Surfactant controlled synthesis of crystalline phosphovanadate nanorods

Phosphovanadate nanorods were obtained in a reaction of vanadium (V) oxide as a precursor and a cationic surfactant, dodecylpyridinium chloride, as structure directing template at pH ∼3 at room temperature. The composition and morphology of the nanorods was established by powder X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The obtained nanorods have diameters of 40-60 nm with lengths up to 1 μm. The effect of reaction parameters such as concentration of surfactant and pH of the solution on the growth of nanorods has been investigated. A plausible mechanism involving the coalescence of nanoparticle ‘seeds’ leading to one-dimensional nanorods is also discussed. The same reaction when performed under hydrothermal condition, keeping other reaction parameters unchanged, resulted in the formation of phosphovanadate nanospheres of diameter 10-15 nm.     

Sonochemical synthesis of ZnO nanoparticles: The effect of temperature and sonication power

ZnO nanoparticles were synthesized by drop-wise addition of ZnCl₂ solution to KOH, in different temperatures and sonication output powers. The morphologies and structure of resulting materials were characterized by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The morphology of the products was determined to be a mixture of nano rods as well as nanoparticles depending to sonication output power and temperature. A reduction in nanoparticles and aggregates sizes as well as amount of byproducts was observed by increasing the sonication output power. A combination of sonication output power and temperature was also studied on the properties of the product. At 70 °C and 45 W sonication output power, the smallest nanoparticles as well as narrower range of sizes in addition to minimum amount of byproducts was obtained in this work.     

Hydrothermal routes to various controllable morphologies of nanostructural lithium aluminate

The α-LiAlO₂ powders have been successfully prepared by a hydrothermal route based on using the surfactant of heax-adecyltrimethyl ammonium bromide (CTAB) as the template. One-dimensional (1D) nanorods with higher and lower aspect ratio, 2D mesoporous microsheets were respectively observed with different concentration of the surfactants. A high specific surface area up to 151 m²/g was obtained by this method. The formation mechanism of the nanostructural lithium aluminate was proposed.     

One-step synthesis of UV-induced Pt nanotrees on the surface of DNA network

Platinum metal nanotrees were prepared with assembling Pt nanoparticles onto DNA network template and reducing metal ions by photoinduced method. The concentration of DNA network and the reaction time play important roles in forming platinum nanotrees. The mechanism on the formation of the Pt nanotree is also discussed.     

Thermal-treatment effect on the photoluminescence and gas-sensing properties of tungsten oxide nanowires

Single-crystalline non-stoichiometric tungsten oxide nanowires were initially prepared using a simple solvothermal method. High resolution transmission electron microscopy (HRTEM) investigations indicate that the tungsten oxide nanowires exhibit various crystal defects, including stacking faults, dislocations, and vacancies. A possible defect-induced mechanism was proposed to account for the temperature-dependent morphological evolution of the tungsten oxide nanowires under thermal processing. Due to the high specific surface areas and non-stoichiometric crystal structure, the original tungsten oxide nanowires were highly sensitive to ppm level ethanol at room temperature. Thermal treatment under dry air condition was found to deteriorate the selectivity of room-temperature tungsten oxide sensors, and 400 °C may be considered as the top temperature limit in sensor applications for the solvothermally-prepared nanowires. The photoluminescence (PL) characteristics of tungsten oxide nanowires were also strongly influenced by thermal treatment.     

Synthesis and characterization of Fe(III)-silicate precipitation tubes

Fe(III)-silicate precipitation tubes synthesized through “silica garden” route have been characterized using a number of analytical techniques including X-ray diffraction, infrared spectroscopy, atomic force microscopy, scanning and transmission electron microscopy. These tubes are brittle and amorphous and are hierarchically built from smaller tubes of 5-10 nm diameters. They remain amorphous at least up to 650 °C. Crystobalite and hematite are the major phases present in Fe(III)-silicate tubes heated at 850 °C. Morphology and chemical compositions at the external and internal walls of these tubes are remarkably different. These tubes are porous with high BET surface area of 291.2 m²/g. Fe(III)-silicate tubes contain significant amount of physically and chemically bound moisture. They show promise as an adsorbent for Pb(II), Zn(II), and Cr(III) in aqueous medium.     

