Solvothermal synthesis of nanorods of ZnO, N-doped ZnO and CdO

ZnO nanorods with diameters in the 80-800 nm range are readily synthesized by the reaction of zinc acetate, ethanol and ethylenediamine under solvothermal conditions. The best products are obtained at 330 °C with a slow heating rate. Addition of the surfactant Triton^®-X 100 gave nanorods of uniform (300 nm) diameter. By adding a small amount of liquid NH₃ to the reaction mixture, N-doped ZnO nanorods, with distinct spectroscopic features are obtained. CdO nanorods of 80 nm diameter have been prepared under solvothermal conditions using a mixture of cadmium cupferronate, ethylenediamine and ethanol at 330 °C. Similarly, Zn_1−xCd_xO nanorods of a 70 nm diameter are obtained under solvothermal conditions starting with a mixture of zinc acetate, cadmium cupferronate, ethanol and ethylenediamine.     

Preparation and characterization of CuO nanorods by thermal decomposition of CuC2O4 precursor

Synthesis of copper oxide (CuO) nanorods was achieved by thermal decomposition of the precursor of CuC₂O₄ obtained via chemical reaction between Cu(CH₃COO)₂·H₂O and H₂C₂O₄·2H₂O in the presence of surfactant nonyl phenyl ether (9)/(5) (NP-9/5) and NaCl flux. Transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), selected-area electron diffraction (SAED) and high-resolution TEM (HRTEM) were used to characterize the structure features and chemical compositions of the as-made nanorods. The results showed that the as-prepared nanorods is composed of CuO with diameter of 30-100 nm, and lengths ranging from 1 to 3 μm. The mechanism of formation of CuO nanorods was also discussed.     

Generation of gold-PEDOT nanostructures at an interface between two immiscible solvents

Gold-poly(3,4-)ethylenedioxythiophene (Au-PEDOT) composite with variant morphology was synthesized through interfacial polymerization at room temperature in the absence of a template, phase transfer catalyst or surfactant. A systematic variation of the relative concentration of the reactants yields morphologies typical of nanorods of diameter approximately 20-30 nm and length of few 0.5-1 μm. Transmission electron microscopy reveals the structure of the nanowire to be the one in which the core is Au and the outer shell is made of PEDOT. Oligomer formation, speculated during the interfacial reaction was confirmed by the analysis of the organic phase using ultraviolet-visible (UV-vis) and nuclear magnetic resonance (NMR) spectroscopy techniques.     

Sub-micrometer sized yttrium oxide fibers prepared through hydrothermal reaction

Yttrium oxide fibers have been synthesized via hydrothermal reaction and subsequent thermal treatment using yttrium chloride as precursor. The products before and after the thermal treatment were characterized by powder X-ray diffractions (XRD), scanning electron microscopy (SEM), ion-chromatograph analysis, and thermogravimetry and differential thermal analysis (TG-DTA). The fiber diameter ranged from 100 to 300 nm, while the length was up to tens of microns. It was found that the chemical composition and morphology of the products were closely related to the pH value of reaction solution, and fibrous products could be obtained at pH 9.5-10.25. These oxide fibers exhibited outstanding high-temperature stability, which maintained their morphology at temperature up to 1400 °C.     

Controlled fabrication of SrMoO4 hierarchical nanosheets in a surfactant-assisted nonaqueous system

Various hierarchical architectures of SrMoO₄ nanosheets (thickness of 8-9 nm) have been successfully prepared in nonaqueous system by a surfactant-assisted solvothermal method. X-ray powder diffraction, scanning electron microscopy and transmission electron microscopy were employed to study the crystal structure and morphologies of the products. Experiments showed that the solvent, surfactant, reaction temperature and reaction time were crucial for the oriented aggregation of the SrMoO₄ nanosheets. Morphological control of these parameters resulted in platelet, column, interlaced multilayer and nest of nanosheets. A possible growth mechanism for these hierarchical architectures has also been proposed according to the morphological evolution with the reaction time. The optical properties of the products were also examined by means of photoluminescence and excitation spectroscopy. Photoluminescence studies revealed that these SrMoO₄ nanocrystals exhibited a greatly strong blue emission under 325-nm excitation with different intensities but centered at the same position of 474 nm.     

