Synthesis and characterization of WO<Subscript>3</Subscript> and WS<Subscript>2</Subscript> hexagonal phase nanostructures and catalytic test in sulfur remotion

The aim of the present study was the synthesis and characterization of WO₃ and WS₂ nanostructures in hexagonal phases and the evaluation of the latter as catalyst in the dibenzothiophene hydrodesulfurization reaction. 2H-WS₂ nanostructures were obtained from a precursor WO₃ nanostructure by a two-step hydrothermal/gas phase reaction under well-controlled conditions. All nanostructures were characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, and the specific surface area of the materials was measured using the BET method. The catalytic activity and selectivity measurements of the resulting unsupported WS₂ nanocatalysts are also presented. Catalytic activity was found to be highest for the 2H-WS₂ from the WO₃ nanostructure sulfided at 773 K (rate constant of 3 × 10⁻⁷ mol/g s).     

Fabrication and magnetic properties of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanocrystalline nanotubes

Aligned NiFe₂O₄ polycrystalline nanotubes have been successfully fabricated inside the nanochannels of porous anodic aluminum oxide (AAO) templates by wetting chemical deposition. A mixture of Fe nitrate and Ni nitrate, which was thermally decomposed at no less than 400 °C, was used to yield NiFe₂O₄ tubes. By varying the deposition conditions and the parameters of the templates, we could tailor the lengths and the outer as well as the inner diameters of the tubes. Transmission electron microscopy (TEM) images reveal that the nanotubes are uniform and well isolated. X-ray diffraction (XRD) and selected area electron diffraction (SAED) demonstrate that the as-obtained nanotubes can be indexed to polycrystalline cubic spinel. The Mössbauer spectra show that the magnetic hyperfine field is reduced with the decrease of the metrical temperature as well as the decrease of the size of nanoparticles.     

Synthesis and structure of multi-layered WS<Subscript>2</Subscript>(CoS), MoS<Subscript>2</Subscript>(Mo) nanocapsules and single-layered WS<Subscript>2</Subscript>(W) nanoparticles

Multi-layered MoS₂ (or WS₂) nanocages stuffed with Mo (or CoS/CoO) nanocrystals have been synthesized by using the reaction between metal nanoparticles and sulfur powders. This simple synthesis method, different from the conventional methods for synthesizing pure inorganic fullerenes, is also potentially important for large-scale synthesis of nanoparticles of other metal dichalcogenide. Besides the multi-layered WS₂ nanocapsules, we have successfully fabricated nanocapsules with a single-layered WS₂ sheet encapsulating W by using the arc-discharge method. We discuss possible mechanisms for the formation of the unique core-shell structured nanocapsules.     

Preparation and characterization of various morphologies of SrFe<Subscript>12</Subscript>O<Subscript>19</Subscript> nano-structures: investigation of magnetization and coercivity

Hard magnetic SrFe₁₂O₁₉ (SrFe) nanostructures were synthesized by a facile chemical precipitation procedure. The influence of temperature, concentration and different capping agents on the particle size and morphology of the magnetic nanoparticles was investigated. The synthesized ferrites were characterized by X-ray diffraction pattern, scanning electron microscope, and Fourier transform infrared spectroscopy. Ferromagnetic property of the hexaferrite nanostructures was determined by vibrating sample magnetometer. The results show hard magnetic ferrite with a high coercivity about 2800–4000 Oe and saturation magnetization around 11–14 emu/g were synthesized.     

Preparation and characterization of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/Ag composite magnetic nanoparticles

Fe₃O₄ magnetic nanoparticles being used as seeding materials, Ag⁺ ions on the Fe₃O₄ magnetic nanoparticles reduced to the metal form by tartaric acid using heated treatment. Thus, Fe₃O₄/Ag composite core-shell magnetic nanoparticles were synthesized. The products were characterized by transmission electron microscope (TEM) and x-ray diffraction (XRD). Both TEM and XRD results showed that the Ag nanoparticles were well distributed on the surface of Fe₃O₄ magnetic nanoparticles. The size for Fe₃O₄/Ag composite magnetic nanoparticles which were spherical shape was ≃40 nm. Furthermore, the magnetic properties of samples were characterized on a vibrating sample magnetometer. Under optimal conditions, Fe₃O₄/Ag composite nanoparticles showed higher magnetism than pure Fe₃O₄ nanoparticles. The text was submitted by the authors in English.     

