Capsule‐like α‐Fe2O3 nanoparticles: Synthesis,characterization, and growth mechanism

Uniform capsule‐like α‐Fe₂O₃ particles were synthesized via a simple hydrothermal method, employing FeCl₃ and CH₃COONa as the precursors and sodium dodecyl sulfate (SDS) as soft template. X‐ray powder diffraction (XRD), field emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), and high‐resolution transmission electron microscopy were used to characterize the structure of synthesized products. Some factors influencing the formation of capsule‐like α‐Fe₂O₃ particles were systematically investigated, including different kinds of surfactants, the concentration of SDS, and reaction times. The investigation on the evolution formation reveals that SDS was critical to control the morphology of final products, and a possible five‐step growth mechanism was presented by tracking the structures of the products at different reaction stages.     

Structure and photoluminescence properties of SrWO4 3D microspheres synthesized by the surfactant‐assisted hydrothermal method

In this paper, we report large‐scale high‐quality SrWO₄ 3D microspheres synthesized in aqueous solutions under mild conditions with cetyl trimethyl ammonium bromide as a simple cationic surfactant. These crystals have been characterized by X‐ray diffraction, transmission electron microscopy and field emission scanning electron microscopy techniques. The crystal growth processes were employed to investigate the formation mechanism of SrWO₄ 3D microspheres. Room‐temperature photoluminescence indicated that the as‐prepared SrWO₄ 3D microcrystals had strong emission peaks at about 432 and 505 nm, respectively.     

Low‐temperature urea‐assisted hydrothermal synthesis of Bi2S3 nanostructures with different morphologies

Different morphologies of single‐crystalline orthorhombic phase bismuth sulfide (Bi₂S₃) nanostructures, including sub‐microtubes, nanoflowers and nanorods were synthesized by a urea‐assisted hydrothermal method at a low temperature below 120 °C for 12 h. The as‐synthesized powders were characterized by X‐ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high‐resolution transmission electron microscopy (HRTEM) and UV‐vis spectrophotometry. The experimental results showed that the sulfur sources had a great effect on the morphology and size of the resulting powders. The formation mechanism of the Bi₂S₃ nanostructures with different morphologies was discussed. All Bi₂S₃ nanostructures showed an appearance of blue shift relative to the bulk orthorhombic Bi₂S₃, which might be ascribed to the quantum size effect of the final products. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of strontium chloroborate whiskers

Single crystalline strontium chloroborate (Sr₂B₅O₉Cl) whiskers with uniform diameter have been synthesized by a facile route based on the calcination of precursor. The precursor was prepared by the sedimentation reaction between SrCl₂ and Na₂B₄O₇ aqueous solution. The products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared spectrum (FT‐IR). An optimal synthesis temperature for preparing Sr₂B₅O₉Cl whiskers was obtained, and the possible formation process was also presented.     

Preparation and magnetic properties of CoWO4 nanocrystals

Cobalt tungstate (CoWO₄) nanocrystals with an average size of 20–50 nm were synthesized via a template‐ or surfactant‐free hydrothermal route. The crystal structure and morphology of the as‐synthesized CoWO₄ sample were characterized by X‐ray diffraction, scanning electron microscopy and transmission electron microscopy. Magnetic measurements on the as‐synthesized CoWO₄ nanocrystals indicate a Néel temperature (T_N) of ∼40 K. This lower T_N may be a result of the nanostructured particles that reduce the exchange coupling. The new synthetic route presented in this paper has potential applications to fabricate other metal tungstates (MWO₄) materials.     