Hydrothermal synthesis of nanocrystalline VO2 from poly(diallyldimethylammonium) chloride and V2O5

Novel vanadium dioxide nanorods were fabricated from V₂O₅ in the presence of a reducing agent, the poly(diallyldimethylammonium chloride) (PDDA) via a hydrothermal method at 180 °C for 48 h. The samples produced were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), infrared spectroscopy (FTIR), nitrogen adsorption (BET) and thermogravimetry (TG/DTG). The nanorods obtained are approximately 50 nm wide and from 300 to 500 nm long and presents high surface area (42 m² g⁻¹). The nanocrystalline B phase VO₂ is not produced by hydrothermal treatment in the absence of the PDDA polyelectrolyte.     

PEG-300 assisted hydrothermal synthesis of 4ZnO·B2O3·H2O nanorods

4ZnO·B₂O₃·H₂O is commonly used as a flame-retardant filler in composite materials. The microstructure of the powder is of importance in its applications. In our study, for the first time, one-dimensional (1D) nanostructure of 4ZnO·B₂O₃·H₂O with rectangle rod-like shape has been synthesized by a hydrothermal route in the presence of surfactant polyethylene glycol-300 (PEG-300). The nanorods have been characterized by X-ray powder diffraction (XRD), inductively coupled plasma with atomic emission spectroscopy (ICP-AES), thermogravimetry (TG) and differential thermal analysis (DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) equipped with selected area electron diffraction (SAED) as well as high-resolution transmission electron microscopy (HRTEM). These nanorods are about 70 nm in thickness, 150-800 nm in width and have lengths up to a few microns. 4ZnO·B₂O₃·H₂O nanorods crystallize in the monoclinic space group P2₁/m, a = 6.8871(19) Å, b = 4.9318(10) Å, c = 5.7137(16) Å, β = 98.81(21)° and V = 191.779(71) Å³.     

Mass-synthesized anatase titania nanocrystals with tunable size and shape via sol-gel in organic solvents with adsorbing ligands

High-quality anatase titania (TiO₂) nanoparticles, nanowires, and nanorods have been mass-synthesized by the modified sol-gel method in the saturated fatty alcohol, acid, and amine systems with adsorbing ligands, respectively. These obtained quasi-spherical TiO₂ nanoparticles showed the mean size of 16.5 nm with a narrow size-distribution. These resulting TiO₂ nanowires had the uniform diameter of 3.8 nm with the length range of 80-180 nm, and TiO₂ nanorods had the uniform diameter of 7.5 nm with the length range of 40-70 nm, respectively. We demonstrated that the shapes, sizes and morphology of these anatase TiO₂ nanocrystals could be controlled systematically by adjusting certain reaction parameters, such as the kind of organic solvents, the alkyl length of organic solvents, and the reaction time. It has been found that the shape of the products was primarily determined by the kind of organic solvents. However, their sizes, size-distributions, and morphology could be controlled by adjusting the alkyl length of organic solvents and the reaction time. Based on the analysis of all experiment results, we have investigated the growth mechanism of these TiO₂ nanocrystals with the different shape. Meanwhile, this synthetic method can be extended further for the preparation of other oxides nanocrystals.     

Synthesis of carbon micro-rods via a solvothermal route

Novel carbon micro-rods with regular and uniform shape have been synthesized in high yield by magnesium acetate and n-butyl alcohol as the precursors via a solvothermal route. The resulting products were characterized by combined techniques including X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) and Raman spectroscopy. The carbon micro-rods exhibit diameters ranging from 500 nm to 1 μm and up to 5-10 μm in length. We have found that the optimal reaction conditions for the growth of the carbon micro-rods were 500 °C and 12 h.     