Formation of TiO<Subscript>2</Subscript> nanotubes by thermal decomposition of poly(vinyl alcohol)-titanium alkoxide hybrid nanofibers

Anatase type TiO₂ nanotubes were formed by calcination of poly(vinyl alcohol)-Ti alkoxide hybrid precursor nanofibers in air. The outer and inner diameters of the TiO₂ nanotubes calcined at 500 °C for 5 h were ca. 440 nm and ca. 270 nm, respectively. The specific surface area of the TiO₂ nanotubes was 38.8 m²/g, and the existence of mesopores (average pore diameter, 14.8 nm) on the nanotube wall was indicated by the nitrogen adsorption isotherm (−196 °C). The photocatalysis of the TiO₂ nanotubes was superior to that of commercially available anatase type TiO₂ nanoparticles.     

Dual-mode protein detection based on Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>-Au hybrid nanoparticles

A facile method of synthesizing Fe₃O₄-Au hybrid nanoparticles is reported utilizing the multifunctional nature of polyethyleneimine (PEI). An abundance of 5 nm gold nanoparticles were attached to 50 nm Fe₃O₄ nanoparticles via the covalent binding between the -NH₂ groups of the PEI and Au nanoparticles, as well as the electrostatic interaction between the negatively charged citrate-coated Au nanoparticles and the positively charged PEI-coated Fe₃O₄ nanoparticles. The as-prepared Fe₃O₄-Au hybrid nanoparticles, which combine the merits of magnetic materials and gold, were successfully employed for the first time in the dual-mode detection of carcinoembryonic antigen (CEA) via electrochemical and surface-enhanced Raman scattering (SERS) methods. Both methods make clever use of Fe₃O₄-Au nanoparticles and can accurately verify the presence of antigens. In particular, the electrochemical immunosensor detection displays a wide linear range (0.01–10 ng/mL) of response with a low detection limit (10 pg/mL), while the SERS method responds to even lower antigen concentrations with a wider detection range. The Fe₃O₄-Au hybrid nanoparticles therefore exhibit great potential for biomedical applications.      

Microwave-hydrothermal synthesis of Y<Subscript>3</Subscript>Fe<Subscript>3.35</Subscript>Al<Subscript>1.65</Subscript>O<Subscript>12</Subscript> nanoparticles for magneto-hyperthermia application

Crystalline aluminum substituted yttrium iron garnet nanoparticles Y₃Fe_3.35Al_1.65O₁₂ (YIG) was synthesized by hydrothermal microwave synthesis at 140 °C with soaking times ranging from 15 to 60 min. X-ray diffraction confirmed the single-phase YIG nanoparticles excluding the presence of any other phases in the reaction products. The Raman spectra revealed that the largest soaking time provides greater energy crystallization causing changes of lattice vibration and a certain degree of disorder in the crystal lattice. Field emission gun-scanning electron microscopy and high resolution transmission electronic microscopic revealed a homogeneous size distribution of nanometric YIG powders with agglomerated particles. Magnetic measurements were achieved by using a vibrating-sample magnetometer unit. YIG nanoparticles have great potential in magneto-hyperthermia application once in vivo applications magnetic induction heating ferromagnetic compounds generate heat in AC magnetic fields.     

Hydrothermal synthesis and magnetic properties of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles and nanorods

NiFe₂O₄ nanoparticles and nanorods were synthesized by a facile hydrothermal treatment of Ni(DS)₂ (Nickel dodecyl sulfate), FeCl₃, and NaOH aqueous solution at 120 °C. The products were characterized by powder X-ray diffraction, transmission electron microscopy, and selected area electron diffraction. The magnetic properties were evaluated using a vibrating sample magnetometer. The probable mechanism of the formation of NiFe₂O₄ nanoparticles and nanorods was discussed.     

