Hydrothermal synthesis and characterization of TiO2 nanorod arrays on glass substrates

Large-scale, well-aligned single crystalline TiO₂ nanorod arrays were prepared on the pre-treated glass substrate by a hydrothermal approach. The as-prepared TiO₂ nanorod arrays were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. X-ray diffraction results show that the main phase of TiO₂ is rutile. Scanning electron microscopy and transmission electron microscopy results demonstrate that the large-scale TiO₂ nanorod arrays grown on the pre-treated glass substrate are well-aligned single crystal and grow along [0 0 1] direction. The average diameter and length of the nanorods are approximately 21 and 400 nm, respectively. The photocatalytic activity of TiO₂ nanorod arrays was investigated by measuring the photodegradation rate of methyl blue aqueous solution under UV irradiation (254 nm). And the results indicate that TiO₂ nanorod arrays exhibit relatively higher photocatalytic activity.     

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.     

Synthesis and photocatalytic properties of TiO2 nanostructures

TiO₂ particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl₄. The as-prepared TiO₂ powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectra and N₂ adsorption–desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO₂. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO₂ exhibited the highest photocatalytic activity.     

Preparation of highly ordered growth of single-crystalline Gd2O2S:Eu nanostructures

A simple and facile template-assisted hydrothermal route has been demonstrated for the shape-selective preparation of highly ordered single-crystalline Gd₂O₂S:Eu³⁺ nanostructures, such as nanotubes, nanorods and nanoflowers. These fabricated nanostructures possess desirable atomic structures, surfaces, morphologies and properties to meet the growing demands and specific requirements of new technologies. The concentration of precursor chemicals, the temperature, the reaction time, and the use of a capping agent are key factors in the morphological control of Gd₂O₂S:Eu³⁺ nanostructures. The morphology and the phase composition of the prepared nanostructures were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy disperse spectroscopy (EDS) and photoluminescence (PL). We believe this technique will be readily adopted in realizing other forms of various nanostructured materials.     

Shape evolution of Cu2S nanostructures in Triton X-100/cyclohexane/water reverse micelles

The shape evolution of Cu₂S nanostructures, which were produced in Triton X-100/cyclohexane/water reverse micelles, was investigated by the transmission electron microscopy technique as a function of aging time, and the effect of the molar ratio of water to surfactant on the size and shape of Cu₂S nanostructures was also discussed. The results suggest that at the initial stage the nucleation process was dominant and the shape of Cu₂S nanostructures was preferably confined by the reverse micelle droplets and took spherical forms. With the extension of the aging time, the growth gradually governed the process and the shape of Cu₂S nanostructures evolved first to nanorods, and then to nanowires gradually. The formation of one-dimensional Cu₂S nanostructures is attributed to a directed aggregation growth process mediated by reverse micelle droplets, which was confirmed by high-resolution transmission electron microscopy. Furthermore, the size and shape of Cu₂S nanostructures can be controlled by changing the molar ratio of water to surfactant.     

Cu2O nanorod thin films prepared by CBD method with CTAB: Substrate effect,deposition mechanism and photoelectrochemical properties

Cuprous oxide (Cu₂O) films with different nanostructures are deposited on different substrates of fluorine-doped SnO₂ (FTO) glass, Cu and Ti foil respectively by using chemical bath deposition (CBD) technique with the presence of cetyltrimethylammonium bromide (CTAB). The samples are characterized by X-ray diffractmeter, scanning electron microscopy and UV–vis diffuse reflectance spectroscopy. The results show that the prepared Cu₂O films are composed of nanorod arrays when there is CTAB in reaction system. Without CTAB, Cu₂O films with nanospheres are formed. The concentration of CTAB is crucial for the controllable synthesis of nanorod structured Cu₂O films with different length to diameter ratio and nanorod array density is dependent on both substrates and CTAB. A possible mechanism for the formation of Cu₂O nanorods is discussed. Additionally, the UV–vis absorption property for Cu₂O nanorods is much better than that for nanospheres. The photovoltage produced under visible light for Cu₂O nanorod films is higher than that for the nanospheres. Although Cu₂O nanorods on Ti foil can absorb the most visible light, those on Cu foil demonstrate better and more stable photoelectrochemical property than those on any other substrates. This study may be extremely useful for Cu₂O based device with nanostructures.     

