Analysis of lead molybdate and lead tungstate synthesized by a sonochemical method

Lead molybdate and lead tungstate nanoparticles were successfully synthesized by a sonochemical method for 1 h. XRD patterns showed the body-centered tetragonal structures of PbMoO₄ and PbWO₄, and were in accordance with those of the simulation and JCPDS software. Calculated lattice parameters are a = b = 5.4233 Å and c = 12.1253 Å for PbMoO₄, and 5.4570 Å and 12.0995 Å for PbWO₄. They are in accordance with those of the corresponding JCPDS software. TEM images show that the particles were 29.09 ± 5.22 nm and 21.05 ± 2.68 nm for PbMoO₄ and PbWO₄, respectively. Raman and FTIR vibrations were investigated to identify a definite existence of the structures.     

Phase evolution and morphology of nanocrystalline BaCe0.9Er0.1O3−δ proton conducting oxide synthesised by a novel modified solution combustion route

Pure BaCeO₃ and 10 mol% Er₂O₃ doped BaCeO₃ (BCE) was synthesised by a novel modified solution combustion synthesis (MCS) route wherein the pH of the precursor solution was varied and the phase formation and morphology were compared with those obtained in conventional solution combustion synthesis (SCS). X-ray diffraction (XRD) studies confirmed the presence of the undesirable BaCO₃ phase in the calcined powders prepared using SCS route whereas the powders synthesised with the modified (MCS) route exhibited a single perovskite phase after calcination. Variation in the pH of the precursor solution resulted in a morphology change from a mix of irregular and globular at pH 4 to more spherical at pH 6 and 8. Fourier transform infrared spectroscopy (FT-IR) studies revealed that calcination time has more pronounced effect on phase formation than calcination temperature. A calcination time of 10 h at 1000 °C resulted in negligible amount of BaCO₃. Such prolonged calcination treatment resulted in substantial grain growth in the SCS sample while the MCS samples were still in the nanocrystalline form. Absence of the ceria peak (464 cm^–1) in the Raman spectra confirmed the presence of a single perovskite BaCeO₃ phase in the sintered pellets as well.     

Synthesis of high quality and monodisperse CdS:Mn/ZnS and CdS:Mn/CdS core–shell nanoparticles

CdS:Mn²⁺/ZnS and CdS:Mn²⁺/CdS core–shell nanoparticles were synthesized in aqueous medium via chemical precipitation method in an ambient atmosphere. Polyvinylpyrrolidone (PVP) was used as a capping agent. The effect of the shell (ZnS and CdS) thickness on CdS:Mn²⁺ nanoparticles was investigated. Inorganically passivated core/shell nanocrystals having a core (CdS:Mn²⁺) diameter of 4 nm and a ZnS-shell thickness of ∼0.5 nm exhibited improved PL intensity. Optimum concentration of doping ions (Mn²⁺) was selected through optical study. For all the core–shell samples two emission peaks were observed, the first one is band edge emission in the lower wavelength side due to energy transfer to the Mn²⁺ ions in the crystal lattice; the second emission is characteristic peak of Mn²⁺ ions (⁴T₁ → ⁶A₁). The XRD, TEM and PL results showed that the synthesized core–shell particles were of high quality and monodisperse.     

Copper-containing polyvinyl alcohol composite systems: Preparation,characterization and biological activity

The present investigation reports, the complex formation of Cu(II) with polyvinyl alcohol (PVA) and the synthesis of PVA-stabilized Cu₂O particles. This PVA–Cu₂O composite has been prepared via chemical reduction method using PVA–Cu(II) complex as precursor. At first, Cu(II) ions were stabilized in PVA matrix via complex formation with OH groups; subsequently, this PVA–Cu(II) macromolecular complex as precursor reacted with ascorbic acid as reducing agent at pH=12 to prepare PVA–Cu₂O composite. The products were characterized by FTIR, XRD, FE-SEM, HRTEM, Visible Spectroscopy and atomic absorption. In the following, the antibacterial properties of as-prepared composites were examined against Gram-positive (Bacillus thuringiensis) and Gram-negative bacteria (Escherichia coli), and the results showed excellent antibacterial activity of these materials.     