Solid-CdS and hollow-ZnS porous submicrospheres: Direct preparation by C-S decomposition of thiol via solvothermal processing

Porous solid-CdS or hollow-ZnS submicrospheres (SMSs) were prepared by reaction of 2-mercaptoethanol as S-source with Cd²⁺ or Zn²⁺ in ethanol using solvothermal route. Without any alkaline, solid-CdS SMSs with an average diameter of 440 nm were obtained and their size distribution in the range of 390-490 nm is above 80%; With the addition of alkaline, single crystal CdS nanorods with high-temperature-stable hexagonal phase were synthesized. With or without poly(N-vinyl-2-pyrrolidone) (PVP), solid-CdS SMSs can be prepared, but the addition of the PVP leads to the preparation of relative uniform CdS-SMSs. Hollow-ZnS SMSs with an average diameter of 340 nm were obtained under the existence of alkaline. The longer reaction time hardly influences on the size of the hollow-ZnS SMSs. More or less amount of alkaline directly influences the morphology of final product. Close-ring-shaped ZnS was prepared under the existence of less alkaline. With or without PVP under preparation reaction, hollow-ZnS SMSs can also be synthesized. Thus, during preparation of either CdS or ZnS, the PVP function is not as template, but as surfactant. The BET measurement results show that the special surface areas of solid-CdS and hollow-ZnS SMSs are 25.56 and 83.55 m²/g, respectively. The adsorption of methylene blue shows that the hollow-ZnS SMSs have very strong adsorption and decomposition ability.     

The effects of addition of citric acid on the morphologies of ZnO nanorods

ZnO nanorods of 25-100 nm in diameter and 0.2-1 μm in length were fabricated through citric acid assisted annealing process. The microstructure of ZnO nanorods was characterized by X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy and field-emission scanning electron microscopy, respectively. As a result, it was found that ZnO nanorods were single crystalline and pure. The effects of the growth conditions such as addition of citric acid, annealing temperature on the morphologies of ZnO nanostructures have also been investigated. At the given temperature the length decreased but the diameter increased with addition of the mass of citric acid. With the rising of the calcining heat, the shape of ZnO changed from rod to granule for a given amount of citric acid. Finally, the mechanism for citric acid assisted annealing synthesis of the ZnO nanostructure is discussed.     

Synthesis of uniform nano-structured lead oxide by sonochemical method and its application as cathode and anode of lead-acid batteries

This paper discusses the results of a research aimed at investigating the synthesis of nano-structured lead oxide through reaction of lead nitrate solution and sodium carbonate solution by the sonochemical method. At the first, lead carbonate was obtained in a synthesized solution and then, after filtration, it was calcinated at the temperature of 320 °C so that nano-structured lead oxide can be produced. The effects of different parameters on particle size and morphology of final lead oxide powder were optimized by a “one at a time” method. The prepared lead oxide powder was characterized by scanning electron microscopy (SEM), transmission electron spectroscopy (TEM) and X-ray diffraction (XRD). Under optimum conditions, uniformed and homogeneous nano-structured lead oxide powder with more spongy morphology and particle size of 20-40 nm was obtained. The synthesized lead oxide, as anode and cathode of lead-acid batteries, showed an excellent discharge capacity (140 mA h/g).     

A novel synthetic route to prepare cubic BN nanorods

Cubic boron nitride nanorods were prepared at 450°C by a low pressure benzene thermal synthesis method using BCl₃ and Li₃N as the reactants. The nanorods with various lengths and diameters were observed by transmission electron microscopy. The analysis of X-ray diffraction pattern and electron diffraction pattern revealed that the nanorods are cBN with a lattice constant of 3.62 Å. The Fourier transformation infrared spectra showed that the dominant phase is cBN, and the B:N ratio of 1.15:1 can be obtained from the X-ray photoelectron spectrum.     

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.     

Synthesis and characterization of ZnS nanowires by AOT micelle-template inducing reaction

ZnS nanowires, with diameters around 30 nm and lengths up to 2.5 μm, had been successfully synthesized from solutions containing an anionic surfactant, sodium bis(2-ethylhexyl)sulfosuccinate (AOT). Powder X-ray diffraction (XRD) pattern, energy-dispersive X-ray spectroscopy (EDS) and selected-area electron diffraction (SAED) pattern indicated that the product was pure polycrystalline cubic-phase β-ZnS. The morphology and size of the as-synthesized product were determined by the transmission electron microscopy (TEM). The effects of some of the key reaction parameters (such as the ratio of surfactant to water, the reactant concentration and reaction temperature, etc.) had been explored in this paper. A growth mechanism of ZnS nanowires by micelle-template inducing reaction was also proposed.     

