical and in the size range of 3-8 nm in diameter. X-ray diffraction (XRD) and electron dispersion spectroscopy (EDS) results showed that the SiO₂ was crystalline and pure. Diffused reflectance, photoluminescence (PL) and cathodoluminescence (CL) results of the SiO₂:Ce³⁺ samples were obtained and compared with each other. The CL degradation and the surface reactions on the surface of the SiO₂:Ce³⁺ were studied with X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). A clear improvement in the chemical stability of the SiO₂:Ce³⁺ annealed at 1000 °C were obtained.     

Fabrication of nanocomposite particles with superparamagnetic and luminescent functionalities

A new kind of superparamagnetic luminescent nanocomposite particles has been synthesized using a modified Stöber method combined with an electrostatic assembly process. Fe₃O₄ superparamagnetic nanoparticles were coated with uniform silica shell, and then 3-aminopropyltrimethoxysilane was used to terminate the silica surface with amino groups. Finally, negatively charged CdSe quantum dots (QDs) were assembled onto the surface of the amino-terminated SiO₂/Fe₃O₄ nanoparticles through electrostatic interactions. X-ray diffraction (XRD), transmission electron microscopy (TEM), microelectrophoresis, UV-vis absorption and emission spectroscopy and magnetometry were applied to characterize the nanocomposite particles. Dense CdSe QDs were immobilized on the silica surface. The thickness of silica shell was about 35 nm and the particle size of the final products was about 100 nm. The particles exhibited favorable superparamagnetic and photoluminescent properties.     

Fabrication and photocatalysis of mesoporous ZnWO4 with PAMAM as a template

Mesoporous ZnWO₄ was prepared with the template of PAMAM. The as-formed samples were characterized by X-ray diffraction (XRD), nitrogen absorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-vis diffuse reflectance spectroscopy (DRS). It is found that the size of pore is in the range of 5-22 nm and that the porosity of ZnWO₄ is composed of aggregated ZnWO₄ nanoparticles. The photocatalytic activities towards degradation of rhodamine B (RhB) and malachite green (MG) under UV light has been investigated. The formation mechanism of mesoporous structures is proposed.     

La-doped ZnO nanoparticles: Simple solution-combusting preparation and applications in the wastewater treatment

La-doped ZnO nanoparticles have been successfully synthesized by a simple solution combustion method via employing a mixture of ethanol and ethyleneglycol (v/v = 60/40) as the solvent. Zinc acetate and oxygen gas in the atmosphere were used as zinc and oxygen sources, and La(NO₃)₃ as the doping reagent. The as-obtained product was characterized by means of powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectrometry and X-ray photoelectron spectroscopy. Experiments showed that La-doped ZnO nanoparticles exhibited the higher capacities for the removal of Pb²⁺ and Cu²⁺ ions in water resource than undoped ZnO nanoparticles.     

Morphology-controlled synthesis of ZnS nanostructures via single-source approaches

ZnS nanoparticles of various morphologies, including hollow or solid spherical, and polyhedral shape, were synthesized from single-source precursor Zn(S₂COC₂H₅)₂ without using a surfactant or template. The as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy. The results indicate that ZnS hollow and solid spheres assembled by nanoparticles can be easily generated by the solution phase thermalysis of Zn(S₂COC₂H₅)₂ at 80 °C using N, N-dimethylformamide (DMF) and ethylene glycol (EG) or water as solvents, respectively, whereas solvothermal process of the same precursor led to ZnS nanoparticles of polyhedral shape with an average size of 120 nm. The optical properties of these ZnS nanostructures were investigated by room-temperature luminescence and UV-vis diffuse reflectance spectra.     

Synthesis,characterization and growth mechanism of ZnO nanowires on NiCl<Subscript>2</Subscript>-coated Si substrates

Well-crystallized ZnO nanowires have been successfully synthesized on NiCl₂-coated Si substrates via a carbon thermal reduction deposition process. The pre-deposited Ni nanoparticles by dipping the substrates into NiCl₂ solution can promote the formation of ZnO nuclei. The as-synthesized nanowires were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and photoluminescence (PL) spectrum. The results demonstrate that the as-fabricated nanowires with about 60 nm in diameter and several tens of micrometers in length are preferentially arranged along [0001] direction with (0002) as the dominate surface. Room temperature PL spectrum illustrates that the ZnO nanowires exist a UV emission peak and a green emission peak, and the peak centers locate at 387 and 510 nm. Finally, the growth mechanism of the nanowires is briefly discussed.     