Hydrothermal synthesis of nano‐crystalline BaMoO4 under mild conditions using simple additive

Large‐scale high‐quality BaMoO₄ nanocrystals have been synthesized in aqueous solutions under mild conditions with citrate as a simple additive. The crystals have bone‐like, spindle‐like and wheatear‐like morphologies assembled from nanoparticles, nanofibers and have been characterized by X‐ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) techniques. The results showed that experimental parameters had great influences on the shape evolution of products. The adjustment of these parameters such as room temperature stirring time, reaction temperature and reaction time of hydrothermal reaction, can lead to obvious morphology changes of products, and the growth mechanism has been proposed. Room‐temperature photoluminescence indicated that the as‐prepared BaMoO₄ nanocrystals had a strong blue emission peak at 481.5 nm. This facile route could be employed to synthesize more promising nanomaterials with interesting self‐assembly structures. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Facile morphology‐controlled hydrothermal synthesis of flower‐like self‐organized ZnO architectures

Flower‐like self‐organized crystalline ZnO architectures were obtained through a facile and controlled hydrothermal process. As‐synthesized products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), high‐resolution transmission electron microscopy (HRTEM), X‐ray diffraction (XRD), electron diffraction and UV‐Vis spectroscopy. XRD and electron diffraction results confirmed the obtained materials are pure wurtzite ZnO. The effects of different ratios of starting materials and solvent on the morphologies of ZnO hydrothermal products were also evaluated by SEM observations. It is suggested that the use of water, rather than ethanol as the solvent, as well as employing a precursor of Zn(Ac)₂ and 2NaOH (v/v) in hydrothermal reactions are responsible for the generation of specific flower‐like self‐assembled ZnO structures. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Controllable synthesis of hierarchical strontium molybdate by sonochemical method

Large‐scale chrysanthemum‐like strontium molybdate (SrMoO₄) with hierarchical structure has been successfully synthesized via a facile and fast ultrasound irradiation approach at room temperature. By varying the experimental conditions, SrMoO₄ with different morphologies, such as spindles, peanuts, spheres, and rods, can be obtained. The products are characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected‐area electron diffraction (SAED). The influent parameters including concentration, pH value, and surfactants have been investigated. A possible growth mechanism is proposed and the shape evolution of the products is characterized. The as‐prepared chrysanthemum‐like SrMoO₄ particles are used as the precursor for electrorheological fluid and their electrorheological property is investigated.     

Preparation of shuttle‐like Sb2S3 nanorod‐bundles via a solvothermal approach under alkaline condition

Uniform shuttle‐like Sb₂S₃ nanorod‐bundles were synthesized via a polyvinylpyrrolidone (PVP) assisted solvothermal approach under alkaline condition, using antimony chloride (SbCl₃) and thiourea (CH₄N₂S, Tu) as the starting materials in ethanol. The phase structure, composition and morphology of the product were characterized by means of X‐ray diffraction (XRD), energy dispersive X‐ray spectrometry (EDS), transmission electron microscopy (TEM), and high‐resolution transmission electron microscopy (HRTEM). XRD and EDS results confirm that the synthesized Sb₂S₃ nanorod‐bundles have an orthorhombic structure and an atomic ratio of 3:2 for S:Sb. TEM and HRTEM results show that the shuttle‐like Sb₂S₃ bundles are composed of nanorods with a size distribution of 20‐40 nm and growing along c‐axis. Furthermore, experiments under different reaction conditions were carried out and the mechanism for the growth of nanorod‐bundles was discussed (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Low temperature synthesis of spindle‐like ZnO nanostructures under microwave irradiation

A simple and general microwave route is developed to synthesize nanostructured ZnO using Zn(acac)₂·H₂O (acac = acetylacetonate) as a single source precursor. The reaction time has a great influence on the morphology of the ZnO nanostructures and an interesting spindle‐like nanostructure is obtained. The microstructure and morphology of the synthesized materials are investigated by X‐ray diffraction (XRD), scanning electron microscopy (SEM), field‐emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high‐resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). It is found that all of them with hexagonal wurtzite phase are of single crystalline structure in nature. Ultraviolet–visible (UV‐vis) absorption spectra of these ZnO nanostructures are investigated and a possible formation mechanism for the spindle‐like ZnO nanostructures is also proposed.     

