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.     

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.     

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.     

Microwave synthesis of SrCO3 one-dimensional nanostructures assembled from nanocrystals using ethylenediamine additive

One-dimensional SrCO₃ nanostructures assembled from nanocrystals have been successfully synthesized by a microwave-assisted aqueous solution method at 90 °C using Sr(NO₃)₂, (NH₄)₂CO₃ and ethylenediamine (C₂H₈N₂). Our experiments show that the microwave heating time plays an important role in the size and morphology of SrCO₃. A rational mechanism based on the oriented attachment self-assembly is proposed for the formation of SrCO₃ nanostructures. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). This method is simple, fast, low-cost and suitable for large-scale production of SrCO₃ nanostructures with different morphologies. We expect that this method may be extended to the preparation of nanostructures of other kinds of carbonates.     

Synthesis and characterization of an electro-deposited polyaniline-bismuth telluride nanocomposite — A novel thermoelectric material

The present work consists of synthesis and characterization of a novel thermoelectric material polyaniline (PANI)-bismuth telluride (Bi₂Te₃) nanocomposite using simultaneous electrochemical reactions and deposition method. The inorganic bismuth nitrate has been used as a dopant for polyaniline to achieve high electrical conductivity. A semi-batch mode of operation has been employed to control the rate of deposition of an individual component and thus the molecular architecture of the composite. The electro-deposited composite film on ITO coated glass substrate has been characterized by X-ray diffraction analysis (XRD), FTIR analysis, scanning electron microscope (SEM), and transmission electron microscope (TEM). The microscopic analysis reveals the formation of rod-like nanostructures of diameter less than 100 nm. It has been found that smaller molecules of Bi₂Te₃ are dispersed in the macromolecules of PANI. The nanocomposite has been characterized by thermoelectric power.     

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.     

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.     

Microwave assisted rapid synthesis of Bi2O3 short nanorods

In this research, a highly efficient and rapid approach of synthesizing Bi₂O₃ short nanorods is reported in aqueous solutions using microwave irradiation of bismuth (III) nitrate in the presence of Polyvinylpyrrolidone (PVP), as a stabilizing polymer. Transmission electron and field-emission scanning electron microscope images clearly indicate the formation of short nanorods in 6 min under microwave irradiation. Conventional heat treatment route yields only Bi₂O₃ powder and it is also comparatively complicated and needs high manufacturing cost. Formation of such short Bi₂O₃ nanorods may be due to the formation of a polymer-metal complex with the stabilizing polymer (PVP).     

A very simple and low cost route to Bi2S3 nanorods bundles and dandelion-like nanostructures

Bi₂S₃ nanorods bundles as well as three-dimensional dandelion-like nanostructures were synthesized in high yield at lower temperature (room temperature or ambient temperature of 15 °C) in a very simple system composed only of Bi(NO₃)₃, thioacetamide (TAA), hydrochloride acid and distilled water. It is the first report to obtain such nanostructures at such a low temperature and by such a simple method, and the reaction does not demand any additional energy such as heating or agitation. A splitting crystal growth and self-assemble mechanism should be responsible for the formation of these structures. This kind of novel Bi₂S₃ nanostructures may find potential applications in hydrogen storage, high-energy batteries, as well as luminescence and catalysis fields.     

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.     

Microwave-assisted synthesis of hierarchical Bi2O3 spheres assembled from nanosheets with pore structure

Hierarchical Bi₂O₃ spheres assembled from nanosheets with nanopore structure have been successfully synthesized by thermal decomposition of the precursor at 400 °C for 3 h in air, which was prepared using Bi(NO₃)₃·5H₂O and poly(vinylpyrrolidone) (PVP) by a microwave-assisted heating method in ethylene glycol (EG) at 150 °C for 10 min. The morphology of Bi₂O₃ is similar to that of the precursor. The products were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectrometry (FT-IR), field-emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TG) and differential scanning calorimetric analysis (DSC). XRD pattern showed that the product had a high degree of crystallinity. FE-SEM micrograph indicated that hierarchical Bi₂O₃ spheres had sizes around 10 μm.     

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.     