SrFe<Subscript>12</Subscript>O<Subscript>19</Subscript> ferrites and hard magnetic PVA nanocomposite: investigation of magnetization,coecivity and remanence

In this work, various morphologies of SrFe₁₂O₁₉ (SrFe) nanostructures were synthesized via a simple sol–gel method. The effect of concentration, temperature and various surfactants on the morphology and particle size of the magnetic seeds was investigated. The prepared magnetic products were characterized by X-ray diffraction, scanning electron microscopy, and Fourier transform infrared spectroscopy techniques. Alternating gradient force magnetometry reveals that the samples exhibit hard magnetic property with the coercivity up to 5300 Oe. Strontium ferrite was added to poly vinyl alcohol to prepare the magnetic polymeric matrix thin film nanocomposites. The saturation magnetization and coercivity decreased due to agglomeration of magnetic nanoparticles in polymer matrix.     

Solvothermal synthesis of CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> hollow spheres

Hollow CoFe₂O₄ spheres consisted of CoFe₂O₄ nanoparticles were synthesized by a facile solvothermal treatment of an ethylene glycol solution of FeCl₃ · 6H₂O, CoCl₂ · 6H₂O, and NaAc at 200 °C in the presence of polyethylene glycol and oleic acid. The products were characterized by powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction, high-resolution transmission microscopy, scanning electron microscopy. The magnetic properties were evaluated using a vibrating sample magnetometer. The probable mechanism of the formation of Hollow CoFe₂O₄ spheres was discussed. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis of In(OH)<Subscript>3</Subscript> and In<Subscript>2</Subscript>O<Subscript>3</Subscript> nanomaterials incorporating Au

In(OH)₃ and In₂O₃ nanocrystals of rectangular shape and incorporating Au were synthesized with a hydrothermal process and thermal decomposition. Powder X-ray diffraction, electron microscopy (SEM, TEM), and energy-dispersive spectroscopy studies reveal that elemental Au nanoparticles are dispersed on the surface of In(OH)₃ rectangular nanocrystals and incorporated into In₂O₃ nanoporous particles. UV–vis spectral measurements reveal a surface-enchanced plasma band near λ ~532 nm for both Au-incorporating nanomaterials. The BET surface areas of Au-incorporating In(OH)₃ and In₂O₃ are 26.2 and 35.5 m²/g, respectively. The incorporation of elemental Au in In(OH)₃ and In₂O₃ nanomaterials is attractive for sensor, catalyst and solar-cell applications.     

Dispersion effect and auto-reconditioning performance of nanometer WS<Subscript>2</Subscript> particles in green lubricant

This paper reported on dispersion effect and dispersing techniques of nanometer WS₂ particles in the green lubricant concocted by us. And it also researched on auto-reconditioning performance of nanometer WS₂ particles to the abrasive surfaces of steel ball from four-ball tribology test and piston ring from engine lubrication test. The treated and untreated nanometer WS₂ particles were analysed by infrared spectrum. And the elementary component and interior elementary distribution of abrasive surface repaired by nanometer WS₂ particles were analysed by multifunction electron spectrometer. The results showed that the combinative method of ultrasonic dispersion, mechanical agitation and surface modification could improve the dispersion uniformity and stability of nanometer WS₂ particles in the green lubricant effectively. And the optimal ratio of the mass between surface modifier and nanometer WS₂ particles was 1: 2.5, the optimal treating time was 5 h. And IR analysis indicated that surface modifier could react with hydroxide radicals on surfaces of WS₂ particles and modify the surfaces, and the long lipophilic groups on surfaces of nanometer WS₂ particles could stretch in oil adequately and form steric hindrance layers between particles which prevented particles from conglomerating and depositing. In addition, tribological tests and surface analysis indicated that there were WS₂ adsorption film and reaction film on abrasive surfaces during the tribological tests, which could fill and level up the furrows on abrasive surfaces. As a result, the abrasive surfaces were repaired effectively by nanometer WS₂ particles.     