Engineering birnessite-type MnO2 nanosheets on fiberglass for pH-dependent degradation of methylene blue

We construct hierarchical MnO₂ nanosheets @ fiberglass nanostructures via one-pot hydrothermal method without any surfactants. The morphology and structure of MnO₂-modified fiberglass composites are examined by focus ion beam scanning electron microscopy (FIB/SEM), X-Ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The birnessite-type MnO₂ nanosheets are observed to grow vertically on the surface of fiberglass. Furthermore, the birnessite-type MnO₂-fiberglass composites exhibit good ability for degradation of methylene blue (MB) in different pH levels. In neutral solution (pH 6.5–7.0), it achieves a high removal rate of 96.1% (2 h, at 60 °C) in the presence of H₂O₂; and in acidic environment (pH 1.5), 96.8% of MB solution (20 mg/L, 100 mL) is decomposed by oxidation within only 5 min. In principles, the rational design of MnO₂ nanosheets-decorated fiberglass architectures demonstrated the suitability of the low-cost MnO₂-modified fiberglass nanostructure for water treatment.     

Synthesis of porous hollow silica spheres using polystyrene-methyl acrylic acid latex template at different temperatures

Porous hollow silica spheres were prepared by using polystyrene-methyl acrylic acid latex as a template and cetyltrimethylammonium bromide as a wall structure-directing agent starting from tetraethoxysilane. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), FT-infrared spectroscopy (FT-IR) and nitrogen adsorption/desorption were used to characterize the hollow silica spheres. When silica-coated latex composites were prepared at room temperature, hollow silica spheres with micropores in the walls were formed after removing the latex templates by calcination. When silica-coated latex composites were aged at a higher temperature of 150 °C, intact mesoporous hollow silica spheres were formed after calcination treatment.     

Intercalation of sulfonated melamine formaldehyde polycondensates into a hydrocalumite LDH structure

A series of sulfonated melamine formaldehyde (SMF) polycondensates possessing different anionic charge amounts and molecular weights was synthesized and incorporated into a hydrocalumite type layered double hydroxide structure using the rehydration method. For this purpose, tricalcium aluminate was dispersed in water and hydrated in the presence of these polymers. Defined inorganic–organic hybrid materials were obtained as reaction products. All SMF polymers tested intercalated readily into the hydrocalumite structure, independent of their different molecular weights (chain lengths) and anionic charge amounts. X-ray diffraction revealed typical patterns for weakly ordered, highly polymer loaded LDH materials which was confirmed via elemental analysis and thermogravimetry. IR spectroscopy suggests that the SMF polymers are interleaved between the [Ca₂Al(OH)₆]⁺ main sheets via electrostatic interaction, and that no chemical bond between the host matrix and the guest anion is formed. The SMF polymers well ensconced within the LDH structure exhibit significantly slower thermal degradation.     

Synthesis and characterization of CdS nanocrystals in Maleic anhydride–Octene-1–Vinylbutyl Ether terpolymer matrix

A Maleic anhydride–Octene-1–Vinylbutyl Ether terpolymer was synthesized via the radical terpolymerization method in order to prepare a new matrix for CdS nanocrystal synthesis. CdS nanocrystals were synthesized through the reaction of thiourea with cadmium chloride. The synthesized terpolymer/CdS nanocrystal composites were characterized by several methods. Energy Dispersive X-ray analysis, Raman spectroscopy and powder X-ray diffraction methods. The room temperature UV–visible absorption spectra show a shift of the absorption edge towards higher energies. The band gap of the CdS nanocomposite is bigger than that of bulk CdS. Raman spectrum exhibits characteristic peaks of CdS. Images of the nanocomposite obtained with Atomic Force Microscopy and Transmission Electron Microscopy are the evidences of CdS nanocrystal formation in the terpolymer. Thermal investigation shows that the nanocomposite is more thermostable than the terpolymer which could be useful for application in thermo aggressive medium.     

Polyol-assisted synthesis of TiO2 nanoparticles in a semi-aqueous solvent

TiO₂ (anatase and rutile) nanoparticles with an average crystallite size of 20-40 nm have been prepared at room temperature by polyol-mediated synthesis technique in a semi-aqueous solvent medium using titanium iso-propoxide as the titanium source, acetone as the oil phase and ethylene glycol as the stabilizer. Phase and microstructure of the resultant materials have been characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy and Raman spectroscopy. Photocatalytic degradation of acetaldehyde using TiO₂ nanoparticles was investigated by gas-chromatography technique.     

Drastic change in shape of tetragonal TeO2 nanowires and their application to transparent chemical gas sensors

We have synthesized one-dimensional structures of tellurium dioxide (TeO₂) by heating of tellurium powders. Their morphology was drastically changed as the growth temperature increased in the range of 400-500 °C, in which high-temperature process facilitated the thickening of the stem nanowires, as well as the growth of secondary branches on the stems. The obtained TeO₂ products were crystalline with tetragonal structure. The TeO₂ nanowire film exhibited a high transmission rate of about 73%. We have investigated the NO₂ sensing properties of the as-fabricated TeO₂ nanowires, in which a linear relationship between sensitivity and the NO₂ gas concentration was observed. Thus, the TeO₂ nanowires demonstrated their potential application to transparent chemical sensors.     

