Well‐defined Sb2S3 nanostructures: citric acid‐assisted synthesis,electrochemical hydrogen storage properties

Well‐defined (three‐dimensional) 3‐D dandelion‐like Sb₂S₃ nanostructures consisted of numerous nanorods have been achieved via a facile citric acid‐assisted solvothermal process. The as‐prepared products were characterized by X‐ray diffraction (XRD), field‐emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and high‐resolution TEM (HRTEM), respectively. The influence factors of the formation of the hierarchical Sb₂S₃ nanostructures are discussed in details based on FESEM characterizations. By simply controlling the quantity of citric acid, the nucleation and growth process can be readily tuned, which brings the different morphologies and nanostructures of the final products. On the basis of a series of contrastive experiments, the aggregation‐based process and anisotropic growth mechanism are reasonably proposed to understand the formation mechanism of Sb₂S₃ hierarchical architectures with distinctive morphologies including nanorods, and dandelion‐like nanostructures. Charge‐discharge curves of the obtained Sb₂S₃ nanostructures were measured to investigate their electrochemical hydrogen storage behaviors. It revealed that the morphology played a key role on the hydrogen storage capacity of Sb₂S₃ nanostructure. The dandelion‐like Sb₂S₃ nanostructures exhibited higher hydrogen storage capacity (108 mAh g⁻¹) than that of Sb₂S₃ nanorods (95 mAh g⁻¹) at room temperature.     

Low temperature synthesis of spindle‐like ZnO nanostructures under microwave irradiation

A simple and general microwave route is developed to synthesize nanostructured ZnO using Zn(acac)₂·H₂O (acac = acetylacetonate) as a single source precursor. The reaction time has a great influence on the morphology of the ZnO nanostructures and an interesting spindle‐like nanostructure is obtained. The microstructure and morphology of the synthesized materials are investigated by X‐ray diffraction (XRD), scanning electron microscopy (SEM), field‐emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high‐resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). It is found that all of them with hexagonal wurtzite phase are of single crystalline structure in nature. Ultraviolet–visible (UV‐vis) absorption spectra of these ZnO nanostructures are investigated and a possible formation mechanism for the spindle‐like ZnO nanostructures is also proposed.     

Facile solvothermal synthesis,growth mechanism and thermoelectric property of flower‐like Bi2Te3

Hierarchical flower‐like Bi₂Te₃ was synthesized through a facile solvothermal method. The crystal structure and morphology of the as‐prepared samples were characterized by X‐ray diffraction (XRD), filed emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and high resolution TEM. The reaction parameters such as reaction time, the amount of glucose, concentration of NaOH and the reaction temperature were systematically investigated. Based on the FESEM observations, a possible mechanism defined as a self‐assembly process accompanied by anisotropic growth mechanism was proposed. Moreover, the thermoelectric properties were measured at the temperature range of 300–600 K. The hierarchical flower‐like Bi₂Te₃ presented good thermoelectrical properties. The maximum ZT value reached up to 0.6 at 600 K, which was higher than that of Bi₂Te₃ nanoparticles.     

Synthesis of TiO2 nanorings and nanorods on TCO substrate by potentiostatic anodization of titanium powder

Various TiO₂ nanostructures, such as nanorings, nanorods were synthesized via potentiostatic anodization of titanium powder under different conditions. The morphology of the obtained TiO₂ nanostructures can be easily tuned by varying applied voltage. The crystal structure, compositional information and morphological structures were characterized by X‐ray diffraction (XRD), X‐ray photoelectron spectra (XPS) and field emission scanning electronic microscopy (FESEM). XRD and XPS analysis confirmed the anodization products were TiO₂. A possible formation mechanism was suggested on the basis of the shape evolution of TiO₂ nanostructures observed by FESEM. The results revealed that the applied voltage played an important role in the formation of various nanostructures. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Controlled synthesis of various morphologies of nanostructured zinc oxide: flower,nanoplate, and urchin

Nanoplates, flower‐like nanostructure of ZnO were successfully synthesized by employing ZnSO₄·7H₂O, NaOH as the starting materials at 120°C under hydrothermal condition. Keeping the same parameters, ZnO urchin shape was obtained by addition of vitamin C at 190°C. Characterizations were carried out by X‐ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) at room temperature. Selected area electron diffraction (SAED) pattern confirms that the product is single crystalline nature. The possible formation mechanisms for synthesized ZnO nanosturcture with various morphologies have also been proposed. PL spectrum from the ZnO flower‐like structures reveals weak UV emission and strong green emission. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis of highly‐ordered hierarchical ZnO nanostructures and their application in dye‐sensitized solar cells

