Cyclic microwave assisted synthesis of Sb2S3 dumb-bells using polyvinylpyrrolidone as a template and splitting agent

Antimony sulfide (Sb₂S₃) was successfully synthesized from antimony chloride (SbCl₃) and sodiumthiosulfate (Na₂S₂O₃) in ethylene glycol (EG) containing different polyvinylpyrrolidone (PVP) masses under cyclic microwave radiation. XRD and SEM show that the products were orthorhombic Sb₂S₃ nanorods forming the dumb-bells. TEM study reveals Sb₂S₃ single-crystal nanorods, growing along the [001] direction. The dumb-bell formation is also proposed, according to the splitting ends and a middle tie-up. Its direct band gap, calculated from UV-visible absorption, is 1.52 eV.     

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.     

Colloidal synthesis of Cu2SnSe3 nanocrystals

While Cu₂SnSe₃ material has various potential applications including acousto-optics and photovoltaics, preparation methods of this material only in a bulk form or a thin film have been reported so far. In this work, for the first time, we demonstrate that highly crystalline Cu₂SnSe₃ nanoparticles can be prepared via colloidal synthesis. The Cu₂SnSe₃ nanocrystals have a cubic crystal structure with a lattice parameter of 5.68 Å, an average diameter of 18 nm, and an atomic ratio of approximately 2:1:3. The nanocrystals can be stably suspended in solution for several months. The suspended nanocrystalline form of Cu₂SnSe₃ could potentially be useful for printable acousto-optic and photovoltaic applications.     

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.     

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.     

Photochemical synthesis and characterization of Bi2S3 nanofibers

Bismuth sulfide (Bi₂S₃) nanofibers have been successfully prepared by a photochemical method from an aqueous solution of bismuth nitrate (Bi(NO₃)₃) and thioacetamide (TAA) in the presence of complexing agents of nitrilotriacetic acid (NTA) at room temperature. It was found that the irradiation time, the pH of the solution, and the species of complexing agents play important roles in the morphology control of the bismuth sulfate (Bi₂S₃) nanomaterials. The nanofibers were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), electron diffraction (ED), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectra (XPS), and UV-Visible absorption spectra (UV-Vis). Probable mechanisms for the photochemical formation of Bi₂S₃ nanofibers in aqueous solutions are proposed. The photochemical method is a convenient approach for controlling the shape for other metal sulfide semiconductor nanocrystals.     

Solar cells with Sb2S3 absorber films

CdS/Sb₂S₃/PbS structures were prepared by sequential chemical deposition of CdS, Sb₂S₃ and PbS thin films on TEC-8 (Pilkington) transparent electrically conductive SnO₂ (TCO) coatings. CdS thin films (100 nm) were deposited with hexagonal structure from Cd-citrate bath and of cubic structure from Cd-ammine/triethanolamine bath. Sb₂S₃ thin films were deposited at 40 °C from a solution mixture of potassium antimony tartrate, triethanolamine, ammonia and thioacetamide(TA) or at 1 to 10 °C from a mixture of antimony trichloride and thiosulfate (TS). These films were made photoconductive by heating at temperatures 250 to 300 °C. When heated in the presence of a chemically deposited Se thin film of 300 nm, a solid solution Sb₂S_1.8Se_1.2 resulted. PbS thin films of 100-200 nm thickness were deposited on the TCO/CdS/Sb₂S₃ or TCO/CdS/Sb₂S_1.8Se_1.2 structure. Graphite paint was applied on the PbS film prior to applying a silver epoxy paint. The cell structures were of area 0.4 cm². The best results reported here is for a cell: TCO/CdS(hex-100 nm)/Sb₂S₃(TS-100 nm)/PbS(200 nm) with open circuit voltage (V_oc) 640 mV, short circuit current density 3.73 mA/cm², fill factor 0.29, and conversion efficiency 0.7% under 1000 Wm^− 2 sunlight. Four series-connected cells of area 1 cm² each gave V_oc of 2 V and short circuit current of 1.15 mA.     

Catalyst-free growth of Sb2Te3 nanowires

In this study, a catalyst-free growth method was discovered to prepare the high-quality single crystal Sb₂Te₃ nanowires from the Al:Ge:Sb:Te thin films. The diameters of Sb₂Te₃ nanowires were found to be ~ 100 nm and their lengths were as great as tens of micrometers. The Al content and the annealing temperature play an important role in the growth of Sb₂Te₃ nanowires. When the Al content (> 12.4 at.%) was sufficiently contained in Al:Ge:Sb:Te film, Sb₂Te₃ nanowires were extruded spontaneously on the surface of thin film with increase in annealing temperatures. Compared with the vapor-liquid-solid method, our method has advantages of low temperature (~ 300 °C) and no impurities, such as a metal catalyst.     

Microwave-enhanced rapid and green synthesis of well crystalline Sb2Se3 nanorods with a flat cross section

Morphology-controlled growth of nanomaterials is an important topic in nanosciences because it is the prerequisite of the applications of nanomaterials. In this work, we reported the microwave-enhanced rapid and green synthesis of Sb₂Se₃ nanorods with a flat cross section through the reaction between selenium powders and sodium antimony tartrate. Microwave irradiation greatly shortened the reaction time, which made the cycle to be as short as 30 min. The intrinsic mechanism for the formation of nanorods with a flat cross section is related to the direction of the unique layer-structured structure of orthorhombic Sb₂Se₃.     