Facile solvothermal synthesis,growth mechanism and thermoelectric property of flower‐like Bi2Te3

Hierarchical flower‐like Bi₂Te₃ was synthesized through a facile solvothermal method. The crystal structure and morphology of the as‐prepared samples were characterized by X‐ray diffraction (XRD), filed emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and high resolution TEM. The reaction parameters such as reaction time, the amount of glucose, concentration of NaOH and the reaction temperature were systematically investigated. Based on the FESEM observations, a possible mechanism defined as a self‐assembly process accompanied by anisotropic growth mechanism was proposed. Moreover, the thermoelectric properties were measured at the temperature range of 300–600 K. The hierarchical flower‐like Bi₂Te₃ presented good thermoelectrical properties. The maximum ZT value reached up to 0.6 at 600 K, which was higher than that of Bi₂Te₃ nanoparticles.     

Synthesis and characterization of semiconductor metal sulfide nanocrystals using microemulsion technique

The semiconductor nanocrystals ZnS, PbS, CdS and CuS were synthesized via microemulsion technique involving metal acetate, reducing agent (Na₂S) and Triton X‐100 as surfactant. Nanocrystals were characterized by X‐ray diffraction (XRD), transmission electron microscopy (TEM) and dynamic light scattering (DLS). The average size of ZnS, PbS, CdS and CuS nanocrystals were found to be 5.6 nm, 13.3 nm, 11.4 nm and 6.2 nm, respectively. Different parameters like surfactant (Triton X‐100) concentration, water‐to‐surfactant ratio (ω), precursor concentration [zinc acetate, (Zn(AC)₂], reducing agent concentration [sodium sulphide, (Na₂S)] were optimized to synthesize ZnS quantum dots.     

Growth and characterization of large La1‐xPbxMnO3+δ (x=0.32–0.35) crystals

Large crystals of La_0.63Pb_0.37Mn O_3+δ with small La(Pb)‐ deficiency of about 0.005‐0.01 at.% were grown by high temperature solution growth method. The structure of the grown crystals was determined as rhombohedral with R‐3 space group by single‐crystal X‐ray diffractometry. The surface morphology of the crystals and the exact chemical composition was examined by scanning electron microscopy and energy dispersive X‐ray analysis methods, respectively. The IR‐transmission spectrum reveals the presence of Mn³⁺O₆‐ and Mn⁴⁺O₆‐ octahedra in the lattice of La_0.63Pb_0.37Mn O_3+δ crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A simple glucose reduction route for the synthesis of sheet‐like copper dendrites

In the current paper we designed a simple glucose reduction route for synthesis of sheet‐like Cu dendrites on a high yield, using CuSO₄ as the starting material. The reaction was carried out at 180 °C for 18 h in the absence of any structure‐directing agent. The product was characterized by X‐ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron diffraction (ED). Some factors influencing the shapes of Cu microcrystals, including the reaction temperature, time, and the concentration of the starting CuSO₄, were investigated. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Controlled synthesis of various morphologies of nanostructured zinc oxide: flower,nanoplate, and urchin

Nanoplates, flower‐like nanostructure of ZnO were successfully synthesized by employing ZnSO₄·7H₂O, NaOH as the starting materials at 120°C under hydrothermal condition. Keeping the same parameters, ZnO urchin shape was obtained by addition of vitamin C at 190°C. Characterizations were carried out by X‐ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) at room temperature. Selected area electron diffraction (SAED) pattern confirms that the product is single crystalline nature. The possible formation mechanisms for synthesized ZnO nanosturcture with various morphologies have also been proposed. PL spectrum from the ZnO flower‐like structures reveals weak UV emission and strong green emission. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystalline bismuth oxide nanorods fabricated on Pt‐coated substrates using a trimethylbismuth and oxygen mixture