Efficient growth of aligned SnO2 nanorod arrays on hematite (α-Fe2O3) nanotube arrays for photoelectrochemical and photocatalytic applications

SnO₂ nanorod arrays were fabricated on hematiete nanotube arrays by an efficient hydrothermal method. The hematiete nanotube arrays were prepared by anodization of pure iron foil in an ethylene glycol solution. SnO₂ nanorod arrays grew from the bottom of hematite nanotubes and were firmly combined with the iron foil substrate. The morphology and microstructure of SnO₂ nanorod arrays are investigated by field-emission scanning electron microscopy, grazing incidence X-ray diffraction and UV–Vis absorbance spectra. The sample presented typical SnO₂ nanorod arrays (reacted for 2 h) generally of 400 nm in length and 50 nm in side width showed the best photocatalytic activity and photoelectrochemical response under the UV illumination. It should be attributed to the effective electron–hole separation and the excellent electron transfer pathway along the 1D SnO₂ nanorod arrays and hematiete nanotube arrays.     

Fabrication and photocatalytic property of ZnO nanorod arrays on Cu2O thin film

ZnO nanorod arrays were fabricated on Cu₂O thin film by a simple low-temperature liquid-phase-deposition method. The samples were characterized by X-ray powder diffraction (XRD) and field emission scanning electron microscopy (FESEM). The UV-Vis spectroscopy showed that the obtained sample was able to absorb a large part of visible light (up to 650 nm). Their photocatalytic activities were investigated by degradation of dye methylene blue (MB) under UV-Vis and visible light irradiation. It was found that the photocatalytic activity of the ZnO/Cu₂O NRs was higher than the ZnO/ZnO NRs under UV-Vis light. In a word, Cu₂O played an important role in enhancing the photocatalytic activity of the ZnO/Cu₂O NRs.     

Synthesis and characterization of novel flower-like CeF3 nanostructures via a rapid microwave method

Novel flower-like CeF₃ nanostructures with a mean diameter of 190 nm were successfully synthesized via a rapid and facile microwave irradiation route using ethylenediaminetetraacetic acid disodium as the complexing reagent. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and photoluminescence (PL). XRD patterns showed that the CeF₃ nanoflowers were hexagonal phase and had good crystallinity and purity. TEM and SEM images showed that the as-prepared CeF₃ samples displayed 3D flower-like nanostructures and had uniform sizes and morphologies. The experimental results revealed that the as-prepared CeF₃ nanoflowers might be assembled by nanodisks. The formation process of the CeF₃ nanoflowers was preliminarily investigated.     

Architecture of Cu2O@TiO2 core–shell heterojunction and photodegradation for 4-nitrophenol under simulated sunlight irradiation

A Cu₂O@TiO₂ core–shell heterojunction photocatalyst was prepared by an in situ hydrolysis and crystallization method. The as-prepared catalyst was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy and photoluminescence (PL) spectroscopy. Under simulated sunlight irradiation, it exhibited high photocatalytic activity and stability for 4-nitrophenol (4-NP) degradation. Compared with neat Cu₂O and Cu₂O/TiO_2(PM) prepared by physical mixing, the heightened photocatalytic activity of Cu₂O@TiO₂ was attributed to the improvement of charge separation since large close interface was formed between the two semiconductors. The in situ method may generally be applied to develop other core–shell heterojunction photocatalysts.     

The preparation of Cu<Subscript>2</Subscript>O@Au yolk/shell structures for efficient photocatalytic activity with a self-generated acid etching method

Cu₂O@Au yolk/shell structures were successfully prepared with a facile self-generated acid etching method at room temperature. The morphology is controllable by adding different amount of HAuCl₄·4H₂O. Scanning electron microscopy and transmission electron microscopy images showed that Au nanoparticles self-assembled into a porous shell around Cu₂O core while the produced etching agent etched the core gradually and formed the cavity. The photocatalytic property of Cu₂O@Au yolk/shell structures was studied by degrading MO under the irradiation of visible light at room temperature. Benefiting from the synergistic effect of cavity micro-reactor and electron transfer, the photocatalytic performance of the as-prepared Cu₂O@Au yolk/shell structures was much better than that of pure Cu₂O. The possible photocatalytic mechanism of the Cu₂O@Au yolk/shell catalysts was proposed and elaborated in this study. It is certified that Yolk/shell structures have potential applications in photocatalysis for its active sites on the large specific area.     