In order to improve the performance of ZnO‐based solar cells, highly‐ordered hierarchical ZnO nanostructures were design and fabricated. The hierarchical nanostructures were grown on FTO (fluorine doped tin oxide, SnO₂:F) glass substrates via a facile, low‐temperature, and low‐cost chemical route. The morphology and structure of the obtained products has been confirmed by field‐emission scanning electron microscopy and X‐ray diffraction measurements. The performance investigation of the prepared dye‐sensitized solar cells (DSSCs) demonstrates that the hierarchical ZnO nanostructure‐based solar cell shows a higher short‐circuit current density compared with the ZnO nanowire counterpart. The enhanced current density may be due to the fact that the surface area of the hierarchical nanostructures is increased. These results indicate that hierarchical ZnO nanostructures are more suitable for the application as photoelectrode of DSSCs. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis of spindle‐shaped α‐FeOOH and α‐Fe2O3 nanocrystals

Spindle‐shaped α‐FeOOH nanocrystals were facilely synthesized using a poly (vinyl pyrrolidone) (PVP)‐assisted route under hydrothermal conditions. The chemical compositions and morphol‐ogies of the as‐prepared samples were characterized in detail by X‐ray power diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscope (TEM). The experimental results reveal that these spindle‐shaped α‐FeOOH nanocrystals have self‐organized into assemblies with hierarchical nanostructures. The crucial roles of PVP in the hydrothermal synthesis of hierarchical α‐FeOOH nanostructures were discussed. The possible formation mechanism was also suggested. Moreover, the spindle‐shaped α‐Fe₂O₃ nanocrystals could be easily obtained after calcining the α‐FeOOH prepared by the PVP‐assisted hydrothermal process. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Facile morphology‐controlled hydrothermal synthesis of flower‐like self‐organized ZnO architectures

Flower‐like self‐organized crystalline ZnO architectures were obtained through a facile and controlled hydrothermal process. As‐synthesized products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), high‐resolution transmission electron microscopy (HRTEM), X‐ray diffraction (XRD), electron diffraction and UV‐Vis spectroscopy. XRD and electron diffraction results confirmed the obtained materials are pure wurtzite ZnO. The effects of different ratios of starting materials and solvent on the morphologies of ZnO hydrothermal products were also evaluated by SEM observations. It is suggested that the use of water, rather than ethanol as the solvent, as well as employing a precursor of Zn(Ac)₂ and 2NaOH (v/v) in hydrothermal reactions are responsible for the generation of specific flower‐like self‐assembled ZnO structures. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Controllable synthesis of hierarchical strontium molybdate by sonochemical method

Large‐scale chrysanthemum‐like strontium molybdate (SrMoO₄) with hierarchical structure has been successfully synthesized via a facile and fast ultrasound irradiation approach at room temperature. By varying the experimental conditions, SrMoO₄ with different morphologies, such as spindles, peanuts, spheres, and rods, can be obtained. The products are characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected‐area electron diffraction (SAED). The influent parameters including concentration, pH value, and surfactants have been investigated. A possible growth mechanism is proposed and the shape evolution of the products is characterized. The as‐prepared chrysanthemum‐like SrMoO₄ particles are used as the precursor for electrorheological fluid and their electrorheological property is investigated.     

Bioinspired synthesis of morphologically controlled SrCO3 superstructures by natural gum acacia

Crystallization of strontium carbonate is performed in aqueous solution using Gum Acacia (GA) as crystal growth modifier. A novel study of hierarchical assembly, specifically interacting inorganic and natural component without introduction of other additives was studied. SrCO₃structures exhibiting the morphologies of well defined nanocrystallites in the form of clusters of hexagonal rods, flower shaped, cross like, doughnut shaped and rice grain shaped are identified by optimizing the conditions and concentration of GA. In continuation, morphology was also examined for mixed metal carbonates (Sr‐LaCO₃, Sr‐TbCO₃). The results indicate that –OH, –COOH and ‐NH₂ functional group moieties of GA play a remarkable role in inhibiting growth morphology of metal carbonates and mixed metal carbonates. Structural characterization of the synthesized materials was investigated by Powder X‐ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive analysis (EDAX), Transmission electron microscopy (TEM), Thermogravimetric analysis (TGA) coupled Mass (MS) and Fourier transform infrared spectroscopy (FT‐IR). This synthesis method can be easily extended to a variety of inorganic nanoparticles, thereby enabling exact control over material properties. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Low‐temperature urea‐assisted hydrothermal synthesis of Bi2S3 nanostructures with different morphologies

