Functionalized TiO2@ZrO2@Y2O3 ：Eu3＋ core-multishell microspheres and their photoluminescence properties

TiO2@ZrO2@Y2O3 ：Eu3＋ composite particles with a core-multishell structure were synthesized through the combination of a layer-by-layer （LBL） self-assembly method and a sol-gel process. The obtained sam- ples were characterized with scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, X-ray photoelectron spectroscopy （XPS）, X-ray diffraction （XRD）, and fluorescence spectropho- tometry. The results showed that the composite particles had a core-multishell structure, spherical morphology, and a narrow size distribution. The presence of a ZrO2 layer on the TiO2 core can effec- tively prevent the reaction between the TiO2 core and a Y203 shell; the temperature for the reaction between the TiO2 core and the Y203 shell in the TiO2@ZrO2@Y2O3 ：Eu core-multishell phosphor can be elevated by 300 ℃ compared to that for TiO2@ZrO2：Eu. Upon excitation of the core-multishell particles in the ultraviolet （254 nm）, the Eu3＋ ion in the Y2O3 ：Eu3＋ shell shows its characteristic red emission （611 nm, 5D0→7F2）, and the photoluminescence （PL） intensity of the phosphor with the core-multishell structure was obviously greater than that of the core-shell TiO2@Y2O3 ：Eu phosphor.     

Preparation and gas sensing performances of palladium surface-modified flower-like SnO2 nanopowders

Flower-like SnO2 nanopowders prepared by a hydrothermal method were surface modified with palla- dium via impregnation. The crystal structure, morphology, and surface chemistry states of the samples were characterized by means of X-ray diffraction （XRD）, scanning electron microscopy （SEM）, and X-ray photoelectron spectroscopy （XPS）, respectively. The gas sensing performances were also investigated. For a hydrothermal temperature of 220 ℃, flower-like SnO2 nanoparticles consist of nanorods with diameters of 40 nm and lengths of 100 nm. The XPS and XRD results reveal that palladium exists in the Pd0 chemical state but the crystal is too small to be detected. The 0.3 wt% Pd modified SnO2 sensor shows better sensi- tivity, up to 21, for 70 μL/L ethanol gas at an optimal working temperature of 250 ℃. The quick response time （3 s） and fast recovery time （-20 s） are the main characteristics of this sensor.     

A novel method for fast and continuous preparation of superfine titanium dioxide nanoparticles in microfluidic system

Previously we had developed a microfluidic system that can be easily fabricated by bending a stainless-steel tube into large circular loops. In this study, a fast and continuous preparation method for superfine TiO₂ nanoparticles (TiO₂-NPs) was developed for the aforementioned microfluidic system. The proposed method can yield anatase TiO₂ in 3.5 min, in contrast to the traditional hydrothermal reaction method, which requires hours or even days. Different reaction conditions, such as reaction temperature (120–200 °C), urea concentration (20–100 g/L), and tube length (5–20 m) were investigated. X-ray diffraction and Brunauer–Emmett–Teller analysis indicate that the as-prepared TiO₂-NPs have crystalline sizes of 4.1–5.8 nm and specific surface areas of 250.7–330.7 m²/g. Transmission electron microscopy images show that these TiO₂-NPs have an even diameter of approximately 5 nm. Moreover, because of their small crystalline sizes and large specific surface areas, most of these as-prepared TiO₂-NPs exhibit considerably better absorption and photocatalytic performance with methylene blue than commercial P5 TiO₂ does.     

Immobilization of Ti02 nanoparticles on activated carbon fiber and its photodegradation performance for organic pollutants

The immobilization of titanium dioxide （TiO2） on activated carbon fiber （ACF）, （TiO2/ACF）, was accomplished by sol-gel-adsorption method followed by calcination at temperatures varying from 300 to 600℃ in an argon atmosphere. The material properties were determined by scanning electron microscope （SEM）, X-ray diffraction （XRD） and nitrogen adsorption. The photodegradation behavior of TiO2 /ACF was investigated in aqueous solutions using phenol and methyl orange （MO） as target pollutants. The effects of calcination temperature, photocatalyst dosage, initial solution pH and radiation time on the degradation of organic pollutants were studied. It was found that organic pollutants could be removed rapidly from water by the TiO2/ACF photocatalyst and the sample calcined at 500℃ exhibited the highest removal efficiency. Kinetics analysis showed that the photocatalytic degradation reaction can be described by a first-order rate equation. In addition, the possibility of cyclic usage of the photocatalyst was also confirmed. Moreover, TiO2 is tightly bound to ACF and can be easily handled and recovered from water. It can therefore be potentially applied for the treatment of water contaminated by organic pollutants.     

