CuBi2O4 single crystal nanorods prepared by hydrothermal method: Growth mechanism and optical properties

The synthesis of copper bismuth oxide (CuBi₂O₄) nanorods with single crystal structure by hydrothermal method is first reported here. The prepared CuBi₂O₄ nanorods are characterized by X-ray diffractometer, scanning electron microscopy, transmission electron microscopy (TEM) and high resolution TEM. It is found that the concentration of reagent cupric acetate has strong effect on the purity and microstructure of the prepared samples. The growth process is investigated in detail. It is proposed that the nanorods are evolved from spherical particles with oriented attachment mechanism followed by dissolution-splitting process. The optical properties of the samples are detected by UV-vis spectrometer and photoluminescence spectrometer and exhibit strong dependence on surface defect states and microstructure feature, which is mainly determined by preparation conditions.     

Synthesis and optical properties of (Gd1−x,Eux)2O2SO4 nano-phosphors by a novel co-precipitation method

(Gd_1−x,Eu_x)₂O₂SO₄ nano-phosphors were synthesized by a novel co-precipitation method from commercially available Gd₂O₃, Eu₂O₃, H₂SO₄ and NaOH starting materials. Composition of the precursor is greatly influenced by the molar ratio of NaOH to (Gd_1−x,Eu_x)₂(SO₄)₃ (the m value), and the optimal m value was found to be 4. Fourier transform infrared spectrum (FT-IR) and thermal analysis show that the precursor (m = 4) can be transformed into pure (Gd_1−x,Eu_x)₂O₂SO₄ nano-phosphor by calcining at 900 °C for 2 h in air. Transmission electron microscope (TEM) observation shows that the Gd₂O₂SO₄ phosphor particles (m = 4) are quasi-spherical in shape and well dispersed, with a mean particle size of about 30-50 nm. Photoluminescence (PL) spectroscopy reveals that the strongest emission peak is located at 617 nm under 271 nm light excitation, which corresponds to the ⁵D₀ → ⁷F₂ transition of Eu³⁺ ions. The quenching concentration of Eu³⁺ ions is 10 mol% and the concentration quenching mechanism is exchange interaction among the Eu³⁺ ions. Decay study reveals that the ⁵D₀ → ⁷F₂ transition of Eu³⁺ ions has a single exponential decay behavior.     

Preparation and super-hydrophilic properties of TiO2/SnO2 composite thin films

SnO₂-TiO₂ composite thin films were fabricated on soda-lime glass with sol-gel technology. By measuring the contact angle of the film surface and the degradation of methyl orange, we studied the influence of SnO₂ doping concentration, heat-treatment temperature and film thickness on the super-hydrophilicity and photocatalytic activity of the composite films. The results indicate that the doping of SnO₂ into TiO₂ can improve their hydrophilicity and photocatalytic activity, and the composite film with 1-5 mol% SnO₂ and heat-treated at 450°C is of super-hydrophilicity. The optimal SnO₂ concentration for the photocatalytic activity is 10 mol% and larger film thickness is helpful to reduce the contact angle of the composite films.     

The preparation,characterization and optical properties of Cd2V2O7 and CdCO3 compounds

Cadmium vanadium oxides (Cd₂V₂O₇) and Cadmium carbonates (CdCO₃) were synthesized via a facile hydrothermal method. X-ray diffraction (XRD), Raman spectroscopy, infrared spectrometer (IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) were employed to characterize the structure, morphology and chemical state of the samples, respectively. The photoluminescence (PL) properties of the as-synthesized Cd₂V₂O₇ and CdCO₃ were measured at room temperature using an excitation wavelength of 325 nm. The Cd₂V₂O₇ shows two visible light emission centers located at 589 and 637 nm, which are supposed to be relevant to local defects in Cd₂V₂O₇. The CdCO₃ shows three emission centers located at 408, 530 and 708 nm, which are supposed to be relevant to the electron transition from the conduction band to valence band and defect related energy level.     

The preparation of TiO2/SiO2 composite hollow spheres with hydrophobic inner surface and their application in controlled release

The TiO₂/SiO₂ composite hollow spheres (CHSs) with hydrophobic inner surface have been successfully synthesized by using carboxyl-functionalized polystyrene spheres as templates. The inner titania shell was selectively modified with stearic acid (SA). The morphologies, structures, drug loading amounts and release rates were characterized and investigated by SEM, TEM, XRD, N₂ adsorption-desorption isotherms, FT-IR, TG and HPLC analysis. Due to the hydrophobic interaction, the modified inner surface slowdown the release of the hydrophobic drug into the aqueous environment. The SA modified CHSs displayed higher drug loading amounts as well as lower release rates than that of unmodified spheres. The studies demonstrate that composite hollow spheres are promising for the multifunctional controlled release.     

