Synthesis of Sb2S3 peanut-shaped superstructures

Peanut-shaped Sb₂S₃ superstructures have been synthesized via a hydrothermal process at 120 °C for 8 h using hydrochloric acid and antimony O-benzyl dithiocarbonate (benzylxanthate, Sb(S₂COC₇H₇)₃) as starting materials. The powder X-ray diffraction (XRD) pattern shows the product corresponds to the pure orthorhombic phase of Sb₂S₃, the purity and composition of which are further confirmed by X-ray photoelectron spectroscopy (XPS). Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) studies reveal that the peanut-shaped Sb₂S₃ superstructures are aggregated by nanorods. The possible mechanistic pathways in the formation of the structures are discussed.     

Microwave synthesis of nanocrystalline Sb2S3 and its electrochemical properties

Nanocrystalline antimony trisulfide (Sb₂S₃) was successfully synthesized via microwave irradiation by the reaction of antimony trichloride (SbCl₃) and thiourea (CS(NH₂)₂) with PVP as the surfactant. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and high resolution TEM (HRTEM). XRD results show that the as-prepared sample is orthorhombic-phase Sb₂S₃. TEM image of the as-prepared Sb₂S₃ shows the rod-like structure. HRTEM image indicates that rodbundles of Sb₂S₃ consists of a number nanorods with the diameter ranging from 30 nm to 50 nm. Detailed HRTEM image demonstrates the preferential direction growth of the Sb₂S₃ nanorods. The electrochemical properties of Sb₂S₃ were primarily investigated by constant current charge/discharge cycling tests in lithium hexafluorophosphate (LiPF₆) solution. The possible electrochemical reaction mechanism was explained. The results indicate that the nanocrystalline Sb₂S₃ shows potential application in the field of the electrode materials.     

Building crystalline Sb2S3 nanowire dandelions with multiple crystal splitting motif

Crystalline dandelion-like antimony (III) sulfide (Sb₂S₃) nanowires were synthesized by a PEG-assisted solvothermal process. The orthorhombic crystal structure and dandelion-like multi-branched nanowire morphology were revealed by X-ray diffractometry (XRD) and scanning electron microscopy (SEM) respectively. High-resolution transmission electron microscopy (TEM) identified that the highly crystalline Sb₂S₃ nanowires grew along the [001] direction with individual wire diameter of 195 ± 52 nm. The band gap of the Sb₂S₃ nanowires was measured to be ca. 1.67 eV. A combination of PEG-templated assembly and crystal splitting mechanism was likely responsible for the growth of the observed nanowire dandelion structures.     

Preparation of ultra-long Sb2Se3 nanoribbons via a short-time solvothermal process

Large-scale antimony selenide (Sb₂Se₃) nanoribbons with uniform size have been prepared by solvothermal method using antimony chloride (SbCl₃), tartaric acid (C₄H₆O₆) and selenium metal powder (Se) as raw materials, N, N-dimethylformamide (DMF) as the solvent at 180 °C for 4 h. The powder X-ray diffraction (XRD) pattern shows the Sb₂Se₃ crystals belong to the orthorhombic phase with calculated lattice constants a = 1.159, b = 1.172 and c = 0.3978 nm. The quantification of EDS analysis peaks gives an atomic ratio of 2:3 for Sb:Se. Transmission electron microscopic (TEM) studies reveal the appearance of as-prepared Sb₂Se₃ is ribbon-like with the typical width of ca. 20 nm. Finally the influences of the reaction conditions are discussed and a possible mechanism for the formation of Sb₂Se₃ nanoribbons is proposed.     

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.     

Preparation of rod-like Sb2S3 dendrites processed in conventional hydrothermal

Large-scale rod-like antimony sulfide (Sb₂S₃) dendrites have been prepared by hydrothermal method using antimony chloride (SbCl₃), citric acid and thioacetamide as raw materials at 160 °C for 12 h. The powder X-ray diffraction pattern shows the Sb₂S₃ crystals belong to the orthorhombic phase with calculated lattice parameters a = 1.120 nm, b = 1.128 nm and c = 0.3830 nm. The quantification of energy dispersive X-ray spectrometry analysis peaks gives an atomic ratio of 2:3 for Sb:S. Transmission electron microscopy micrograph studies reveal the appearance of the as-prepared Sb₂S₃ is dendrites-like which is composed of nanorods with the typical width of 300-500 nm and length of 5-20 µm. Finally the influences of the reaction conditions are discussed and a possible mechanism for the formation of rod-like Sb₂S₃ dendrites is proposed.     