Characterization of Cu3SbS4 microflowers produced by a cyclic microwave radiation

Copper antimony sulfide (Cu₃SbS₄) crystals were produced from mixtures of different molar ratios of CuCl, SbCl₃ and thiourea in 40 and 60 ml ethylene glycol (EG) by a 300 W cyclic microwave radiation (CMR) for different lengths of time. In the present research, tetragonal Cu₃SbS₄ microflowers, characterized by X-ray and electron diffraction including electron microscopy and Raman analyses, were successfully produced in the 40 ml solution containing 2:2:4 molar ratio Cu:Sb:S for 40 cycles. Their UV-visible absorption was studied to determine the energy gap (E_g). A formation mechanism was also proposed to relate with the experimental results.     

Polyol method synthesis and characterization of nanoscale Sb2Se3 wires

Sb₂Se₃ nanowires ([0 0 1] orientation) with diameter of ∼100 nm and high aspect ratio were successfully synthesized in large scale by a facile nonaqueous polyol method, where home-prepared NaHSe alcohol solution is used as selenium source and PEG-400 serves as an excellent solvent and structure director. The product was characterized by XRD, TEM, SAED, HRTEM, EDS and diffuses reflectance spectroscopy, respectively. The effects of the experimental conditions on the final morphologies were also investigated. The method is promising to be extended to synthesize other V₂VI₃ compound semiconductor 1D nanostructure.     

Hydrothermal synthesis and characterization of Bi2O3 nanowires

An alternative two-step method has been proposed for the synthesis of Bi₂O₃ nanowires with a diameter of about 40 nm from common and cost-effective Bi(NO₃)₃·5H₂O, Na₂SO₄, and NaOH. That is, first, Bi₂O(OH)SO₄ nanowires were prepared through the precipitation reaction of Bi(NO₃)₃·5H₂O and Na₂SO₄ in distilled water under the ambient condition and second, monoclinic phase Bi₂O₃ nanowires were prepared via the hydrothermal reaction of Bi₂O(OH)SO₄ and NaOH at 120 °C for 12 h. The resultant products were characterized by X-ray diffraction, field emission scanning electron microscope, and high resolution transmission electron microscopy. In addition, the photocatalytic studies indicated that the as-synthesized Bi₂O₃ nanowires were a kind of promising photocatalyst in remediation of water polluted by some chemically stable azo dyes.     

Improved photodegradation activity of TiO2 via decoration with SnS2 nanoparticles

The particles of TiO₂ modified with various amounts of SnS₂ nanoparticles (TiO₂/SnS₂) were synthesized via the hydrothermal method by reacting SnCl₄·5H₂O with thioacetamide in 5% (vol.) acetic acid aqueous solution in the presence of TiO₂. The obtained products were characterized by using X-ray diffraction, X-ray photoelectron spectroscopy, UV–Vis diffuse reflection spectra, scanning and transmission electron microscopy. The photodegradation activities of TiO₂/SnS₂ composites have been investigated by using methyl orange as target in water under the light irradiation of 250–400, 360–600 and 400–600 nm. It was found that the photodegradation activity of TiO₂/SnS₂ composites depended on the mass ratio of SnS₂ and the wavelength of the irradiating light. The composites containing 33% SnS₂ exhibited the maximum activity under the light irradiation of 250–400 and 360–600 nm. However, the more SnS₂ in the composites, the higher activity appeared under the irradiation of 400–600 nm light. All the results reveal that the composites possess much better activity than the pristine TiO_2.     

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.     

New compounds Cu2MnTi3S8 and Cu2NiTi3S8 with thiospinel structure

Cu₂MnTi₃S₈ and Cu₂NiTi₃S₈ compounds were prepared by high-temperature synthesis. The crystal structure of these quaternary phases was investigated by X-ray powder diffraction. The compounds are described in the thiospinel structure (space group ) with the lattice constants a = 1.00353(1) nm (Cu₂MnTi₃S₈) and a = 0.99716(1) nm (Cu₂NiTi₃S₈). The atomic parameters were calculated in anisotropic approximation (R_I = 0.0456 and R_I = 0.0520 for Cu₂MnTi₃S₈ and Cu₂NiTi₃S₈, respectively).     

Microwave-assisted hydrothermal synthesis and optical property of Co3O4 nanorods

Single crystalline Co₃O₄ nanorods have been successfully synthesized through thermal decomposition of the precursor, which was obtained by the microwave-assisted hydrothermal route. The obtained sample was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectrometer (FT-IR), and X-ray photoelectron spectroscopy (XPS). The results confirm that the resulting oxide was pure single-crystalline Co₃O₄ nanorods. The optical property test indicates that the absorption peak of the nanorods shifts towards short wavelength. And the blue shift phenomenon might be ascribed to the quantum effect.     

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).     

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.     

Mechanochemical synthesis and characterization of TiB2 and VB2 nanopowders

A novel method for the synthesis of transition-metal boride nanopowder has been developed using a mechanochemical reaction between LiBH₄, LiH and transition-metal chloride (TiCl₃ and VCl₃) by high energy ball milling. This method successfully produces TiB₂ and VB₂ particles dispersed within a soluble LiCl matrix. Subsequent washing with distilled water, ethanol and acetone to remove the LiCl matrix phase yields TiB₂ and VB₂ nanopowders of 15-60 nm particle size. From the X-ray diffraction patterns and high resolution transmission electron microscopy image, it is found that each particle is polycrystalline consisting of 3-5 nm crystallites. Neither particle nor crystallite size are increased significantly after heating at 680 °C.