Optimized synthesis and photovoltaic performance of TiO2 nanoparticles for dye-sensitized solar cell

This paper presents response surface methodology （RSM） as an efficient approach for modeling and optimizing TiO2 nanoparticles preparation via co-precipitation for dye-sensitized solar cell （DSSC） perfor- mance. Titanium （IV） bis-（acetylacetonate） di-isopropoxide （DIPBAT）, isopropanol and water were used as precursor, solvent and co-solvent, respectively. Molar ratio of water, aging temperature and calcina- tion temperature as preparation factors with main and interaction effects on particle characteristics and performances were investigated, Particle characteristics in terms of primary and secondary sizes, crys- tal orientation and morphology were determined by X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. Band gap energy and power conversion efficiency of DSSCs were used for perfor- mance studies. According to analysis of variance （ANOVA） in response surface methodology （RSM）, all three independent parameters were statistically significant and the final model was accurate. The model predicted maximum power conversion efficiency （0.14%） under the optimal condition of molar ratio of DIPBAT-to-isopropanol-to-water of 1 ： 10：500, aging temperature of 36 C and calcination temperature of 400 ℃. A second set of data was adopted to validate the model at optimal conditions and was found to be 0.14 ± 0.015%, which was very close to the predicted value. This study proves the reliability of the model in identi（ving the optimal condition for maximum performance.     

Hydrothermal synthesis of Mn-Zn ferrites from spent alkaline Zn-Mn batteries

Nanocrystalline Mn-Zn ferrites （Mno.GZno.4Fe204） with particle size of 12 nm were synthesized hydrotherreally using spent alkaline Zn-Mn batteries, and accompanied by a study of the influencing factors. The nanocrystals were examined by powder X-ray diffraction （XRD） for crystalline phase identification, and scanning electron microscopy （SEM） for grain morphology. The relationship between concentration of Fe（II）, Mn（II）, and Zn（II） and pH value was obtained through thermodynamic analysis of the Fe（II）-Mn（II）-Zn（II）-NaOH-H2O system. The results showed that all ions were precipitated completely at a pH value of 10-11. The optimal preparation conditions are： co-precipitation pH of 10.5, temperature of 200 ℃ and time of 9 h.     

Facile aqueous synthesis and thermal insulating properties of low-density glass/TiO2 core/shell composite hollow spheres

Anatase TiO₂ shells assembled on hollow glass microspheres (HGM) with tunable morphologies were successfully prepared through a controllable chemical precipitation method with urea as the precipitator. Thus, glass/TiO₂ core/shell composite hollow spheres with low particle density (0.40 g/cm³) were fabricated. The phase structures, morphologies, particle sizes, shell thicknesses, and chemical compositions of the composite microspheres were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). The morphology of the TiO₂ shell can be tailored by properly monitoring the reaction system component and parameters. The probable growth mechanism and fabrication process of the core/shell products involving the nucleation and oriented growth of TiO₂ nanocrystals on hollow glass microspheres was proposed. A low infrared radiation study revealed that the radiation properties of the products are greatly influenced by the unique product shell structures. A thermal conductivity study showed that the TiO₂/HGM possess low thermal conductivity that is similar to that of the pristine HGMs. This work provides an additional strategy to prepare low-density thermal insulating particles with tailored morphologies and properties.     

Microwave-hydrothermal preparation of a graphene/hierarchy structure MnO2 composite for a supercapacitor

Graphene/hierarchy structure manganese dioxide (GN/MnO₂) composites were synthesized using a simple microwave-hydrothermal method. The properties of the prepared composites were analyzed using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) measurements. The electrochemical performances of the composites were analyzed using cyclic voltammetry, electrochemical impedance spectrometry (EIS), and chronopotentiometry. The results showed that GN/MnO₂ (10 wt% graphene) displayed a specific capacitance of 244 F/g at a current density of 100 mA/g. An excellent cyclic stability was obtained with a capacity retention of approximately 94.3% after 500 cycles in a 1 mol/L Li₂SO₄ solution. The improved electrochemical performance is attributed to the hierarchy structure of the manganese dioxide, which can enlarge the interface between the active materials and the electrolyte. The preparation route provides a new approach for hierarchy structure graphene composites; this work could be readily extended to the preparation of other graphene-based composites with different structures for use in energy storage devices.     