Tin dioxide nanoparticles: Reverse micellar synthesis and gas sensing properties

Tin dioxide (SnO₂) nanoparticles have been synthesized by reverse micellar route using cetyltrimethyl ammoniumbromide (CTAB) as the surfactant. Monophasic tin dioxide (SnO₂) was obtained using NaOH as the precipitation agent at 60 °C, however, when liquor NH₃ was used as precipitating agent then crystalline SnO₂ nanoparticles are obtained at 500 °C. SnO₂ prepared using NaOH show crystallite size of 4 and 12 nm after heating at 60 and 500 °C respectively using X-ray line broadening studies. Transmission electron microscopy (TEM) studies show agglomerated particles of sizes 70 and 150 nm, respectively. The grain size was found to be 6-8 nm after heating the precursor obtained (using liquor NH₃) at 500 °C by X-ray line broadening and the TEM studies. Dynamic light-scattering (DLS) studies show the aggregates of SnO₂ nanoparticles with uniform size distribution. Mössbauer studies show an increase of s-electron density at the Sn sites compared to bulk SnO₂ and a finite quadrupole splitting indicative of lowering of symmetry around tin atoms. The gas sensing characteristics have also been investigated using n-butane which show high sensitivity and fast recovery time.     

Growth of PbS nanopyramidal particulate films for potential applications in quantum-dot photovoltaics and nanoantennas

We report a simple interfacial process called the liquid-liquid interface reaction technique (LLIRT) that leads to the formation of nanosized PbS particulate films with hitherto unreported pyramidal morphology. The resultant PbS films were characterized by transmission electron microscopy (TEM) with selected area electron diffraction (SAED), X-ray diffractometery (XRD), atomic force microscopy (AFM), near field scanning optical microscopy (NSOM) and UV-vis spectroscopy. The pyramidal morphology is speculated to originate from the preferred orientation of the 2 2 0 plane of cubic PbS. Our nanopyramidal PbS particulate films display remarkably sharp excitonic peak centered around 656 nm that accounts for a band gap of 1.8 eV suggesting, in turn, their potential application in QD photovoltaics. Interestingly, the feasibility of such nanopyramids to potentially act as nanoantennas (as revealed by the NSOM) is also suggested.     

pH-dependant structural and morphology evolution of Ni(OH)2 nanostructures and their morphology retention upon thermal annealing to NiO

Nickel hydroxide nanosheets, nanobelts and nanorods were prepared by hydrothermal treatment of the precipitates obtained at different pH values. The morphology and crystal structure of the products could be controlled simply by adjusting the pH value at precipitation. Interconnected nanosheets of hexagonal β-Ni(OH)₂ with thickness around 10–20 nm were formed at pH ∼ 11, whereas nanobelts with typical widths around 40–80 nm, and nanorods with diameters around 50–60 nm of phase pure α-Ni(OH)₂ containing intercalated sulphate ions were obtained in the pH range ∼9.5–8.5. Thermal annealing of the hydroxides at 500 °C yielded cubic phase NiO with morphologies similar to their hydroxide precursors. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and energy dispersive X-ray (EDX) analysis were used to characterize the as-prepared products. The role of pH in controlling the phase and morphology of the products was discussed.     

Template-free hydrothermal synthesis of PbS nanorod by the oriented attachment mechanism

In this work, PbS nanocubes and nanorods were fabricated via a facile hydrothermal method without using any template and surfactant. The structure and morphology of as-prepared PbS nanocrystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and high-resolution transmission electron microscopy (HRTEM). It was found that the anisotropic structure of PbS nanorods were composed of numerous assembled nanocubes, which had an uniform morphology with the mean diameters of about 100-200 nm and lengths of 0.5-7 μm. Furthermore, a possible growth mechanism was proposed to explain the formation of the nanorods on the basis of the time-dependent experimental results.     

Synthesis and gas sensing characteristics of SnO2 “dandelions”

SnO₂ dandelions-like architectures that composed of numerous one-dimensional tetragonal prism nanorods were synthesized by a simple hydrothermal method with the help of the surfactant poly(vinyl pyrrolidone) (PVP). The structure and morphology of resulting samples were characterized by means of X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FESEM). The results show that diameter of as-synthesized nanorods are less than 50 nm. The sensors fabricated from the SnO₂ nanorods exhibited good sensitivity, high selectivity and rapid response and recovery times to ethanol vapors at 280 °C.