Synthesis of quasi-1D cuprous oxide nanostructure and its structural characterizations

A wealth of superfine polycrystalline cuprous oxide (Cu₂O) nanowires have been synthesized with hydrazine hydrated (N₂H₄·H₂O), act as the reducing agent, and Cu(OH)₂ nanowires, act as a soft template and surfactant, at room temperature. Two methods were employed for the synthesis of these nanowires, i.e. with and without capping agent (polyethylene glycol Mw 8000). Techniques of powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) pattern, electron diffraction X-ray (EDX) spectroscopy, and UV-visible (UV-vis) spectroscopy have been used to characterize the morphology, structure, crystallinity, purity, and composition of nanowires. The average diameters of Cu₂O nanowires, prepared with and without capping agent, were observed to be 8-10 and 12-15 nm and lengths of several microns, respectively. It is found that capping agent (PEG) confines the dimensions of synthesized nanowires. In addition, the observed optical band gap of products show blue-shift effect compared to the bulk Cu₂O (E_g=2.17 eV), which ascribe it as a promising material for the conversion between solar energy and electrical or chemical energy.     

Catalyst-free synthesis of GeO2 nanowires using the thermal heating of Ge powders

Germanium dioxide (GeO₂) nanowires have been synthesized by means of the simple evaporation of solid Ge powders, without using metal catalysts. The nanowires, with a diameter of about 90–200 nm, were characterized using scanning electron microscopy (SEM), X-ray diffractometry (XRD), and transmission electron microscopy (TEM). The obtained GeO₂ nanowires were crystalline with a hexagonal structure. The growth mechanism was discussed with respect to the vapor–solid process. The photoluminescence measurement revealed two emission peaks at about 2.45 eV and 2.91 eV at room temperature, opening up a route to potential applications in future optoelectronic nanodevices. Raman measurement of as-synthesized GeO₂ nanowires was made at room temperature.     

Effect of growth temperature on the ZnO nanowires prepared by thermal heating of Zn powders

ZnO nanowires have been synthesized by heating Zn powders under nitrogen (N₂) gas atmosphere. The influence of the growth temperature on the morphology, structure, and photoluminescence (PL) properties of ZnO nanowires has been investigated. At the higher-temperature growth process, thinner nanowires have been obtained. Interestingly, it is observed that the variation of growth temperature has significantly affected the photoluminescence spectra of the ZnO nanowires, showing an enhancement in the relative intensity of the green to UV emission bands with the increase of the growth temperature. In addition, the oxygen sensing properties of the as-synthesized ZnO nanowires were tested.     

Characteristics of SiOx nanowires synthesized via the thermal heating of Cu-coated Si substrates

We have demonstrated the growth of SiO_x nanowires by the simple heating of the Cu-coated Si substrates. We have applied X-ray diffraction, scanning electron microscopy and transmission electron microscopy techniques to characterize the structure of the samples. The as-synthesized SiO_x nanowires had amorphous structures with diameters in the range of 20–80 nm. The thickness of the Cu layer affected the resultant sample morphology, favoring the nanowire formation at smaller thickness. Photoluminescence spectra of the nanowires exhibited blue emission. We have proposed the possible growth mechanism.     

Preparation of silver nanowires coated with TiO2 using chemical binder and their applications as photoanodes in dye sensitized solar cell

In this study, the core–shell structured Ag@TiO₂ wire was prepared for application to dye-sensitized solar cell (DSSC). The Ag nanowire, having an excellent electrical conductivity, was synthesized by using the facile microwave-assisted polyol reduction process. The diameter and length of Ag wires were 40–50 nm and 20–30 μm, respectively, and the face-centered cubic silver crystal structure was obtained. In the presence of 2-mercaptoethanol as a chemical binder, the entire surface of Ag wire was coated with the TiO₂ shell, which has thickness of 20 nm, through solvothermal method. The crystalline structure of TiO₂ shell was the anatase phase possessing an advantage to achieve the high efficiency in DSSC. The core–shell structured Ag@TiO₂ wire exhibited the high thermal stability. The high conversion efficiency (5.56%) in fabricated device with Ag@TiO₂ electrode, which is about 10% higher than reference cell, was achieved by enhancement of short-current density (J_sc) value. The core–shell structured Ag@TiO₂ wire could effectively reduce the charge recombination through the contribution to electron shortcut for improvement in the electron transfer rate and lifetime.     