Fabrication of nano-sized Ca(OH)2 with excellent adsorption ability for N2O4

Uniform nano-sized calcium hydroxide (Ca(OH)₂) monocrystal powder was synthesized from calcium oxide in a surfactant solution via a digestion method by decreasing the surface tension of the reaction system to control the growth of crystalline Ca(OH)₂. The Ca(OH)₂ monocrystal powder samples were characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), and Fourier transform-infrared spectroscopy (FT-IR). The NO_x adsorption ability of the samples was evaluated, and the influence of various types and concentrations of surfactants on powder agglomeration and then the specific surface area in the precipitation process were studied. The specific surface area of the samples was found as high as 58 m²/g and 92 m²/g and the particle size, 300–400 nm and 200–300 nm in the presence of 10 wt% PEG600 and 0.086 mL/L SDS at a reaction time of 5 h, respectively. The product has an exceptionally strong adsorption ability for NO_x, which makes it a highly promising adsorbent for emission control and air purification.     

Phase evolution of （K,Na）NbO3 powder prepared by high temperature mixing under hydrothermal conditions

（Na, K）NbO3 （KNN） powders were successfully prepared by high temperature mixing method （HTMM） under hydrothermal conditions to study the effect of reaction time on the formation of KNN for three K＋/（K＋ ＋Na＋） ratios of 0.6, 0.7 and 0.8. The products were characterized by X-ray diffraction （XRD）, scanning electron microscope （SEM）, transmission electron microscopy （TEM） and selected area electron diffraction （SAED）, to show the change of phase and morphology of the as-prepared particles with the K＋/（K＋ ＋ Na＋） molar ratio in the solution. Pure Na-rich KNN monoclinic phase and pure K-rich KNN orthorhombic phase could be obtained quickly after mixing the solutions at high temperature when the K＋/（K＋ ＋Na＋） molar ratio was either 0.6 or 0.8. When the K＋/（K＋ ＋Na＋） molar ratio was 0.7, however, the K-rich KNN orthorhombic phase grain formed first, followed by the Na-rich KNN monoclinic phase grain, with the two phases coexisting in the final product.     

Catalytic oxidation of benzene over Ce–Mn oxides synthesized by flame spray pyrolysis

Flame spray pyrolysis (FSP) was utilized to synthesize Ce–Mn oxides in one step for catalytic oxidation of benzene. Cerium acetate and manganese acetate were used as precursors. The materials synthesized were characterized using X-ray diffraction (XRD), N₂ adsorption, X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), Raman spectroscopy, and H₂-temperature programmed reduction (H₂-TPR) and their benzene catalytic oxidation behavior was evaluated. Mn ions were evidenced in multiple chemical states. Crystalline Ce–Mn oxides consist of particles with size <40 nm and specific surface areas (SSA) of 20–50 m²/g. Raman spectrums and H₂-TPR results indicated the interaction between cerium and manganese oxides. Flame-made 12.5%-Ce–Mn oxide exhibited excellent catalytic activity at relatively low temperatures (T₉₅ about 260 °C) compared to other Ce–Mn oxides with different cerium-to-manganese ratios. Redox mechanism and strong interaction conform to structure analysis that Ce–Mn strong interaction formed during the high temperature flame process and the results were used to explain catalytic oxidation of benzene.     

Synthesis of PS/Ag asymmetric hybrid particles via phase separation and self-assembly

This article presents a facile approach to preparation of polystyrene/silver （PS/Ag） asymmetric hybrid par- ticles. In this method, polystyrene/polyglycidyl methacrylate （PS/PGMA） Janus particles were synthesized via internal phase separation triggered by evaporation of dichloromethane （DCM） from PS/PGMA/DCM- in water emulsion droplets. Then, the Janus particles were aminated and sequentially carboxylated to obtain PS/PGMA-NH2 and PS/PGMA-COOH particles. Ag＋ self-assembled on the surface of PGMA hemi- sphere of the functionalized PS/PGMA particles by coordinating with amine/carboxyl. PS/Ag asymmetric hybrid particles with 7.29 wt% of Ag were obtained by reduction of Ag＋, Scanning electron microscopy, energy-dispersive X-ray spectroscopy and transmission electron microscopy results confirmed that Ag was asymmetrically distributed on the surface of polymer particles.     