Large-scale fabrication of H2(H2O)Nb2O6 and Nb2O5 hollow microspheres

Hollow micro-sized H₂(H₂O)Nb₂O₆ spheres constructed by nanocrystallites have been successfully synthesized via a bubble-template assisted hydrothermal process. In the reaction process, H₂O₂ acts as a bubble generator and plays a key role in the formation of the hollow structure. An in situ bubble-template mechanism has been proposed for the possible formation of the hollow structure. The spherelike assemblies of these H₂(H₂O)Nb₂O₆ nanoparticles have been transformed into their corresponding pseudohexagonal phase Nb₂O₅ through a moderate annealing dehydration process without destroying the hierarchical structure. Optical properties of the as-prepared hollow spheres were investigated. It is exciting that the absorption edge of the hollow Nb₂O₅ microspheres shifts about 18 nm to the violet compared with bulk powders in the UV/vis spectra, indicating its superior optical properties.     

Magnetic properties and photoabsorption of the Mn-doped CeO2 nanorods

Mn-doped CeO₂ nanorods have been prepared from CeO₂ particles through a facile composite-hydroxide-mediated (CHM) approach. The analysis from X-ray photoelectron spectroscopy indicates that the manganese doped in CeO₂ exists as Mn²⁺. The magnetic measurement of the Mn-doped CeO₂ nanorods exhibits an enhanced ferromagnetic property at room temperature with a remanence magnetization (Mr) of 1.36 × 10⁻³ emu/g and coercivity (Hc) of 22 Oe. Comparative UV-visible spectra reveal the shift of the absorption peak of the CeO₂ from ultraviolet region to visible light region after being doped with Mn. The room temperature ferromagnetic properties and light absorption of the Mn-doped CeO₂ nanorods would have potential applications in photocatalysis and building of photovoltaic devices.     

Facile fabrication of SiO2/Al2O3 composite microspheres with a simple electrostatic attraction strategy

SiO₂/Al₂O₃ composite microspheres with SiO₂ core/Al₂O₃ shell structure and high surface area were prepared by depositing Al₂O₃ colloid particles on the surface of monodispersed microporous silica microspheres using a simple electrostatic attraction and heterogeneous nucleation strategy, and then calcined at 600 °C for 4 h. The prepared products were characterized with differential thermal analysis and thermogravimetric analysis (DTA/TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption and X-ray photoelectron spectroscopy (XPS). It was found that uniform alumina coating could be deposited on the surface of silica microspheres by adjusting the pH values of the reaction solution to an optimal pH value of about 6.0. The specific surface area and pore volume of the SiO₂/Al₂O₃ composite microspheres calcined at 600 °C were 653 m² g⁻¹ and 0.34 ml g⁻¹, respectively.     

Microstructure and optical absorption of FeS2 films formed by sulfurizing precursive iron of various crystallite scales

Precursive iron films with various crystallite scales were prepared by sputtering on substrates heated at different temperatures. The iron films were annealed in sulfur vapor at 673 K to form pyrite films. The structural and optical characters were determined. High substrate temperatures produce large crystallites in the precursive iron films. The pyrite films are composed of a surface layer with coarse columnar grains and a bottom layer with fine equiaxed grains. Sufficient formation and growth of iron grains result in improved crystallinity of the pyrite films. The optical absorption characteristics depend mainly on the crystallinity of the pyrite films or the crystallizing status of the precursive iron films. The optical absorption coefficient of the pyrite films decreases with the increase of iron grain diameter from 12 to 39 nm. The band gap of the pyrite films increases with the increase of iron grain diameter from 12 to 53 nm.     

The optical properties of Bi3.25La0.75Ti3O12 thin films with different thickness prepared by chemical solution deposition

Bi_3.25La_0.75Ti₃O₁₂(BiLT) thin films with different thickness were successfully deposited onto fused quartz by chemical solution deposition. X-ray diffraction analysis shows that BiLT thin films are polycrystalline with (0 0 2)-preferred orientation. The dispersion of refractive indices of the BiLT thin films was investigated by the optical transmittance spectrum. The optical band gap energy was estimated from the graph of (hνα)² versus hν. The results show that the refractive index and band-gap energy of the BiLT thin films decrease with the films thickness.     