Effects of Nd concentration on structural and magnetic properties of ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles

Zinc ferrite nanomaterials have been received significant attention in recent years on account of their potential applications in the fields of electronics, optoelectronics and magnetics. To enhance the magnetic properties of zinc ferrites, Nd-doped zinc ferrites (ZnFe_2?xNd_xO₄, x?=?0, 0.01, 0.02, 0.03) nanoparticles (NPs) have been prepared by the sol–gel method. The effects of Nd doping concentration on the structural and magnetic properties of zinc ferrites were studied. The results of X-ray diffraction, scanning electron microscopy, transmission electron microscopy and X-ray photoelectron spectroscopy indicated that the Nd ions were incorporated into the crystal lattice of ZnFe₂O₄ and substituted for the Fe³⁺ sites. Unlike pure zinc ferrites with paramagnetism, Nd doped ZnFe₂O₄ NPs were superparamagnetic at room temperature. Vibrating sample magnetometry results showed, with the increase of Nd content, the saturation magnetization of Nd doped ZnFe₂O₄ NPs increased.     

Different morphologies fabrication of NiAl<Subscript>2</Subscript>O<Subscript>4</Subscript> nanostructures with the aid of new template and its photocatalyst application

In the area of water purification, nanotechnology offers the possibility of an efficient removal of pollutants and germs. Nowadays, nanostructures used for detection and removal of chemical and biological substances include metals, azo dyes, nutrients, cyanide, organics, algae, bacteria, parasites, and etc. In the current study, an attempt is made to synthesize and characterization of NiAl₂O₄ nanostructures in an aqueous environment through the simple sol–gel method. Besides, three capping agents as glycine, asparagine, and alanine were used to investigate their effects on the morphology and particle size of NiAl₂O₄ nanostructures. This method starts from of the precursor complex, and involves the formation of homogeneous solid intermediates, reducing atomic diffusion processes during thermal treatment. The formation of pure crystallized NiAl₂O₄ nanocrystals occurred when the precursor was heat-treated at 800 °C in air for 150 min. The stages of the formation of NiAl₂O₄, as well as the characterization of the resulting compounds were done made using UV–Vis diffuse reflectance spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray microanalysis, and X-ray diffraction. The magnetic properties of as-prepared NiAl₂O₄ nanostructures were also investigated with vibrating sample magnetometer. Furthermore, the photocatalytic properties of as synthesized NiAl₂O₄ were evaluated by degradation of methyl orange as water contaminant.     

Co<Subscript>2</Subscript>SiO<Subscript>4</Subscript> nanostructures/nanocomposites: synthesis and investigations of optical,magnetic, photocatalytic,thermal stability and flame retardant properties

Cobalt orthosilicate (Co₂SiO₄) nanostructures and nanocomposites were successfully synthesized via a sol–gel method, by controlling different conditions. The gels were prepared starting from cobalt (II) acetatete tetrahydrate (Co(CH₃COO)₂·4H₂O), tetraethyl orthosilicate, NH₃ and carbohydrate at calcination temperature 500–700 °C for 5 h. We choose 700 °C as optimum calcination temperature base on XRD results. SEM images showed that NH₃ and glucose are optimum catalysis and capping agent, respectively, in our experimental conditions. For the first time, glucose, fructose, sucrose, maltose and lactose were applied as capping agents to green synthesis of cobalt orthosilicates. The optical and magnetic properties of Co₂SiO₄ nanostructures were investigated by UV–Vis and VSM, respectively. Also, for the first time photocatalytic behavior of these nanostructures was evaluated using UV–Vis and degradation of methyl orange, methylene blue, erythrosine and eosine. DSC and TG curves of the nanocomposites showed both thermal stability and flame retardant property for Co₂SiO₄ nanocomposites prepared in the presence of the PS and PSU.     

Preparation of magnetic composites through SrO-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass crystallization

Glasses with nominal compositions 11SrO · 5.5Fe₂O₃ · 4.5Al₂O₃ · 4B₂O₃ (1) and 15SrO · 5.5Fe₂O₃ · 4.5Al₂O₃ · 4B₂O₃ (2) were prepared by rapidly quenching oxide melts between counterrotating steel rollers. The glasses were then heat-treated in the range 650–950°C to produce glass-ceramic samples. The samples were characterized by X-ray diffraction, electron microscopy, and magnetic measurements. The phase composition of the glass-ceramics was determined, and their microstructure and magnetic properties were studied. The annealing temperature was shown to have a strong effect on the coercivity of the materials, which reaches 650 and 570 kA/m for compositions 1 and 2, respectively.     