TiO2-loaded activated carbon fiber: Hydrothermal synthesis,adsorption properties and photo catalytic activity under visible light irradiation

TiO₂-loaded activated carbon fibers (ACF) were prepared by a hydrothermal method. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrometry and UV–vis diffuse reflectance spectra (DRS). SEM images showed that the TiO₂ nanoparticles were deposited on the surface of ACF, and the particle size and loading amount of TiO₂ were varied by changing the initial concentration of tetrabutyl titanate (TBOT). The results of an ash experiment showed that the loading amounts of TiO₂ were 18.4%, 43.3%, 52.5%, 75.1%, and 91.1% for initial concentrations of TBOT of 0.07, 014, 0.21, 0.28, and 0.35 mol/L, respectively. Physical interactions played an important role in the formation of TiO₂/ACF composite fibers that absorb UV and visible light. Compared with those of ACF, improved adsorption and photocatalytic activity toward Rhodamine B (RhB) were observed for TiO₂/ACF composite fiber. The Rhodamine B could be removed efficiently by TiO₂/ACF composite fibers, and the TiO₂ loading amount had a significant effect on the photocatalytic activity of TiO₂/ACF composite fibers.     

Effects of multi-dopants (Zn and Ho) in stabilizing spinel structure for cathode materials in lithium rechargeable batteries—Novel chelated sol–gel synthesis

Multi-doped spinels, namely LiMn₂O₄ and LiZn_xHo_yMn_2−x−yO₄ (x = 0.10–0.18; y = 0.02–0.10), for use as cathode materials for lithium-ion rechargeable batteries were synthesized via sol–gel method, using lauric acid as the chelating agent, to obtain micron-sized particles. The physical properties of the synthesized samples were investigated using differential thermal analysis, Fourier-transform infrared spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy, energy-dispersive X-ray analysis, and electrochemical methods. XRD showed that LiMn₂O₄ and LiZn_xHo_yMn_2−x−yO₄ have high degrees of crystallinity and good phase purities. The SEM images of LiMn₂O₄ showed an ice-cube morphology with particles of size 1 μm. Charge–discharge studies showed that undoped LiMn₂O₄ delivered the discharge capacity of 124 mA h/g with coulombic efficiency of 95% during the first cycle, whereas doped spinels delivered discharge capacities of 125, 120, and 127 mA h/g in the first cycle with coulombic efficiencies of 96%, 91%, and 91%, respectively.     

In situ synthesis of CNTs/Fe–Ni/TiO2 nanocomposite by fluidized bed chemical vapor deposition and the synergistic effect in photocatalysis

Carbon nanotube (CNTs)/Fe–Ni/TiO₂ nanocomposite photocatalysts have been synthesized by an in situ fluidized bed chemical vapor deposition (FBCVD) method. The composite photocatalysts were characterized by XRD, Raman spectroscopy, BET, FESEM, TEM, UV–vis spectroscopy, and XPS. The results showed that the CNTs were grown in situ on the surface of TiO₂. Fe(III) in TiO₂ showed no chemical changes in the growth of CNTs. Ni(II) was partly reduced to metal Ni in the FBCVD process, and the metal Ni acted as a catalyst for the growth of CNTs. The photocatalytic activities of CNTs/Fe–Ni/TiO₂ decreased with the rise of the FBCVD reaction temperature. For the sample synthesized at low FBCVD temperature (500 °C), more than 90% and nearly 50% of methylene blue were removed under UV irradiation in 180 min and under visible light irradiation in 300 min, respectively. The probable mechanism of synergistic enhancement of photocatalysis on the CNTs/Fe–Ni/TiO₂ nanocomposite is proposed.     