Reversible transformations of silver oxide and metallic silver nanoparticles inside SiO2 films

Reversible transformation of silver oxide and metallic nanoparticles inside a relatively porous silica film has been established. Annealing of Ag-doped films in oxidizing (air) atmosphere at 450 °C yielded colorless films containing AgO_x. These films were turned yellow when heated in H₂-N₂ (reducing atmosphere) due to the formation of Ag nanoparticles. This yellow coloration (due to nano Ag⁰) and bleaching (conversion of Ag⁰ → Ag⁺) are reversible. Optical and photoluminescence spectra are well consistent with this coloration and bleaching. The soaking test of the air-annealed film in Na₂S₂O₃ solution supports the presence of Ag⁺. Grazing incidence X-ray diffraction and transmission electron microscopy studies reveal the formation of Ag-oxides and Ag nanoparticles in the oxidized and reduced films, respectively.     

Electrodeposition of As2Se3 thin films

Semiconducting As₂Se₃ thin films have been prepared from an aqueous bath at room temperature onto stainless steel and fluorine-doped tin oxide (F.T.O.)-coated glass substrates using an electrodeposition technique. It has been found that As₂O₃ and SeO₂ in the volumetric proportion as 4:6 and their equimolar solutions of 0.075 M concentration forms good quality films of As₂Se₃. The films are annealed in a nitrogen atmosphere at temperature of 200 °C for 2 h. The films are characterised by scanning electron microscopy, X-ray diffraction and optical absorption techniques. Studies reveal that asdeposited and annealed thin films are polycrystalline in nature. The optical band gap has been found to be 2.15 eV for the above-mentioned composition and concentration of the film.     

Structural characterization and novel optical properties of defect chalcopyrite ZnGa2Te4 thin films

Stoichiometric thin film samples of the ternary ZnGa₂Te₄ defect chalcopyrite compound were prepared and characterized by X-ray diffraction technique. The elemental chemical composition of the prepared bulk material as well as of the as-deposited film was determined by energy-dispersive X-ray spectrometry. ZnGa₂Te₄ thin films were deposited, by conventional thermal evaporation technique onto highly cleaned glass substrates. The X-ray and electron diffraction studies revealed that the as-deposited and the annealed ZnGa₂Te₄ films at annealing temperature t_a ≤ 548 K are amorphous, while those annealed at t_a ≥ 573 K (for 1 h), are polycrystalline. The optical properties of the as-deposited films have been investigated for the first time at normal incidence in the spectral range from 500 to 2500 nm. The refractive index dispersion in the transmission and low absorption region is adequately described by the Wemple–DiDomenico single oscillator model, whereby, the values of the oscillator parameters have been calculated. The analysis of the optical absorption coefficient revealed an in-direct optical transition with energy of 1.33 eV for the as-deposited sample. This work suggested that ZnGa₂Te₄ is a good candidate in solar cell devices as an absorbing layer.     

Preparation, characterization and microwave absorption properties of polyaniline/Co0.5Zn0.5Fe2O4 nanocomposite

The polyaniline (PAni)/Co_0.5Zn_0.5Fe₂O₄ nanocomposite was prepared by an in situ polymerization in an aqueous solution. The products were characterized by Fourier transform infrared (FT-IR) spectrometer, ultraviolet-visible (UV-vis) spectrometer, X-ray diffraction (XRD) and transmission electron microscope (TEM). The average particle size of the PAni/Co_0.5Zn_0.5Fe₂O₄ was estimated to be about 70 nm by TEM. The reflection loss (dB) of the nanocomposite was measured at different microwave frequencies in X-band (8.2-12.4 GHz), U-band (12.4-18 GHz) and K-band (18-26.5 GHz) by radar cross-section (RCS) method according to the national standard GJB-2038-94. The results showed the reflection loss of the PAni/Co_0.5Zn_0.5Fe₂O₄ nanocomposite was higher than that of the PAni. The maximum reflection loss of the PAni/Co_0.5Zn_0.5Fe₂O₄ nanocomposite was about −39.9 dB at 22.4 GHz with a bandwidth of 5 GHz (full frequency width at about a half of the peak response). In conclusion, this sample is a good microwave shielding and absorbing materials at higher frequency.     

Sub-2 nm SnO2 nanocrystals: A reduction/oxidation chemical reaction synthesis and optical properties

A simple reduction/oxidation chemical solution approach at room temperature has been developed to synthesize ultrafine SnO₂ nanocrystals, in which NaBH₄ is used as a reducing agent instead of mineralizers such as sodium hydroxide, ammonia, and alcohol. The morphology, structure, and optical property of the ultrafine SnO₂ nanocrystals have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD), differential scanning calorimetry and thermogravimetric analysis (DSC-TGA), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy. It is indicated that the uniform tetragonal ultrafine SnO₂ nanocrystals with the size below 2 nm have been fabricated at room temperature. The band gap of the ultrafine SnO₂ nanocrystals is about 4.1 eV, exhibiting 0.5 eV blue shift from that of the bulk SnO₂ (3.6 eV). Furthermore, the mechanism for the reduction/oxidation chemical reaction synthesis of the ultrafine SnO₂ nanocrystals has been preliminary presented.     