Facile synthesis of ZnO nanorod arrays and hierarchical nanostructures for photocatalysis and gas sensor applications

A facile one-step hydrothermal route was demonstrated to grow ZnO nanorod arrays and hierarchical nanostructures on arbitrary substrates without any catalysts and seeds coated before the reaction, which are prerequisite in the current two-step protocol. Meanwhile, ZnO nanoflowers composed of nanorods were obtained at the bottom of the autoclaves in the absence of substrates. An in situ spontaneous-seeds-assisted growth mechanism was tentatively proposed on the basis of the experimental data to explain the growth process of ZnO nanostructures. Moreover, the obtained ZnO nanorod arrays exhibited superior photocatalytic activity for decomposing methyl orange, and the nanoflowers showed better gas sensing performance towards some flammable gases and corrosive vapors with high sensitivity, rapid response-recovery characteristics, good selectivity and long-term stability.     

Hydrothermally fabricated surfactant-free CuxAg1−xS composites with enhanced photocatalytic activity and stability

Here, we report the stable and surfactant-free Cu_xAg_1?xS composites as nanorod clusters was fabricated by a simple hydrothermal method for the degradation of pesticides including malathion (MLT), monocrotophos (MCP), and chlorpyrifos (CPS) under ultraviolet (UV) light. The degradation of MLT, MCP, and CPS using Cu_0.5Ag_0.5S were up to 97% after 1?h of UV irradiation. The Cu_0.5Ag_0.5S nanorods displayed enhanced photocatalytic activity and the rate of degradation was higher than that of pure CuS and Ag₂S due to an efficient electron transfer process. The stability and reusability assays indicated that the Cu_0.5Ag_0.5S retained more than 90% of activity after five cycles of use. The photocatalytic mechanism was explored from the obtained results of enhanced photocatalytic activity of Cu_xAg_1?xS nanorod clusters.     

Synthesis, characterization, and hydrophobic properties of Bi2S3 hierarchical nanostructures

Novel Bi₂S₃ hierarchical nanostructures self-assembled by nanorods are successfully synthesized in mild benzyl alcohol system under hydrothermal conditions. The hierarchical nanostructures exhibit a flower-like shape. X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED) were used to characterize the as-synthesized samples. Meanwhile, the effect of various experimental parameters including the concentration of reagents and reaction time on final product has been investigated. In our experiment, PVP plays an important role for the formation of the hierarchical nanostructures and the possible mechanism was proposed. In addition, Bi₂S₃ film prepared from the flower-like hierarchical nanostructures exhibits good hydrophobic properties, which may bring nontrivial functionalities and may have some promising applications in the future.     

Cu2S nanostructures prepared by Cu-cysteine precursor templated route

A facile Cu-cysteine precursor templated route for the synthesis of Cu₂S nanowires, dendritic-like and flowerlike nanostructures is reported. The Cu-cysteine precursors are prepared through the reaction between Cu²⁺, l-cysteine and ethanolamine at room temperature, and the morphologies of Cu-cysteine precursors can be controlled by adjusting the molar ratio of l-cysteine to Cu²⁺. The Cu-cysteine precursors are used as both templates and source materials for the subsequent preparation of polycrystalline Cu₂S nanostructures by thermal treatment, and the morphologies of the precursors can be well preserved after the thermal transformation to Cu₂S nanostructures. The samples are characterized using X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy and Fourier transform infrared spectroscopy.     

Synthesis and photoluminescence properties of the ZnO@SnO<Subscript>2</Subscript> core–shell nanorod arrays

The ZnO@SnO₂ core–shell nanorod arrays have been synthesized. As the cores, ZnO nanorod arrays were first prepared by aqueous chemical growth method. Then using a simple liquid-phase deposition method, SnO₂ was deposited on the ZnO nanorod arrays. Scanning electron microscopy, transmission electron microscopy, and X-ray diffraction were used to characterize the morphologies and structures of the products. Photoluminescence properties were also investigated. It was found that the ZnO@SnO₂ core–shell nanorod arrays showed enhanced UV and green emissions when compared with the bare ZnO nanorod arrays.     