Preparation and electrochemical performance of carbon-coated LiFePO4/LiMnPO4-positive material for a Li-ion battery

Lithium iron phosphate (LiFePO₄)/lithium manganese phosphate (LiMnPO₄)-positive material was successfully prepared through ball milling and high-temperature sintering using manganese acetate, lithium hydroxide, ammonium dihydrogen phosphate, and ferrous oxalate as raw materials. The as-prepared samples were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, a constant current charge–discharge test, cyclic voltammetry, and electrochemical impedance spectroscopy. The effects of lithium iron phosphate coating were also discussed. Because of its special core–shell structure, the as-prepared LiMn_0.7Fe_0.3PO₄–LiFePO₄–C exhibits excellent electrochemical performance. The discharge capacity reached 136.6 mAh/g and the specific discharge energy reached 506.9 Wh/kg at a rate of 0.1 C.     

Solvent-less synthesis of zinc oxide nanostructures from Zn(salen) as precursor and their optical properties

ZnO nanoparticles, 10–20 nm in size, were synthesized by heat treatment in air at 500 °C for 5 h., using [N,N′-bis(salicylaldehydo) ethylene diamine]zinc(II), i.e., Zn(salen), as precursor, which was obtained by a solvent-free solid–solid reaction. Heat-treated products were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and transmission electron microscopy. Room temperature photoluminescence spectra of ZnO nanostructures are dominated by green emission attributed to oxygen vacancy related donor–acceptor transition.     

Sol-gel synthesis and characterization of hydroxyapatite nanorods

In the present study hydroxyapatite （HA） nano-hexagonal rods with 70-90 nm diameter and 400-500 nm length are synthesized using a simple sol-gel route with calcium nitrate and potassium dihydrogenphosphate as calcium and phosphorus precursors respectively. Deionized water was used as a diluting media for HA sol preparation and ammonia was used to adjust the pH = 9. After aging, the HA gel was dried at 60 ℃ and calcined at different temperatures ranging from 300 to 700 ℃. The dried and calcined powders were characterized for phase composition using X-ray diffractrometry, elemental dispersive X-ray and Fourier transform infrared spectroscopy. Rietveld analysis showed the calcined HA powders of high purity with a hexagonal unit cell structure. Calcination yielded HA nanopowders of increased particle size and crystallinity with increase in temperature. The particle size and morphology was studied using transmission electron microscopy. The aspect ratio （length to diameter ratio） of HA nanorods was measured to be between 6 and 7.     

Fabrication of magnetic nanosized γ-FeNi-coated ceramic core–shell microspheres by heterogeneous precipitation and thermal reduction

Precursors with NiCO₃·2Ni(OH)₂·2H₂O- and Fe₂O₃·nH₂O-coated alumina, graphite and cenosphere were synthesized by precipitation using ferrous sulfate, nickel sulfate, ammonium bicarbonate, alumina, graphite and cenosphere as the main starting materials. Magnetic γ-FeNi-coated alumina, graphite and cenosphere core–shell structural microspheres were subsequently prepared by thermal reduction of the as-prepared precursors at 600 °C for 2 h. Precipitation parameters, e.g. concentration of ceramic micropowders (10 g/L), sulfate solution (0.2 mol/L), rate of adding reactants (3 mL/min) and pH value were optimized by a trial-and-error method. Powders of the precursors and the resulting coating of γ-FeNi with grain size below 40 nm on alumina, graphite and cenosphere microspheres were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The magnetic properties of the nanosize γ-FeNi-coated alumina, graphite and cenosphere microspheres were measured by vibrating sample magnetometer (VSM). The results show that the core–shell structural γ-FeNi-coated ceramic microspheres exhibited higher coercivity than pure γ-FeNi powders, indicating that these materials can be used for high-performance functional materials and devices.     

Modification of silica with PMMA via ultrasonic irradiation and its application for reinforcement of polyacrylates

Polymethyl methacrylate （PMMA） encapsulated silica nanocomposite particles were prepared by ultra- sonically induced in situ polymerization of methyl methacrylate （MMA） on the surface of silica sol. The nanoparticles were characterized by Fourier transform infrared spectroscopy （FFIR）, transmission electron microscopy （TEM）, thermogravimetry （TG）, scanning electron microscopy （SEM）. The results showed that core-shell structure nanocomposite particles with an average size of 36 nm were obtained, and the thickness of polymer encapsulating layer was about 8 nm. The pretreatment of silica sol with tert-butyl hydroperoxide （TBHP） and the addition of ~-methacryloxypropyl trimethoxysilane （MAPTS） significantly enhanced the encapsulation effect. Modified by the polymer layer, the silica particles could be well dispersed in matrices and utilized to improve the mechanical performance of polyacrylates.