Different morphologies of single‐crystalline orthorhombic phase bismuth sulfide (Bi₂S₃) nanostructures, including sub‐microtubes, nanoflowers and nanorods were synthesized by a urea‐assisted hydrothermal method at a low temperature below 120 °C for 12 h. The as‐synthesized powders were characterized by X‐ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high‐resolution transmission electron microscopy (HRTEM) and UV‐vis spectrophotometry. The experimental results showed that the sulfur sources had a great effect on the morphology and size of the resulting powders. The formation mechanism of the Bi₂S₃ nanostructures with different morphologies was discussed. All Bi₂S₃ nanostructures showed an appearance of blue shift relative to the bulk orthorhombic Bi₂S₃, which might be ascribed to the quantum size effect of the final products. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Surfactant‐assisted synthesis of novel star‐like PbWO4 hierarchical architectures

Large‐scale star‐like PbWO₄ hierarchical architectures were controllably synthesized by a facile surfactant‐assisted technology under mild conditions in the presence of a mixed solvent of ethylene glycol and water. The morphology, structure, and phase composition of PbWO₄ architectures were characterized by X‐ray diffraction (XRD), field emission scanning electron microscopy (FE‐SEM), field emission transmission electron microscopy (FE‐TEM), and nitrogen adsorption‐desorption isotherms. The possible formation mechanism of the star‐like PbWO₄ architectures (initial nucleating stage and a subsequent self‐assembly stage) was proposed based on the observations from a time‐dependent morphology evolution process, which may pave the way to shape‐controlled synthesis of inorganic nanocrystals with the complex structures. This route provides a facile strategy to fabricate complex hierarchical PbWO₄ structures. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Hydrothermal conversion of ZnO2 to ZnO flowers: A mechanistic investigation and characterization

In this article, we report a novel but simple method for the phase transformation of ZnO₂ to flower‐like ZnO microstructures hydrothermally at 90 °C with and without the assistance of hexadecylamine as surfactant. The generation of zincate ion ZnO$^{2-}_{2}$ as a growth unit from the reaction between ZnO₂ and peroxide ion O$^{2-}_{2}$ in situ plays a key role in the phase transformation of ZnO₂ to ZnO. The morphology, structure, and composition of the products have been investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Powder X‐ray diffraction (PXRD) and energy dispersive X‐ray analysis (EDX). It has been demonstrated that the as‐fabricated ZnO flowers are composed of self‐assembled brooms and rods in the presence and absence of hexadecylamine respectively. On the basis of experimental results, a possible reaction mechanism and the growth processes involved in the formation of flower‐like ZnO microstructures are discussed.     

Synthesis of strontium carbonate rods and hierarchical branches in the presence of two organic additives

In this paper, strontium carbonate (SrCO₃) crystals have been synthesized in the presence of two organic additives, including sodium citrate and hexamethylenetetramine (HMT). Scanning electron microscopy, transmission electron microscopy (TEM), Fourier transform infrared spectroscopy, X‐ray powder diffractometry and selected area electron diffraction (SAED) were used to characterize the products. The results indicate that SrCO₃rods with the ratio of length to diameter about 20 are obtained in the aqueous solution containing sodium citrate. While polycrystalline SrCO₃ hierarchical branches with about 10 μm length are produced by using HMT.The possible formation mechanism of the SrCO₃crystals obtained in above two systems is discussed, which can be interpreted by particle‐aggregation based non‐classical crystallization laws. Sodium citrate and HMT may direct the formation of SrCO₃ rod‐like or branch‐like structures by adsorbing onto certain facets of SrCO₃ crystals. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Photoluminescent hierarchical Zno micro‐flower and its surface wettability

The flower‐like ZnO with micro‐nano hierarchical structure is successfully obtained by a simple hydrothermal synthesis, using sodium dodecyl benzene sulfonate (SDBS) as a structure direct agent. The resulted ZnO micro‐flowers are very uniform in morphology with particle sizes around 1 µm. A number of techniques, including X‐ray diffraction (XRD), field emission scan electron microscopy (FESEM), energy‐dispersive spectroscopy (EDS), fourier transform infrared (FTIR) spectra and thermogravimetry analysis (TGA), are used to characterize the obtained ZnO. The self‐assemble of ZnO nano‐sheets under the direction of SDBS leads to the formation of ZnO micro‐flowers. The room temperature photoluminescence property of the obtained flower‐like ZnO exhibits a broad visible light emission. The surface of as‐made ZnO shows a very hydrophilic property, while the special micro‐nano hierarchical structure enables the ZnO micro‐flower a superhydrophobic surface after modification of fluoroalkylsilane.     