Photoluminescence properties of the In2O3 octahedrons synthesized by carbothermal reduction method

In₂O₃ octahedrons were synthesized by carbothermal reduction method. The products were characterized by X-ray diffraction (XRD), energy dispersive X-ray (EDX), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction analysis (SAED) and room-temperature photoluminescence (PL) spectra. The results show that the products are single-crystalline In₂O₃ octahedrons with the arrises length in the range of 400-3000 nm. The PL spectra displays blue and green emission peaks which can be indexed to default and oxygen vacancies; blue-shift and intensity decrease was observed when excitation wavelength decreases from 380 nm to 325 nm. The growth mechanism of the In₂O₃ octahedrons is discussed.     

Large-scale synthesis of ultralong Sb2S3 sub-microwires via a hydrothermal process

This paper describes an ethylene glycol (EG)-assisted approach to the large-scale ultralong Sb₂S₃ sub-microwires, formed by a simple hydrothermal reaction between SbCl₃ and Na₂S in the presence of distilled water. Transmission electron microscopy and scanning electron microscopy studies indicate that these Sb₂S₃ sub-microwires possess a diameter around 200 nm and length up to 100 μm. High-resolution transmission electron microscopy and selected area electron diffraction studies reveal that each Sb₂S₃ sub-microwire is a single-crystal along the [0 0 1] direction. The possible formation mechanism of the sub-microwires was discussed. The effects of volume ratio of EG/water, reaction temperature and the concentration of CO(NH₂)₂ on the morphology of Sb₂S₃ sub-microwires were also investigated.     

Molten salt synthesis of single-crystal Co3O4 nanorods

The synthesis of the single-crystal Co₃O₄ nanorods by molten salt approach was reported for the first time. The products were characterized by Transmission electron microscopy (TEM), X-ray diffraction (XRD), High-resolution transmission electron microscopy (HRTEM) and Selected-area electron diffraction (SAED). TEM results indicate that these nanorods have diameters of about 150 nm and lengths of about 2 μm. According to the analysis of the SAED and HRTEM results, we drew the conclusion that these nanorods grew along an unusual [− 1,− 1,15] direction by Ostwald ripening mechanism.     

Synthesis of Sb2O3 nanorods under hydrothermal conditions

Sb₂O₃ nanorods were successfully prepared via a mild hydrothermal route based on the reactions between SbCl₃ and NH₃·H₂O in aqueous solution at 120-180 °C for 12 h. The as-prepared Sb₂O₃ nanorods were characterized by X-ray diffraction (XRD), transmission electronic microscopy (TEM), and X-ray photoelctron spectroscopy (XPS). Results showed that NH₃·H₂O played a significant role in the formation of Sb₂O₃ nanorods. The presence of NH₃·H₂O could greatly favor the reaction progress toward the right-hand side and led to the orientation growth of Sb₂O₃ nanorods. A possible mechanism for the formation of Sb₂O₃ nanocrystallites was discussed.     

Synthesis and characterization of C3N4 nanowires and pseudocubic C3N4 polycrystalline nanoparticles

C₃N₄ nanowires and pseudocubic C₃N₄ polycrystalline nanoparticles have been synthesized by the reaction between C₃N₃Cl₃ and NaN₃ with Zn powder as catalyst. The process was carried out using a constant-pressure benzene thermal method at 40 MPa and 220 °C. The prepared nanowires have a diameter range of 3-6 nm and length range of 100-200 nm, while the diameters of the nanoparticles range from 10 nm to 40 nm. The as-prepared samples were characterized by X-ray powder diffraction (XRD), Fourier transform spectroscopy (FTIR), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy (XPS).     

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.     