Synthesis of Se nanoparticles by using TSA ion and its photocatalytic application for decolorization of cango red under UV irradiation

In this study, we describe a size-controlled synthesis of selenium nanoparticles based on the reduction of selenious acid (H₂SeO₃) by UV-irradiated tungstosilicate acid (H₄SiW₁₂O₄₀, TSA) solution which serves both as reducing reagent and stabilizer. The nanoparticles are characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS), the Raman spectra, transmission electron microscopy (TEM) and Zetasizer, respectively. The characteristic catalytic behavior of the Se nanoparticles is established by studying the decolorization of cango red in the presence of UV light. It is obvious that selenium catalyzes the reaction efficiently. The results show that the rate of dye decolorization varies linearly with the nanoparticle concentration and the rate of dye decolorization decreases with the size of the Se nanoparticles increasing.     

TiO2 supported on rod-like mesoporous silica SBA-15: Preparation, characterization and photocatalytic behaviour

TiO₂ nanoparticles have been successfully incorporated in the pores of mesoporous silica SBA-15 with different morphologies by a wet impregnation method. The composites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), inductively coupled plasma (ICP) emission spectroscopy, transmission electron microscopy (TEM), N₂-sorption and UV-Vis diffuse reflectance spectroscopy. The photodegradation of methyl orange (MO) was used to study their photocatalytic property. It is indicated that the morphology of SBA-15 had a great influence on the photocatalytic activity of the composites. When TiO₂/SBA-15 composite was prepared by loading TiO₂ nanoparticles on uniform rod-like SBA-15 of 1 μm length, it showed higher photocatalytic degradation rate than that on less regular but much larger SBA-15 support. This difference was rationalized in terms of the homogeneously distributed and shorter channels of rod-like SBA-15, which favored mass transport and improved the efficient utilization of the pore surface.     

Preparation and characterization of nanometer-scale powders ceria by electrochemical deposition method

Ceria (CeO₂) nanoparticles of 10-30 nm in average particle size have been synthesized via electrochemical deposition method in cerium(III) chloride solution with an undivided cell as electrochemical cell and ethanol-acetylacetone as additives. X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation infrared spectroscopy (FT-IR) and thermal analysis (TG-DTA) are introduced to characterize the samples. The results indicate that the as-prepared powders after being treated at 650 °C are nanocrystalline with the cubic fluorite structure and the sphericity in shape. It is revealed that the size of ceria nanoparticles can be decreased effectively by adding the ethanol-acetylacetone solution. In addition, the possible formed mechanism of CeO₂ nanometer-scale powder. The role of additive is also investigated in this paper.     

Preparation and photoluminescence study of mesoporous indium hydroxide nanorods

Mesoporous indium hydroxide nanorods were successfully synthesized by a mild one-step one-pot method. The obtained samples were characterized by X-ray diffraction, transmission electron microscopy with selected area electron diffraction, N₂ adsorption, ultraviolet-visible absorption and photoluminescence, respectively. Transmission electron microscopy showed that there were some pores in the samples, which were mainly composed of rod-like shapes with length of 300 nm and diameter of 90 nm. N₂ adsorption/desorption measurements confirmed that the prepared powder was mesoporous with average pore diameter of 3.1 nm. The ultraviolet-visible absorption spectroscopy analysis indicated that the band gap energy of the samples was 5.15 eV. Photoluminescence spectrum showed that there were two strong emissions under ultraviolet light irradiation. The growth mechanism of indium hydroxide nanorods and the role of cetyltrimethyl ammonium bromide were also discussed.     

Preparation of monodispersed cobalt-boron spherical nanoparticles and their behavior during the catalytic decomposition of hydrous hydrazine

Monodispersed cobalt-boron spherical nanoparticles have been prepared through solution plasma processing in the presence of hexadecyltrimethyl ammonium bromide for the first time. The particle size of cobalt-boron can be adjusted by changing either the plasma time or the concentration of hexadecyltrimethyl ammonium bromide. The samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. During the decomposition of hydrous hydrazine, the obtained monodispersed cobalt-boron spherical nanoparticles exhibit higher catalytic activity and hydrogen selectivity than regular cobalt-boron prepared by direct reduction of Co²⁺ with BH₄⁻. The experimental investigations indicate that hydrous hydrazine along with the monodispersed cobalt-boron spherical nanoparticles may find application in small-scale on-board hydrogen storage and supply.