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.     

Controllable fabrication of heterostructured Au/Bi2O3 with plasmon effect for efficient photodegradation of rhodamine 6G

ABSTRACT

Three-dimensional (BiO)₂CO₃ (BSC) nanostructures were synthesised by a hydrothermal reaction, and Bi₂O₃ nanoparticles were then obtained by calcining BSC precursor at different temperatures. BSC and Bi₂O₃ samples were then sputtering coated with Au to get the resultant Au/BSC and Au/Bi₂O₃ for the investigation of the effect of the Au coating on the photocatalytic performance of the samples. The phase structure, morphology and composition of the samples were characterised by X-ray diffraction, scanning electron microscopy and energy-dispersive spectroscopy (EDS). UV–vis diffuse reflectance spectra were used to measure the response of different catalysts to UV–vis light. The photocatalytic activity was investigated for the degradation of rhodamine 6G at room temperature and the light intensity was 1 sun. Bi₂O₃ exhibited better photocatalytic performance than BSC due to the narrow band gap of Bi₂O₃, and the coating of Au also endowed the samples with higher photocatalytic capability as compared to the bare one.     

Spatiotemporally Synchronous Oxygen Self-Supply and Reactive Oxygen Species Production on Z-Scheme Heterostructures for Hypoxic Tumor Therapy

Photodynamic therapy (PDT) efficacy has been severely limited by oxygen (O₂) deficiency in tumors and the electron–hole separation inefficiency in photosensitizers, especially the long-range diffusion of O₂ toward photosensitizers during the PDT process. Herein, novel bismuth sulfide (Bi₂S₃)@bismuth (Bi) Z-scheme heterostructured nanorods (NRs) are designed to realize the spatiotemporally synchronous O₂ self-supply and production of reactive oxygen species for hypoxic tumor therapy. Both narrow-bandgap Bi₂S₃ and Bi components can be excited by a near-infrared laser to generate abundant electrons and holes. The Z-scheme heterostructure endows Bi₂S₃@Bi NRs with an efficient electron–hole separation ability and potent redox potentials, where the hole on the valence band of Bi₂S₃ can react with water to supply O₂ for the electron on the conduction band of Bi to produce reactive oxygen species. The Bi₂S₃@Bi NRs overcome the major obstacles of conventional photosensitizers during the PDT process and exhibit a promising phototherapeutic effect, supplying a new strategy for hypoxic tumor elimination.     

Synthesis and properties of β-Ga2O3 nanostructures

A novel method was utilized to synthesize one-dimensional β-Ga₂O₃ nanostructures. In this method, β-Ga₂O₃ nanostructures have been successfully synthesized on Si(111) substrates through annealing sputtered Ga₂O₃/Mo films under flowing ammonia in a quartz tube. The as-obtained samples were analyzed in detail using the methods of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDX) attached to the HRTEM instrument. The results show that the formed nanostructures are single-crystalline Ga₂O₃. The annealing temperature has an evident influence on the morphology of the β-Ga₂O₃ nanostructures. The growth mechanism of the β-Ga₂O₃ nanostructures is also discussed by conventional vapor-solid (VS) mechanism.     

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.     

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.     

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.     

Enhancement of photosensitivity by annealing in Bi2S3 thin films grown using SILAR method

Bi₂S₃ thin films were grown by successive ionic layer adsorption and reaction method (SILAR) onto the glass substrates at room temperature. The as prepared thin film were annealed at 250 °C in air for 30 min. These films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and electrical measurement systems. The X-ray diffraction patterns reveal that Bi₂S₃ thin film have orthorhombic crystal structure. SEM images showed uniform deposition of the material over the entire glass substrate. The optical energy band gap observed to be decreased from 1.69 to 1.62 eV for as deposited and annealed films respectively. The I–V measurement under dark and illumination condition (100 W) show annealed Bi₂S₃ thin film gives good photoresponse as compared to as deposited thin film and Bi₂S₃ thin film exhibits photoconductivity phenomena suggesting its useful in sensors device. The thermo-emf measurements of Bi₂S₃ thin films revealed n-type electrical conductivity.