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.     

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 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.     

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.     

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, 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.     

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.     

Low temperature reduction route to synthesise bismuth telluride (Bi2Te3) nanoparticles: structural and optical studies

Herein, we report the synthesis of highly yielded bismuth-telluride (Bi₂Te₃) nanoparticles at 50 °C by direct wet chemical route in which the bismuth and tellurium precursors have been dissolved in deionised water, ethylene glycol and hydrazine hydrate. This method is very facile, inexpensive and less hazardous and ensures almost complete yield of the precursors. The powder product was well characterised by powder X-ray diffraction, UV-Vis spectroscopy, Fourier transform infrared spectroscopy, energy dispersive X-ray diffraction, transmission electron microscopy and scanning electron microscopy. It is investigated that the synthesised powder has a rhombohedral structure of Bi₂Te₃ with average diameters of the particles about 35 nm. Thus, the synthesis process has been modified to design nanostructures of thermoelectric materials with related crystal structures.     

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.     

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.     

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.     

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).     

Effect of substrate temperature on the structural,morphological and optical properties of copper bismuth sulfide thin films deposited by electron beam evaporation method

Copper bismuth sulfide thin films were deposited at 200 °C, 300 °C, 400 °C and 500 °C on the glass substrates by electron beam evaporation method. X-ray diffraction study revealed that the copper bismuth sulfide films of single and mixed phases were formed as a function of substrate temperatures. Substrate temperature of 300 °C and 400 °C formed single phase Cu₄Bi₄S₉ and Cu₄Bi₅S₁₀ films respectively whereas substrate temperature of 500 °C formed mixed phases of Cu₄Bi₄S₉ and Cu₄Bi₅S₁₀ film. Crystallite size, dislocation density and microstrain of the films were modified by the various substrate temperatures. Surface morphology of the film Cu₄Bi₅S₁₀ deposited at 400 °C examined by scanning electron microscopy showed the distribution of spherical shaped particles on the film surface. The presence of copper, bismuth and sulfur elements in the deposited films was confirmed using energy dispersive spectral studies. The calculated direct optical band gap energy of the films deposited at different substrate temperature varied from 1.47 to 1.64 eV and the absorption coefficient is in the order of 10⁶ cm^?1.     

Synthesis of bismuth micro- and nanospheres by a simple refluxing method

Well-separated bismuth micro- and nanospheres were successfully prepared from bismuth citrate and urea by a simple refluxing reaction at 198 °C in ethylene glycol in the presence of poly(vinyl pyrrolidone) (PVP). The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDX). The larger Brunauer–Emmett–Teller (BET) surface area of these micro- and nanospheres was found to be 17.34 m²/g by the results of N₂ adsorption. It was found that the amount of PVP have an influence on the morphologies of bismuth nanostructure. The possible growth mechanism of bismuth micro- and nanospheres was also discussed.     

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.     

Influence of gamma irradiation on structural,optical, and electrical characterization of Bi2S3 thin films

The induced effects of the gamma rays on properties of bismuth sulfide (Bi₂S₃) thin films synthesized using successive ionic layer adsorption and reaction (SILAR) have been investigated in details in this work. The Bi₂S₃ thin films are prepared on glass substrate and then exposed with low gamma radiation dose in the range of 0–1000 Gy. X-ray diffraction (XRD) confirmed the orthorhombic structural phase. Also, it was noticed in the XRD result that the crystallite size decreased from 115.29 to 73.63 nm with increasing gamma rays doses. For surface properties as well as stoichiometry of the prepared and irradiated thin film have been studied by field emission scanning electron microscope (FESEM). The optical transmission of irradiated samples increased and the energy band gap (E) decreased from 2.78 to 2.52 eV with gamma dose. Photoluminescence (PL) spectra revealed the improvement in the emission characteristics of Bi₂S₃ thin films with irradiation in the range of 250–1000 Gy. Impedance spectroscopy investigation exhibited that the resistance due to grain boundaries meaningfully contributed to the electrical characteristics of the Bi₂S₃ thin films. The achieved results suggested that Bi₂S₃ thin films are a good tool for further study of dosimetry and radiation sensing application.

     

Room temperature synthesis of bismuth oxyfluoride nanosheets and nanorods

At room temperature, two different morphological nanoscaled BiO_xF_3 − 2x (BiOF nanosheets and Bi₂₆O₃₈F₂ nanorods) have been prepared via a simple solution-based route in the presence of diethanolamine (DEA) and NaOH. The compositions and morphologies of bismuth oxyfluoride can be selectively prepared by varying the type of additives. The products were characterized by X-ray diffraction (XRD), energy-disperse X-ray analysis (EDXA), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray photoelectron spectrum (XPS). A possible mechanism was introduced to explain the formation of the products.     

A simple route to synthesis of BaCO3 nanostructures in water/ethylene glycol mixed solvents

Barium carbonate (BaCO₃) nanostructures with different morphologies were synthesized using Ba(NO₃)₂ and (NH₄)₂CO₃ in the water/ethylene glycol (EG) mixed solvents by oil bath heating at 80 °C for 30 min. The molar ratio of water to EG had an effect on the morphology of BaCO₃. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM).     

l-Cystine-assisted growth of Sb2S3 nanoribbons via solvothermal route

l-Cystine was successfully used as a novel kind of sulfur source to grow Sb₂S₃ nanoribbons at 180 °C for 24 h in a mixed solution made of ethylene glycol and distilled water. The nanoribbons were usually tens of micronmeters in length, typically 100–300 nm in width. The structure of the nanoribbons was determined to be of the orthorhombic phase. A reasonable possible mechanism for the growth of Sb₂S₃ nanoribbon structures has been proposed. The as-obtained Sb₂S₃ products were examined using diverse techniques including X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), selected-area electron diffraction, and high-resolution TEM.