D-penicillamine assisted hydrothermal synthesis of Bi2S3 nanoflowers and their electrochemical application

Single crystalline flower-like Bi₂S₃ nanostructures were successfully synthesized via a simple, facile and green hydrothermal method, with the assistance of D-penicillamine. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), and found their morphologies mainly depend on the ratios of Bi^3 + to D-penicillamine, as well as the reaction temperature and time. And the possible growth mechanism has been discussed in some detail. In addition, the as-prepared Bi₂S₃ nanoflowers show good hydrogen storage ability. This strategy can be potentially expanded to prepare other metal chalcogenides materials.     

Characterization of Bi2S3 nanorods and nano-structured flowers prepared by a hydrothermal method

Bismuth sulfide nanorods and nano-structured flowers were synthesized by hydrothermal reaction of bismuth nitrate pentahydrate and thiourea solutions, containing 1 and 2 ml of 65% HNO₃, respectively. By using X-ray diffraction (XRD), selected area electron diffraction (SAED), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution TEM (HRTEM), the products were specified as orthorhombic Bi₂S₃ in the shapes of nanorods and flower-like clusters of nanorods, with the growth of nanorods in the [001] direction. A diffraction pattern was also simulated, and was in good accordance with the SAED pattern obtained from the experiment.     

Fabrication of three-dimensional snowflake-like bismuth sulfide nanostructures by simple refluxing

Three-dimensional snowflake-like bismuth sulfide nanostructures were successfully synthesized by simple refluxing at 160 °C in ethylene glycol, using bismuth citrate and thiourea as reactants. The crystal structures and morphologies of the products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and energy dispersive X-ray spectroscopy (EDX). The Bi₂S₃ nanostructure was built up by highly ordered one-dimensional Bi₂S₃ nanorods, which was aligned in an orderly fashion. Ethylene glycol plays a critical role in the creation of bismuth sulfide three-dimensional nanostructures, which serves as an excellent solvent and structure director. Bismuth citrate, a linear polymer, also makes for the formation of the three-dimensional nanostructures.     

Solvent directed fabrication of Bi2WO6 nanostructures with different morphologies: Synthesis and their shape-dependent photocatalytic properties

In this work, Bi₂WO₆ with complex morphologies, namely, flower-like, pancake-like, and tubular shapes have been controllably synthesized by a facile solvothermal process. The as-obtained samples are systematically investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM). The effects of solvents on the morphologies of Bi₂WO₆ nanostructures are systematically investigated. According to the time-dependent experiments, a two-step growth mode basing on Ostwald ripening process and self-assembly has been proposed for the formation of the flower-like and pancake-like Bi₂WO₆ nanostructures. The photocatalytic properties of Bi₂WO₆ nanostructures are strongly dependent on their shapes, sizes, and structures for the degradation of rhodamine B (RhB) under visible-light irradiation. The deduced reasons for the differences in the photocatalytic activities of these Bi₂WO₆ nanostructures are further discussed.     

Rapid synthesis of Bi2S3 nanocrystals with different morphologies by microwave heating

Single-crystalline Bi₂S₃ nanocrystals with urchinlike and rod-like morphologies have been successfully synthesized using Bi₂O₃, HCl, Na₂S₂O₃ and ethylene glycol (EG) by a simple and fast microwave heating method. Both urchinlike and rod-like Bi₂S₃ nanostructures could be formed under microwave heating at 190 °C for 30 s. Urchin-like Bi₂S₃ nanostructures were prepared using sodium dodecyl sulfate (SDS) or in the absence of any surfactant. However, Bi₂S₃ nanorods were obtained in the presence of cetyltrimethylammonium bromide (CTAB). The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), electron diffraction (ED) and ultraviolet-visible (UV-Vis) absorption spectra.     

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.     

Effect of mixed solvent on the morphologies of nanostructured Bi2S3 prepared by solvothermal synthesis

Different morphologies of nanostructured bismuth sulfide (Bi₂S₃) including nanotubes and nanorods have been prepared by solvothermal synthesis at a low temperature of 120 °C for 12 h using various mixed solvents as the reaction medium and urea as the mineralizer. X-ray diffraction analysis showed that all the as-prepared Bi₂S₃ samples are orthorhombic phase. Transmission electron microscopy analysis showed that the morphologies of the nanostructures are mainly related to the viscosity and surface tension of the mixed solvent used in the solvothermal synthesis.     

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).     