Studies on fabrication of urchin‐like WO3·H2O hollow spheres and their photocatalytic properties

Urchin‐like tungsten oxide hydrate (WO₃ · H₂O) hollow spheres were successfully synthesized via a self‐sacrifice template method at low temperature. The effects of reaction parameters on the preparation were studied in solution. The growth mechanism was also proposed on the basis of experimental results. In addition, the acid amount and temperature have important effects on size control of the as‐obtained samples. The achieved nanoarchitectures have typical diameters of 4–6 μm with nanoflakes of several nanometers at surface. Crystal structure, morphology, and composition of final nanostructures were characterized by X–ray diffraction (XRD) and scanning electron microscopy (SEM). Degradation experiments of organic contaminant were also performed on samples of hollow spheres and walnut‐like structures under visible‐light illumination. Hollow sphere sample exhibited better photocatalytic capability than walnut‐like sample. Possible mechanism was studied for WO₃ · H₂O assisted photocatalytic degradation of organic contaminant under visible light.     

Morphology‐photocatalytic properties‐growth mechanism for ZnO nanostructures via microwave‐assisted hydrothermal synthesis

ZnO nanostructures with various morphologies including rod‐like, sheet‐like, needle‐like and flower‐like structures were successfully synthesized via a fast and facile microwave‐assisted hydrothermal process. Reaction temperature, reaction time and the addition of NaOH were adjusted to obtain ZnO with different morphologies. Scanning electron microscopy(SEM), transmission electron microscope(TEM), X‐ray diffraction (XRD) and ultraviolet spectrophotometer (UV) were used to observe the morphology, crystal structure, ultraviolet absorption and photocatalytic activity of the obtained ZnO. The results indicated that growth rate of ZnO nanostructure along [001] direction was more sensitive to temperature compared with those along [101] and [100] directions. The competition between anionic surfactant and OH⁻ played an important role in the formation of ZnO with various morphologies. Flower‐like ZnO had better ultraviolet absorption property and excellent photocatalytic activity than ZnO in the other morphologies. On the basis of the above results, a possible growth mechanism for the formation of ZnO nanostructures with different morphologies was described.     

Controllable synthesis and field emission properties of In2O3 nanostructures

Large‐scale In₂O₃ nanorods, nanocubes and nanowires have been successfully synthesized by chemical vapor deposition route under atmospheric pressure. The structures and morphologies were characterized by x‐ray diffraction (XRD), scanning election microscopy (SEM) and high‐resolution transmission electron microscopy (HRTEM). The growth mechanisms of these In₂O₃ nanostructures were analyzed in detail based on the experimental results. Field‐emission measurements of these nanostructures demonstrated that nanorods with rectangular cross‐section possessed good performance with a turn‐on field of 2.47 Vμm^–1 and a field enhancement factor of 4597. The room‐temperature photoluminescence (PL) spectrum of the In₂O₃ nanostructure showed UV emission centered at about 396 nm and visible emissions located at 541 and 623 nm. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Controllable synthesis of TiO2 nanoparticles employing substrate/dielectrophoresis/sol‐gel

Due to size‐dependent catalytic selectivity, the size and special morphology are of great importance to applications of TiO₂. The synthesis method of size and morphology control has been in need of innovation. In this study, TiO₂ nanoparticles(TiO₂‐NPs) with well‐defined morphology and homogenous size were synthesized using a novel method, in which bamboo substrate, dielectrophoresis (DEP) technology and a sol‐gel process were combined(substrate/ DEP/ sol‐gel). Powder X‐ray diffraction (XRD) and scanning electron microscopy (SEM) techniques were used to characterize the TiO₂‐NPs. Further study showed that, with this combined method, the size and the uniformity of TiO₂‐NPs can be controlled by changing the voltage of DEP. The number and arrangement of TiO₂ nanorods can be controlled by changing the voltage. Substrate/ DEP/ sol‐gel proved to be an efficient way to form special morphologies of TiO₂‐NPs. A visible‐light catalytic activity experiment showed that among three preparation methods, the substrate/ DEP/ sol‐gel method made TiO₂‐NPs with the highest catalytic activity for degradation of methyl orange. TiO₂‐NPs produced by the DEP/ sol‐gel process presented higher catalytic activity than TiO₂‐NPs produced by only a sol‐gel process.     

Controllable synthesis of novel In2O3 nanostructures and their field emission properties

Three kinds of novel indium oxide (In₂O₃) nanostructures, namely, nanorods, nanoflowers and nanowhiskers were synthesized on silicon substrate via a simple vapor‐phase transport method under atmospheric pressure. The In₂O₃nanostructures were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), and energy‐dispersive X‐ray spectrometer (EDS) spectrum. The Raman spectra of these nanostructures showed four sharp scattering peaks centered at 308, 365, 522, and 628 cm^‐1, whose position and intensity were characteristic of standard Raman spectra for In₂O₃. The Room‐temperature photoluminescence (PL) spectra showed visible emissions centered around 576, 592, and 624 nm. Field emission measurements demonstrated that the nanoflowers possessed the best performance with a turn‐on field of 3.54 V/µm and a threshold field of 9.83 V/µm. And the field enhancement factors of these nanostructures are high enough for the application of field emission display devices. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)