Facile synthesis and characterization of CdTiO<Subscript>3</Subscript> nanoparticles by Pechini sol–gel method

In this work, CdTiO₃ nanoparticles were synthesized through reaction between Cd(CH₃COO)₂.2H₂O, Ti(OC₄H₉)₄, trimesic acid as a new chelating agent and ethanol as solvent by Pechini sol–gel method. X-ray diffraction (XRD) patterns showed that CdTiO₃ nanostructures have rhombohedral structure with diameter of about 35.61 nm. The structure, morphology and size of CdTiO₃ nanoparticles were characterized by FT-IR, XRD, SEM and EDAX. The optical properties of the products were studied by DRS. Based on the results of experiments, it was found that temperature and time of calcination, pH and the solvent of reaction are important parameters for formation of CdTiO₃ nanoparticles. Utilizing trimesic acid (benzene-1,3,5-tricarboxylic acid) as a new chelating agent for preparation of CdTiO₃ nanostructures was initiative of this work.     

Enhanced electrochemical performance of Na<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>2</Subscript>F<Subscript>3</Subscript> for Na-ion batteries with nanostructure and carbon coating

Carbon-coating Na₃V₂(PO₄)₂F₃ nanoparticles (NVPF@C NP) were prepared by a hydrothermal assisted sol–gel method and applied as cathode materials for Na-ion batteries. The as-prepared nanocomposites were composed of Na₃V₂(PO₄)₂F₃ nanoparticles with a typical size of ~?100 nm and an amorphous carbon layer with the thickness of ~?5 nm. Cyclic voltammetry, rate and cycling, and electrochemical impedance spectroscopy tests were used to discuss the effect of carbon coating and nanostructure. Results display that the as-prepared NVPF@C NP demonstrates a higher rate capability and better long cycling performance compared with bare Na₃V₂(PO₄)₂F₃ bulk (72 mA h g^?1 at 10 C vs 39 mA h g^?1 at 10 and 1 C capacity retention of 95% vs 88% after 50 cycles). The remarking electrode performance was attributed to the combination of nanostructure and carbon coating, which can provide short Na-ion diffusion distance and rapid electron migration.     

Electrocatalytic applications of platinum-decorated TiO<Subscript>2</Subscript> nanotubes prepared by a fully wet-chemical synthesis

Pt-decorated \(\hbox {TiO}_{2}\) nanotubes Pt@TiO₂ are prepared only by applying a set of facile wet-chemical redox reactions to ion track-etched polycarbonate templates. First, a homogeneous layer of Pt nanoparticles is deposited onto the complex template surface by reducing potassium tetrachloroplatinate with absorbed dimethylaminoborane. Second, the template is coated with a conformal \(\hbox {TiO}_{2}\) layer, using a chemical bath deposition reaction based on titanium(III) chloride. After the removal of the template, the rutile-type \(\hbox {TiO}_{2}\) nanotubes remain decorated with Pt nanoparticles and nanoparticle-clusters on their outside. During the process, neither vacuum techniques nor external current sources or addition of heat are employed. The crystallinity, composition, and morphology of the composite nanotubes are analysed by X-ray diffraction, scanning and transmission electron microscopy as well as by energy-dispersive X-ray spectroscopy. Finally, the obtained materials are examplarily applied in the electrooxidation of ethanol and formic acid, and their performances have been evaluated. Compared to conventional carbon black-supported Pt nanoparticles, the Pt@TiO₂ nanotubes show higher reaction rates. Mass activities of 2.36 \(\hbox {A}\hbox { mg}_{\rm Pt}^{-1}\hbox { cm}^{-2}\) are reached in ethanol oxidation and 7.56 \(\hbox {A}\hbox { mg}_{\rm Pt}^{-1}\hbox { cm}^{-2}\) in the formic acid oxidation. The present structures are able to exploit the synergy of Pt and \(\hbox {TiO}_{2}\) with a bifunctional mechanism to result in powerful but easy-to-fabricate catalyst structures. They represent an easily producible type of composite nanostructures which can be applied in various fields such as in catalytics and sensor technology.