Synthesis of Sb2Te3 nanopowders by vacuum arc plasma evaporation

Taking elemental antimony and tellurium as source materials, Sb₂Te₃ nanopowders were prepared by vacuum arc plasma evaporation technique. Microstructure and morphology of the samples were characterized via X-ray diffraction and field emission scanning electron microscope. Compositional analysis was carried out by energy dispersive analysis of X-rays. Lattice constants (a = 4.267 Å, c = 30.469 Å) of Sb₂Te₃ nanopowders are calculated by (015) and (110) diffraction peaks of X-ray diffraction patterns. Field emission scanning electron microscope surface morphology of the nanopowders shows the irregular polyhedron and rhombohedral structure. Atoms percentage of the nanopowders is calculated by quantitative analysis using energy dispersive analysis of X-rays spectrum. The experimental results show that the percentages of Sb and Te atoms are 41.3% and 58.7% respectively.     

Preparation of Sb<Subscript>2</Subscript>S<Subscript>3</Subscript> film on functional organic self-assembled monolayers by chemical bath deposition

In this work, self-assembled monolayers (SAMs) of octadecyltrichlorosilane (OTS) were applied to induce the nucleation and growth of the antimony sulfide (Sb₂S₃) films on the functional ITO glass substrate at low temperature. The structure, morphology, and optical properties of the Sb₂S₃ films were investigated by X-ray diffraction, scanning electron microscopy, X-ray energy dispersive spectroscopy, and UV–vis spectroscopy. After thermal treatment at 200 °C for 1 h in air, the orthorhombic Sb₂S₃ was formed as a predominant phase in the deposited thin films. When the deposited films were thermally treated at 400 °C for 1 h in air, the orthorhombic Sb₂S₃ was decomposed and a cubic Sb₂O₃ was formed. The optical band energies of the as-deposited and thermally treated Sb₂S₃ films at 200 °C for 1 h in air and nitrogen were found to be 2.05 eV, 1.77, and 1.76 eV, respectively. As chemical templates, the OTS-functionalized SAMs played an important role in controlling the nucleation and growth of Sb₂S₃ films at low temperature. The results obtained from different preparation parameters applied in the present work will allow controlling the growth of the Sb₂S₃ films with uniform surface.     

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).     

Synthesis RMn2O5 (R = Gd and Sm) nano- and microstructures by a simple hydrothermal method

Single-phase RMn₂O₅ (R = Gd and Sm) nano- and microstructures have been successfully synthesized via a simple hydrothermal process at 250 °C for 24 h using NaOH as mineralizer. X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selective area electron diffraction patterns (SAED) were used to characterize the as-synthesized GdMn₂O₅ and SmMn₂O₅ samples. The effect of NaOH concentration and the molar ratio of Mn²⁺/Mn⁷⁺ on the morphology and size of the final products was studied, and a possible formation mechanism of RMn₂O₅ (R = Gd and Sm) nanoplates and nanorods under hydrothermal conditions was proposed.     

Hydrothermal synthesis of single-crystal BaTiO3 dendrites

In this paper, we report a simple hydrothermal method without any surfactants, for the first time, to synthesize single-crystal BaTiO₃ dendrites. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). The KOH concentration was found to be vital to the final formation of BaTiO₃ dendrites. An obvious morphology evolution from sphere-like shape to dendrite was observed when KOH concentration was decreased from 1 M to 0.1 M. It is rational to expect that dendritic structures of other perovskite oxides may also be synthesized by this simple method.     

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 and characterization of octahedral PbF2

The novel 3D octahedron-like PbF₂ structures with dimension of 2-4 µm have been successfully synthesized by a simple route at low temperature. The morphologies and structures of as-prepared products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The growth mechanism has been proposed for octahedral PbF₂. It was found that the aging time is important for the formation of 3D octahedron-like PbF₂ structures. The room-temperature photoluminescence measurements revealed a strong blue emission band at 485 nm. It was indicated that the as-prepared octahedral PbF₂ could have the potential application in optoelectronic devices.     

Photocatalytic degradation of pendimethalin over Cu2O/SnO2/graphene and SnO2/graphene nanocomposite photocatalysts under visible light irradiation

The Cu₂O/SnO₂/graphene (CSG) and SnO₂/graphene (SG) nanocomposite photocatalysts were prepared by simple sol-gel growth method, and characterized by Fourier transform infrared spectra (FTIR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET) measurements, respectively. The photocatalytic efficiency of catalysts were evaluated by degradation of pendimethalin under visible light irradiation (λ > 420 nm), which conformed that CSG and SG exhibited better photocatalytic activity than SnO₂ or graphene alone. An effort has been made to correlate the photoelectro-chemical behavior of these samples to the rate of photocatalytic degradation of pendimethalin.