Materials properties of electrodeposited SnS0.5Se0.5 films and characterization of photoelectrochemical solar cells

Thin films of tin sulfoselenide (SnS_0.5Se_0.5) have been electrodeposited from an aqueous solution on tin oxide coated glass substrates by potentiostatic technique. XRD pattern of SnS_0.5Se_0.5 films showed polycrystalline nature and orthorhombic structure. The presence of Sn, S, and Se of the films were confirmed by XPS analysis. All films showed an indirect band gap. Surface morphological studies were carried out using Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) analyses. Mott-Schottky plots have been drawn (in the dark condition) to evaluate the semiconductor parameters which confirmed the p-type nature of the films. The photoelectrochemical behavior of the SnS_0.5Se_0.5 films was studied in the electrolyte containing 0.1 M (FeCl₂/FeCl₃) + 0.05 M H₂SO₄ and the results are reported.     

Cathodoluminescence of CaWO4 and SrWO4 thin films prepared by spray pyrolysis

Thin films of CaWO₄ and SrWO₄ were prepared on glass substrates by spray pyrolysis. The effects of preparation conditions and monovalent, bivalent and trivalent cation doping on cathodoluminescence (CL) properties of the films were studied. Polycrystalline CaWO₄ and SrWO₄ films formed a scheelite structure after being annealed above 300°C. They exhibited analogous cathodoluminescence consisting of a blue emission band at 447 nm and a blue-green emission band at 487 nm. The blue and blue-green emission intensities increased with substrate and annealing temperature. Annealing atmosphere and doping with Ag⁺, Pb²⁺ and La³⁺ did not influence the characteristics of the blue and blue-green emissions, whereas Eu³⁺ did. The results indicated both the blue and blue-green emissions originated from the WO₄²⁻ molecular complex. The luminance and efficiency for CaWO₄ film were 150 cd/m² and 0.7 lm/W at 5 kV and 57 μA/cm².     

Synthesis and characterization of ZnO/SiO2 core/shell nanocomposites and hollow SiO2 nanostructures

In this paper, we prepared the ZnO nanoparticles by a simple hydrothermal method and fabricated the ZnO/SiO₂ core/shell nanostructures through a sol-gel chemistry process successfully. The hollow SiO₂ nanostructures were obtained by selective removal of the ZnO cores. The structure, morphology and composition of the products were determined by the techniques of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). The results indicated that the ZnO nanoparticles were sphere-like shape with the average size of 60 nm and belonged to hexagonal wurtzite crystal structure. With the coating of SiO₂, the vibration modes of Si-O-Si and Si-OH were found. Furthermore, the measurement results of optical properties showed that spectra of bare ZnO nanoparticles and ZnO/SiO₂ core/shell nanocomposites exhibited similar emission features, including a blue emission peak and an orange emission band.     

Dopant induced variations in microstructure and optical properties of CeO2 nanoparticles

Nanocrystalline CeO₂ particles doped in the range of 0-20% of Ca²⁺, La³⁺, and Zr⁴⁺ have been prepared from hydrothermal synthesis of nitrate solutions at 200 °C and the influences of the dopants on microstructure and optical properties of the nanoparticles have been investigated. The unit cell parameter is found to be modified by −0.39, +0.83 and +0.16% for doping of 20% Zr⁴⁺, La³⁺, and Ca²⁺, respectively. For each batch prepared, nanoparticles with a narrow size distribution of 5-15 nm have been obtained. A high-resolution transmission electron microscopy investigation reveals that these particles are single crystals mostly having hexagonal, square or circular two-dimensional projections. UV-visible spectra of doped powders exhibit shift of the absorption edge and absorption peak with respect to those of the undoped CeO₂ particles and has been attributed to compensation of Ce³⁺ and decreasing crystallite size as result of doping.     

Hydrothermal synthesis and vacuum ultraviolet-excited luminescence properties of novel Dy-doped LaPO4 white light phosphors

Novel LaPO₄:Dy³⁺ white light phosphors with monoclinic system were successfully synthesized by hydrothermal method at 240 °C. The strong absorption at around 147 nm in excitation spectrum was assigned to the host absorption which suggested that the vacuum ultraviolet-excited energy was efficiently transferred from the host to the Dy³⁺ ion. The f-d transition of Dy³⁺ ion was observed locating at 182 nm. Under 147 nm excitation, La_1−xPO₄:xDy³⁺ phosphor exhibited two emission bands locating at 571 nm (yellow) and 478 nm (blue) which corresponded to the hypersensitive transitions ⁴F_9/2-⁶H_13/2 and ⁴F_9/2-⁶H_15/2. It was the two emission bands that lead to the white light.