The current work reports the fabrication of crystalline Bi₂O₃ nanorods on Pt‐coated Si substrates using trimethylbismuth and O₂ as the bismuth and the oxygen sources, respectively, in the metalorganic chemical vapor deposition process. Their microstructures were characterized by scanning electron microscopy, X‐ray diffraction, and transmission electron microscopy. The obtained nanorods were crystalline, with their diameters in the range of 20–200 nm. The absence of tip‐nanoparticle and the presence of predeposited Bi₂O₃ layer indicated that the growth was dominated by a vapor‐solid process. The photoluminescence measurements of the Bi₂O₃ nanorods at room temperature exhibited an emission band peaked at around 422 nm. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Hydrothermal synthesis of Bi2Te3 nanowires through the solid-state interdiffusion of Bi and Te atoms on the surface of Te nanowires

Polycrystalline Bi₂Te₃ nanowires were prepared by a hydrothermal method that involved inducing the nucleation of Bi atoms reduced from BiCl₃ on the surface of Te nanowires, which served as sacrificial templates. A Bi–Te alloy is formed by the interdiffusion of Bi and Te atoms at the boundary between the two metals. The Bi₂Te₃ nanowires synthesized in this study had a length of 3–5 μm, which is the same length as that of the Te nanowires, and a diameter of 300–500 nm, which is greater than that of the Te nanowires. The experimental results indicated that volume expansion of the Bi₂Te₃ nanowires was a result of the interdiffusion of Bi and Te atoms when Bi was alloyed on the surface of the Te nanowires. The morphologies of Bi₂Te₃ are strongly dependent on the reaction conditions such as the temperature and the type and concentration of the reducing agent. The morphologies, crystalline structure and physical properties of the product were analyzed by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS).     

Monodisperse CeO2 sub‐micro spherical aggregates with controllable building blocks

Monodisperse CeO₂ spherical aggregates with diameters ranging from 200 to 300 nm have been successfully synthesized through a facile hydrothermal method. The structure and morphology of the samples were characterized by powder X‐ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and field‐emission scanning electron microscopy (FE‐SEM). The building blocks (primary nanocrystals) of the spherical aggregates could be effectively tuned by adding different amount of urea. Furthermore, N₂ adsorption/desorption experiment displays a gradual increase of BET surface areas of spherical aggregates with increasing the amount of urea. Finally, the formation mechanism of CeO₂ spherical aggregates was preliminarily discussed. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Hydrothermal conversion of ZnO2 to ZnO flowers: A mechanistic investigation and characterization

In this article, we report a novel but simple method for the phase transformation of ZnO₂ to flower‐like ZnO microstructures hydrothermally at 90 °C with and without the assistance of hexadecylamine as surfactant. The generation of zincate ion ZnO$^{2-}_{2}$ as a growth unit from the reaction between ZnO₂ and peroxide ion O$^{2-}_{2}$ in situ plays a key role in the phase transformation of ZnO₂ to ZnO. The morphology, structure, and composition of the products have been investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Powder X‐ray diffraction (PXRD) and energy dispersive X‐ray analysis (EDX). It has been demonstrated that the as‐fabricated ZnO flowers are composed of self‐assembled brooms and rods in the presence and absence of hexadecylamine respectively. On the basis of experimental results, a possible reaction mechanism and the growth processes involved in the formation of flower‐like ZnO microstructures are discussed.     

Size-controlled synthesis of LaAlO3 by reverse micelle method: Investigation of the effect of water-to-surfactant ratio on the particle size

Lanthanum monoaluminate (LaAlO₃) nanoparticles have been synthesized using microreactors made of poly(oxyethylene) nonylphenyl ether (Igepal CO-520)/water/cyclohexane microemulsions. The control of particle size was achieved by varying the water-to-surfactant molar ratio. The synthesized and calcined powders were characterized by thermogravimetry–differential thermal analysis (TGA-DTA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). Differential thermal analysis showed that LaAlO₃ phase transformation decreases with increase in water/surfactant (R) value. Pure LaAlO₃ phase was synthesized by annealing at 800 °C for 2 h in air directly from amorphous precursors, without formation of intermediate phase. The average particle size was found to increase with increase in water-to-surfactant ratio (R). FTIR analysis was carried to monitor the elimination of residual oil and surfactant phases from the microemulsion-derived precursor and calcined powder.