Facile synthesis of highly branched jacks-like ZnO nanorods and their applications in dye-sensitized solar cells

Highly branched, jacks-like ZnO nanorods architecture were explored as a photoanode in dye-sensitized solar cells, and their photovoltaic performance was compared with that of branch-free ZnO nanorods photoanodes. The highly branched network and large pores of the jacks-like ZnO nanorods electrodes enhances the charge transport, and electrolyte penetration. Thus, the jacks-like ZnO nanorods DSSCs render a higher conversion efficiency of η = 1.82% (V_oc = 0.59 V, J_sc = 5.52 mA cm⁻²) than that of the branch-free ZnO nanorods electrodes (η = 1.08%, V_oc = 0.49 V, J_sc = 4.02 mA cm⁻²). The incident photon-to-current conversion efficiency measurements reveal that the jacks-like ZnO nanorods DSSCs exhibit higher internal quantum efficiency (∼59.1%) than do the branch-free ZnO nanorods DSSC (∼52.5%). The charge transfer resistances at the ZnO/dye/electrolyte interfaces investigated using electrochemical impedance spectroscopy showed that the jacks-like ZnO nanorods DSSC had high charge transfer resistance and a slightly longer electron lifetime, thus improving the solar-cell performance.     

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.     

A mild solvothermal route to α-Fe2O3 nanoparticles

A mild solvothermal route has been developed to synthesize α-Fe₂O₃ nanoparticles using Fe(NO₃)₃ as a starting material. The results from XRD and TEM indicate the α-Fe₂O₃ powders possess a rhombohedrally centered hexagonal structure, and the size of particles from alcohothermal method at 160 °C is about 50-100 nm.     

Sonochemical preparation and characterization of SrZrxTi1−xO3/CdS composites

CdS nanoparticles coating SrZr_xTi_1−xO₃ (x=0.27) microparticles were obtained by sonochemical reaction, and the as-prepared composites products were characterized by TEM, XRD, FT-IR and other techniques and the fabrication mechanism was also discussed. Moreover, the photocatalystic properties of the final products were investigated by degradation of methylene blue. By coating CdS nanoparticles, the absorption of the UV-Vis spectrum of SrZr_xTi_1−xO₃ red-shifted, but the emission fluorescence spectrum blue-shifted. Adjusting the reactant concentration can control the thickness of the CdS layer.     

A novel synthetic route to prepare cubic BN nanorods

Cubic boron nitride nanorods were prepared at 450°C by a low pressure benzene thermal synthesis method using BCl₃ and Li₃N as the reactants. The nanorods with various lengths and diameters were observed by transmission electron microscopy. The analysis of X-ray diffraction pattern and electron diffraction pattern revealed that the nanorods are cBN with a lattice constant of 3.62 Å. The Fourier transformation infrared spectra showed that the dominant phase is cBN, and the B:N ratio of 1.15:1 can be obtained from the X-ray photoelectron spectrum.     

Synthesis and optical properties of ZnS hollow spheres from single source precursor

A facile one-pot synthesis of ZnS hollow spheres has been carried out via a chemical transformation induced inside-out Ostwald ripening process from a single source precursor. The size and shell thickness of the ZnS hollow spheres can be controlled by adjusting the reaction temperature and reaction time, respectively. Photoluminescence spectra show a dominant emission peak at 470 nm accompanied by several weaker peaks. UV-vis measurement reveals that the obtained ZnS hollow spheres exhibit “hollow effect”. The formation process of ZnS hollow spheres has been discussed.     

Photoluminescence of nanocrystalline SrMgF4 prepared by a solution chemical route

SrMgF₄ was prepared by precipitation in aqueous solution. Alkaline earth metal acetates and ammonium fluoride were used as precursors. After drying and annealing the samples at different temperatures and times, single phase SrMgF₄ was obtained. By varying the annealing conditions, the mean crystallite size could be adjusted. Furthermore, the thermally treated samples displayed UV-excited intensive broad band luminescence in the visible region. The emissions colour and intensity can be adjusted by the tempering conditions. X-Ray diffraction, TEM-microscopy, fluorescence and IR-spectroscopy were used for analysis.     

Growth of PbS nanopyramidal particulate films for potential applications in quantum-dot photovoltaics and nanoantennas

We report a simple interfacial process called the liquid-liquid interface reaction technique (LLIRT) that leads to the formation of nanosized PbS particulate films with hitherto unreported pyramidal morphology. The resultant PbS films were characterized by transmission electron microscopy (TEM) with selected area electron diffraction (SAED), X-ray diffractometery (XRD), atomic force microscopy (AFM), near field scanning optical microscopy (NSOM) and UV-vis spectroscopy. The pyramidal morphology is speculated to originate from the preferred orientation of the 2 2 0 plane of cubic PbS. Our nanopyramidal PbS particulate films display remarkably sharp excitonic peak centered around 656 nm that accounts for a band gap of 1.8 eV suggesting, in turn, their potential application in QD photovoltaics. Interestingly, the feasibility of such nanopyramids to potentially act as nanoantennas (as revealed by the NSOM) is also suggested.     