Bi2Te3纳米结构的制备、磁性掺杂和结构表征

通过液相法制备Bi2Te3纳米管,设计并优化了Co离子的掺磁方案。通过扫描电镜、透射电镜、X射线衍射、红外光谱和能量色散X射线光谱对制备的样品进行了结构表征。实验结果表明,液相法可制备出晶相良好的Bi2Te3纳米管、Co离子均匀掺杂的Bi2Te3纳米结构样品。     

Characterization of Bi2S3 with different morphologies synthesized using microwave radiation

Bi₂S₃ with different morphologies (nanoparticles, nanorods and nanotubes) was synthesized using bismuth nitrate pentahydrate (Bi(NO₃)₃·5H₂O) and two kinds of sulfur sources (CH₃CSNH₂ and NH₂CSNH₂) in different solvents (water, ethylene glycol and propylene glycol) via a microwave radiation method at 180 W for 20 min. X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that all of the products are orthorhombic Bi₂S₃ phase of nanoparticles, nanorods and nanotubes, influenced by the sulfur sources and solvents. Formation mechanisms of the products with different morphologies are also proposed.     

Synthesis of flower-like,pinon-like and faceted nanoplates (BiO)2CO3 micro/nanostructures with morphology-dependent photocatalytic activity

The flower-like, pinon-like and faceted nanoplates (BiO)₂CO₃ micro/nanostructures were fabricated by a one-pot template-free method based on hydrothermal treatment of the aqueous mixture of bismuth citrate and sodium carbonate. The morphology of (BiO)₂CO₃ can be simply controlled by the reaction temperature. X-ray diffraction, scanning electron microscopy, UV–vis diffuse reflection spectra, and photoluminescence spectra were applied to analyze the microstructures and properties of the samples. The flower-like and pinon-like (BiO)₂CO₃ superstructures were hierarchically self-assembled by nanoplates and showed increased light absorption owing to the multiple light reflection between the nanoplates. The thickness of nanoplates was increased with the increasing reaction temperatures due to the preferred growth along the (110) plane. The (BiO)₂CO₃ with various micro/nanostructures showed morphology-dependent photocatalytic activity toward removal of aqueous RhB. The as-prepared flower-like (BiO)₂CO₃ microspheres exhibited highest photocatalytic activity due to the large surface area, increased light absorption, enhanced charge carriers separation, and special architectures of hierarchical nanoplates microspheres, exceeding that of the P25.     

A simple chemical route to Bi2S3 hierarchical columniform structures assembled by nanorod-based lamellae

Bi₂S₃ hierarchical columniform structures assembled by nanorod-built lamellae have been first synthesized by a simple wet chemical method through the reaction between Bi(NO₃)₃?5H₂O and CS₂ at 80 °C for 14 h using DMSO as solvent without any surfactants. These new Bi₂S₃ structures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Compared to ethylene glycol and DMF, DMSO supplied an excellent chemical environment favorable to the generation of Bi₂S₃ quickly in heterogeneous condition. The influences of the synthetic parameters were discussed and a possible growth mechanism for the formation of these complex structures was proposed.     

Synthesis of flower-like Boehmite (AlOOH) via a simple solvothermal process without surfactant

Boehmite (AlOOH) with hierarchical flower-like structures was synthesized by the solvothermal reaction of AlCl₃·6H₂O in the presence of ethanol and toluene at 200 °C for 24 h. The product was characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that boehmite with flower-like nanostructures, which aggregated together by the weak hydrogen bonds, was formed through dissolution-deposition process of boehmite microcrystals and the toluene has a great effect on the morphology of product in the reaction system. Meanwhile, the γ-Al₂O₃ was also obtained by calcination of above product at 500 °C for 2 h, and the flower-like morphology kept no change. The surface area of γ-Al₂O₃ powder was determined to be 166.8 m²/g by N₂ adsorption measurement. The possible formation mechanism of flower-like boehmite nanostructures was proposed and discussed.     

Novel flower-like (Bi(Bi2S3)9I3)2/3 nanostructure as efficient photocatalyst for photocatalytic desulfurization of benzothiophene under visible light irradiation

Here, we report the preparation of hierarchical flower-like (Bi(Bi₂S₃)₉I₃)_2/3 nanostructures that acts as a strong photocatalyst in the desulfurization of benzothiophene. We optimized the reaction time, type of capping agent and reflux temperature to tune the shape of porous flower-like (Bi(Bi₂S₃)₉I₃)_2/3 nanostructures to achieve the highest desulfurization performance. We investigated the characteristic shape, size, purity, and optical response of the flower-shape nanostructures using XRD, EDS, FESEM, UV–Vis-DRS analysis. The flower-like (Bi(Bi₂S₃)₉I₃)_2/3 nanostructures showed a significant photocatalytic property in desulfurization of benzothiophene as a model fuel. The hierarchical flower-like (Bi(Bi₂S₃)₉I₃)_2/3 photocatalyst with an energy gap of 1.15 eV, exhibits a 92% photocatalytic desulfurization performance after 2 h of visible light irradiation. The (Bi(Bi₂S₃)₉I₃)_2/3 nanostructures show a high photocatalytic reproducibility after 4 rounds of exposure. We proposed a photo-oxidation mechanism based on the active species scavenging, which revealed the role of photo-produced h⁺ and O₂^? species as essential in the photocatalytic desulfurization process. These findings provide a new prospect and design strategy for the development of efficient photocatalysts in desulfurization process.     