Synthesis, characterization and antibacterial action of hollow titania spheres

Hollow titania spheres were synthesized using the cationic polystyrene lattices which were prepared by polymerization in suspension of styrene using 2,2′-azobis (2-methylpropionamidine) dihydrochloride (AMPA) as an initiator. These cationic colloidal particles were dispersed in absolute ethanol in the presence of poly(vinylpyrrolidone) (PVP), solution of sodium chloride (NaCl) and mixed with ethanolic solutions of titanium tetraisopropoxide (TTIP). Subsequently, hollow spheres of titania compounds were obtained by calcinations of the so-coated polystyrene lattices at elevated temperature in air. The hollow titania spheres were characterized with scanning electron microscopy (SEM), FT-infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Moreover, antibacterial action of illuminated hollow titania spheres on pure culture of Escherichia coli (E. coli) was studied. A decrease of E. coli concentration was observed after illumination of bacteria in the presence of hollow titania spheres.     

Growth of single wall carbon nanotubes using PECVD technique: An efficient chemiresistor gas sensor

In this work, the uniform and vertically aligned single wall carbon nanotubes (SWCNTs) have been grown on Iron (Fe) deposited Silicon (Si) substrate by plasma enhanced chemical vapor deposition (PECVD) technique at very low temperature of 550 °C. The as-grown samples of SWCNTS were characterized by field emission scanning electron microscope (FESEM), high resolution transmission electron microscope (HRTEM) and Raman spectrometer. SWCNT based chemiresistor gas sensing device was fabricated by making the proper gold contacts on the as-grown SWCNTs. The electrical conductance and sensor response of grown SWCNTs have been investigated. The fabricated SWCNT sensor was exposed to ammonia (NH₃) gas at 200 ppm in a self assembled apparatus. The sensor response was measured at room temperature which was discussed in terms of adsorption of NH₃ gas molecules on the surface of SWCNTs. The achieved results are used to develope a miniaturized gas sensor device for monitoring and control of environment pollutants.     

Shape-controlled synthesis of nickel phosphide nanocrystals and their application as hydrogen evolution reaction catalyst

Monodisperse nickel phosphide (Ni₂P) nanorods and nanoparticles were synthesized by one step solution-phase route, in which the mixture of trioctylphosphine oxide (TOPO) and trioctylphosphine (TOP) was used as solvent, capping agent and phosphor source. The morphologies of the Ni₂P nanocrystals were controlled simply by varying the dropping rate of metal source. The as-prepared Pt-free Ni₂P nanocrystals exhibit the enhanced electrocatalytic activity toward hydrogen evolution reaction (HER) compared to pure commercial Ni nanoparticles. Therefore, the obtained Ni₂P nanocrystals appear to be promising non precious metal electrocatalysts for HER.     

A novel strategy to synthesize cobalt hydroxide and Co3O4 nanowires

Cobalt hydroxide ultra fine nanowires were prepared by a facile hydrothermal route using hydrogen peroxide. This method provides a simple, low cost, and large-scale route to produce β-cobalt hydroxide nanowires with an average diameter of 5 nm and a length of ca. 10 μm, which show a predominant well-crystalline hexagonal brucite-like phase. Their thermal decomposition produced highly uniform nanowires of cobalt oxide (Co₃O₄) under temperature 500 °C in the presence of oxygen gas. The produced cobalt oxide was characterized by X-ray diffraction, transmission electronic microscopy, and selected-area electron diffraction. The results indicated that cobalt oxide nanowires with an average diameter of 10 nm and a length of ca. 600 nm have been formed, which show a predominant well-crystalline cubic face-centered like phase.     

Preparation of graphene encapsulated copper nanoparticles from CuCl2-GIC

Graphene encapsulated metallic copper nanoparticle composite was prepared by reduction of stage-2 CuCl₂-graphite intercalation compounds, using both metallic potassium and potassium borohydride/ethylenediamine matrix as reducing reagents. X-ray diffraction, high-resolution transmission electron microscopy and Raman spectroscopy were employed to characterize the reduction products. The results show that the copper nanoparticles in the graphite matrix are 30 to 70 nm in size. The copper concentration in the reduction product is experimental-condition dependant. A severe structure disorder of graphitic carbon occurs during the reduction procedure. The formation procedure of copper particles in the graphene sheets is discussed briefly.