Morphological control and photodegradation behavior of rutile TiO2 prepared by a low-temperature process

Flower-like rutile titania nanocrystals were prepared via a simple aqueous-phase stirring for 24 h at a low temperature of 75 °C, employing only TiCl₄, HCl as the starting materials. XRD result proved the formation of rutile TiO₂. The observations from TEM and SEM showed that the products were large-scale flower-shaped structures composed of radial nanorods. Comparative experiments demonstrated that pinecone-like, needlelike rutile TiO₂ could be easily achieved by varying the volume ratio of TiCl₄ / H₂O. The growth mechanisms of TiO₂ nanostructures prepared under different conditions and their photodegradation behavior were also discussed. It was found that the flower-like structures exhibited the highest photocatalytic activity in the photodegradation of aqueous brilliant red X-3B solution.     

Decoration of Cu nanowires with chemically modified TiO2 nanoparticles for their improved photocatalytic performance

In this work, TiO₂ nanoparticles/Cu nanowires (TiO₂NPs@CuNWs) binary composites with tunable coverage of TiO₂ nanoparticles were prepared by a facile method of mixing oleic acid-modified TiO₂ nanoparticles with as-prepared Cu nanowires. Characterization studies including X-ray diffraction spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy were applied to investigate the structure and morphology of the as-synthesized TiO₂NPs@CuNWs binary composites. The photocatalytic activity of TiO₂NPs@CuNWs binary composites was examined by photodegradation of methyl orange. The enhanced photocatalytic efficiency of TiO₂NPs@CuNWs nanocomposites was ascribed to the moderate specific surface area, mesoporous structures, and the electron sink effect of the Cu nanowires. In principle, our investigation indicates that the TiO₂@Cu self-assembled nanostructures can be a promising candidate of composite photocatalysts.     

Rapid preparation and photocatalytic properties of octahedral Cu2O@Cu powders

To improve the photocatalytic properties of Cu₂O, octahedral Cu₂O@Cu powders were prepared by a convenient and rapid two-step liquid phase reduction method. Glucose (C₆H₁₂O₆) and thiourea dioxide (CH₄N₂O₂S, TD for short) were used as pre-reductant and secondary-reductant separately. The microstructure and composition of the products obtained after the reduction processes were analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). With the increasing of TD content, the secondary reduced products changed from solid octahedral Cu₂O to octahedral Cu₂O@Cu composites and finally hollow octahedral Cu₂O/Cu composites. The corresponding calculated mass of Cu increased from 6.2 wt% to 80.2 wt%. The photocatalytic behavior of the reduced particles were analyzed by monitoring the degradation of methyl orange solution (MO for short) and electrochemical tests. Photocatalytic performance tests showed that octahedral Cu₂O@Cu powders had an excellent photocatalytic activity. The MO degradation rate was improved from 1.4% for photocatalysts without CuNPs to 92.9% after introducing 13.4 wt% CuNPs under visible light irradiation for 60 min. This simple and rapid synthesis process allowed for the fabrication of octahedral Cu₂O@Cu material with photocatalytic performance superior to pure octahedral Cu₂O and hollow octahedral Cu₂O/Cu materials.     

Surfactant-free synthesis of Bi2WO6 multilayered disks with visible-light-induced photocatalytic activity

The synthesis of bismuth tungstate (Bi₂WO₆) multilayered disk which was constructed by oriented square nanoplates was easily realized via a simple surfactant-free hydrothermal method. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM) were used to investigate the as-obtained product. The results indicated that the three-dimensional (3D) Bi₂WO₆ multilayered disk was constructed by self-assembly of square nanoplates via a perfect oriented manner. The formation mechanism of the product was carefully investigated on the basis of the results of time-dependent experiments. In addition, studies of the photocatalytic property demonstrated that the as-obtained Bi₂WO₆ could exhibit excellent visible-light-driven photocatalytic activity for the degradation of Rhodamine B (RhB).