Synthesis and characterization of bismuth sulfide nanowires through microwave solvothermal technique

One-dimensional (1D) bismuth sulfide (Bi₂S₃) semiconducting nanowires have been successfully synthesized through mircrowave assisted solvothermal technique. The obtained product was characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and UV-vis spectrophotometry. The result shows that the Bi₂S₃ nanowires are single crystals grown along the [001] (c-axis) direction. The growth of Bi₂S₃ nanofibers with a preferential direction of c-axis can be ascribed to its particular structure. The optical measurement shows a blue shift relative to the bulk orthorhombic Bi₂S₃, which might be ascribed to the high aspect ratio of the nanowires.     

Preparation of Bi2S3 nanorods via a hydrothermal approach

Large-scale bismuth sulfide (Bi₂S₃) nanorods with uniform size have been prepared by hydrothermal method using bismuth chloride (BiCl₃) and sodium sulfide (Na₂S·9H₂O) as raw materials at 180 °C and pH = 1-2 for 12 h. The powder X-ray diffraction (XRD) pattern shows the Bi₂S₃ crystal belongs to the orthorhombic phase with calculated lattice constants a = 1.1187 nm, b = 1.1075 nm and c = 0.3976 nm. Furthermore, the quantification of X-ray photoelectron spectra (XPS) analysis peaks gives an atomic ratio of 1.9:3.0 for Bi:S. Field emission scanning electron microscopy (FE-SEM) and transmission electron microscopic (TEM) studies reveal that the appearance of the as-prepared Bi₂S₃ is rod-like with typical lengths in the range of 2-5 μm and diameters in the range of 10-30 nm. Finally the influences of the reaction conditions are discussed and a possible mechanism for the formation of Bi₂S₃ nanorods is proposed.     

Synthesis of SnO2 flower-like architectures by varying the hydrothermal reaction time

We successfully synthesized hierarchical SnO₂ flower-like architectures assembled with nanorods via a facile hydrothermal route under mild condition. The structures and morphologies of the obtained hierarchical architectures were characterized by means of powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. By varying hydrothermal reaction time, we obtained the sphere-like and flower-like SnO₂. The evolution that the morphology changing from sphere-like to flower-like was systematically investigated. Moreover, the mechanism of formation for this structure was proposed in detail.     

Synthesis and characterization of WO3 nanostructures prepared by an aged-hydrothermal method

Nanostructures of tungsten trioxide (WO₃) have been successfully synthesized by using an aged route at low temperature (60 °C) followed by a hydrothermal method at 200 °C for 48 h under well controlled conditions. The material was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive Spectroscopy (EDS), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Specific Surface Area (S_BET) were measured by using the BET method. The lengths of the WO₃ nanostructures obtained are between 30 and 200 nm and their diameters are from 20 to 70 nm. The growth direction of the tungsten oxide nanostructures was determined along [010] axis with an inter-planar distance of 0.38 nm.     

Morphological evolution in single-crystalline Bi2Te3 nanoparticles, nanosheets and nanotubes with different synthesis temperatures

A general surfactant-assisted wet chemical route has been developed for the synthesis of a variety of bismuth telluride (Bi₂Te₃) single-crystalline nanostructures with varied morphologies at different temperatures in which hydrazine hydrate plays as an important solvent. Bi₂Te₃ sheet grown nanoparticles, nanosheets and nanotubes have been synthesized by a simplest wet chemical route at 50, 70 and 100 °C within 4 h. Bi₂Te₃ sheet grown nanoparticles are obtained in agglomerate state and they are found with many wrinkles. Various types of Bi₂Te₃ nanotubes are also found which are tapered with one end open and the other closed. X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) pattern and energy dispersive X-ray (EDX) spectroscopy were employed to characterize the powder product. It is found that all nanoparticles, nanosheets and nanotubes are well-crystallized nanocrystals and morphologies of the powder products are greatly affected by different synthesis temperatures. The formation mechanisms of bismuth telluride nanostructures are also discussed.     

Microwave-assisted synthesis and characterization of 3D flower-like Bi2S3 superstructures

Bismuth sulfide (Bi₂S₃) microcrystallines with three-dimensional (3D) flower-like superstructures were prepared by the microwave irradiation method with bismuth nitrate (Bi(NO₃)₃·5H₂O) and thiourea ((NH₂)₂CS) as raw materials and ethylene glycol as solvent. The powder X-ray diffraction (XRD) pattern shows the product belongs to the orthorhombic Bi₂S₃ phase. The quantification of X-ray photoelectron spectra (XPS) analysis peaks gives an atomic ratio of 1.9:3.0 for Bi:S. Transmission electron microscopic (TEM) and scanning electron microscopy (SEM) studies reveal that the superstructure of the as-prepared Bi₂S₃ consists of sticks extending radially from a nucleation site. The reaction progress and a possible mechanism were proposed.