Zinc oxide micro- and nanoparticles: Synthesis, structure and optical properties

Zinc oxide (ZnO) spherical nanoparticles (SNPs) and bitter-melon-like (BML) microparticles were synthesized by a hydrothermal route using a zinc (Zn) plate as a source and substrate at various synthesis conditions. The structural analysis confirmed the formation of ZnO with hexagonal wurtzite phase on the hexagonal Zn substrate with growth of the ZnO microparticles along the [1 0 1] direction. The UV-vis absorption spectra of the ZnO microparticles indicated absorption peaks in the UV region which can be attributed to the band gap of ZnO. The room temperature photoluminescence (PL) of the ZnO microparticles exhibited a broad emission band, which is fitted with four Gaussian peaks and were assigned to transitions involving free excitons and various defect centers. The growth model for the formation of ZnO micro- and nanoparticles is presented.     

Grain growth and microstructural evolution of yttrium aluminum garnet nanocrystallites during calcination process

An yttrium aluminum garnet (YAG) precursor precipitate was synthesized by urea method using yttria (Y₂O₃) and aluminum nitrate (Al(NO₃)₃·9H₂O) as raw materials. The fresh wet precipitate was dried by supercritical carbon dioxide (CO₂) fluid and the resulting powder was calcined at temperatures from 600 to 1600 °C. Crystallization of YAG was detected at 800 °C, and completed at 900 °C. HRTEM images of the YAG product obtained above 900 °C revealed crystallographically specific oriented attachment along the [1 1 2] direction. Based on the observation of the particle morphology a possible growth mechanism of YAG nanoparticles was presented. The fast increase on the average crystallite size of YAG at temperatures from 900 to 1300 °C is attributed to the crystallographically specific oriented attachment growth process. As the growth process proceeds at higher temperatures, oriented attachment based growth becomes less important because of the increase on particle size, and the self-integration assisted by the Ostwald ripening becomes dominant.     

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.     

A study of size dependent structure, morphology and luminescence behavior of CdS films on Si substrate

Size tunable cadmium sulfide (CdS) films deposited by a dip coating technique on silicon (100) and indium tin oxide/glass substrates have been characterized using X-ray diffraction, X-ray reflectivity, transmission electron microscopy, atomic force microscopy and photoluminescence spectroscopy. The structural characterization indicated growth of an oriented phase of cadmium sulfide. Transmission electron microscopy used to calculate the particle size indicated narrow size dispersion. The tendency of nanocrystalline CdS films to form ordered clusters of CdS quantum dots on silicon (100) substrate has been revealed by morphological studies using atomic force microscopy. The photoluminescence emission spectroscopy of the cadmium sulfide films has also been investigated. It is shown that the nanocrystalline CdS exhibit intense photoluminescence as compared to the large grained polycrystalline CdS films. The effect of quantum confinement also manifested as a blue shift of photoluminescence emission. It is shown that the observed photoluminescence behavior of CdS is substantially enhanced when the nanocrystallites are assembled on silicon (100) substrate.     

A novel solution-phase route for the synthesis of crystalline silver nanowires

A unique solution-phase route was devised to synthesize crystal Ag nanowires with high aspect-ratio (8-10 nm in diameter and length up to 10 μm) by the reduction of AgNO₃ with Vitamin C in SDS/ethanol solution. The resultant nanoproducts were characterized by transmission electron microscope (TEM), X-ray diffraction (XRD) and electron diffraction (ED). A soft template mechanism was put forward to interpret the formation of metal Ag nanowires.     

Role of glycine-to-nitrate ratio in influencing the powder characteristics of La(Ca)CrO3

Ultrafine La(Ca)CrO₃ (LCC) powders were prepared through glycine-nitrate gel combustion process. The effect of glycine-to-nitrate ratio on batch size, particle size, nature of agglomeration and densification was studied. As-prepared powders when calcined at 700 °C resulted in LCC along with a small amount of CaCrO₄. The primary particle size obtained in case of stoichiometric and fuel-rich precursor was found to be 25–60 and 60–180 nm, respectively. It was found that the final powder had softer agglomerates with increasing glycine-to-nitrate ratio, which in turn improved the sintered density. The powder obtained through fuel-rich precursor could be sintered to ≈98% of its theoretical density at 1300 °C without applying any ball milling operation.