Controlled synthesis of Ce(OH)CO3 flowers by a hydrothermal method and their thermal conversion to CeO2 flowers

Highly uniform Ce(OH)CO₃ flowers were successfully prepared in large quantities using a facile hydrothermal approach from the reaction of Ce(NH₄)(NO₃)₄ with CO(NH₂)₂ at 160 °C in a water–N₂H₄ complex. The influences of the N₂H₄ content and temperature on flower formation were discussed. CeO₂ flowers were prepared by thermal conversion of Ce(OH)CO₃ flowers at 500 °C in air. Both Ce(OH)CO₃ and CeO₂ flowers were characterized by X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The UV–vis adsorption spectrum of the CeO₂ flowers showed that the band gap energy (E_g) is 2.66 eV, which is lower than that of bulk ceria.     

Hydrothermal preparation of nanocrystalline ZnO2

A green hydrothermal method was proposed for the synthesis of nanocrystalline ZnO₂, using Zn₅(CO₃)₂(OH)₆ powder and 6 vol% H₂O₂ aqueous solution as the starting materials. Characterization results from X-ray diffraction, Raman, high resolution transmission electron microscopy and selected area electron diffraction revealed that the products synthesized at 80–120 °C for 6–18 h were pure cubic phase ZnO₂ nanocrystals. Room temperature photoluminescence spectra of the as-synthesized ZnO₂ nanocrystals displayed a wide and strong emission band in the visible region of about 525–570 nm upon laser excitation at 325 nm, which may have originated from their surface state and other crystal defects.     

Spatiotemporal variations of PM2.5 and PM10 concentrations between 31 Chinese cities and their relationships with SO2, NO2, CO and O3

The variations of mass concentrations of PM_2.5, PM₁₀, SO₂, NO₂, CO, and O₃ in 31 Chinese provincial capital cities were analyzed based on data from 286 monitoring sites obtained between March 22, 2013 and March 31, 2014. By comparing the pollutant concentrations over this length of time, the characteristics of the monthly variations of mass concentrations of air pollutants were determined. We used the Pearson correlation coefficient to establish the relationship between PM_2.5, PM₁₀, and the gas pollutants. The results revealed significant differences in the concentration levels of air pollutants and in the variations between the different cities. The Pearson correlation coefficients between PMs and NO₂ and SO₂ were either high or moderate (PM_2.5 with NO₂: r = 0.256–0.688, mean r = 0.498; PM₁₀ with NO₂: r = 0.169–0.713, mean r = 0.493; PM_2.5 with SO₂: r = 0.232–0.693, mean r = 0.449; PM₁₀ with SO₂: r = 0.131–0.669, mean r = 0.403). The correlation between PMs and CO was diverse (PM_2.5: r = 0.156–0.721, mean r = 0.437; PM₁₀: r = 0.06–0.67, mean r = 0.380). The correlation between PMs and O₃ was either weak or uncorrelated (PM_2.5: r = −0.35 to 0.089, mean r = −0.164; PM₁₀: r = −0.279 to 0.078, mean r = −0.127), except in Haikou (PM_2.5: r = 0.500; PM₁₀: r = 0.509).     

Synthesis of potassium sodium niobate powders using an EDTA/citrate complexing sol–gel method

Potassium sodium niobate (KNN) powders were synthesized by a modified sol–gel method, using as starting chemicals potassium carbonate, sodium carbonate, and niobium hydroxide, and, as esterification and chelating agents, respectively, ethylene glycol (EG) and ethylene diamine tetraacetic acid (EDTA)/citrate. The effects of citric acid (CA), EG, and EDTA on the stability of the precursor sol were systemically investigated. The powders and gels were characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis-differential scanning calorimetry (TGA-DSC). The results indicated that a stable precursor sol was formed when n(CA):n(Mⁿ⁺) = 3:1, n(EDTA):n(NH₄OH) = 1:3.5, and n(CA):n(EG) = 1:2. The xerogel was calcined at 500–950 °C to prepare the KNN powder. Pure KNN perovskite phase with a cube-like structure was synthesized at 850 °C from the precursor sol for a K/Na molar ratio of 1.2. The formation mechanism of the KNN perovskite phase was also discussed.     

Hydrothermal synthesis of ultrathin hexagonal nickel hydroxide nanosheets

Nickel hydroxide, Ni(OH)₂ is widely used in electrodes of nickel-based alkaline secondary batteries. Ultrathin hexagonal Ni(OH)₂ nanosheets of space group P-3m1 were hydrothermally prepared at 200 °C for 10 h. Their diameter and thickness were 200–300 and 3–5 nm, respectively. Their formation was attributed to the oriented assembly of growing particles, which was assisted by surfactant molecules. The specific surface area of the Ni(OH)₂ nanosheets was 8.66 m²/g. Their magnetization curve exhibited linear paramagnetic behavior across the entire measurement region.     

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.     

Composition and morphology of the thermal decomposition products of 3Mg(OH)2·MgCl2·8H2O nanowires

The thermal decomposition of 3Mg(OH)₂·MgCl₂·8H₂O (318MHCH) nanowires synthesized from agglomerated Mg(OH)₂ microspheres was investigated. The influence of heating rate and temperature on the composition and morphology of the products was investigated. Thermogravimetric-differential scanning calorimetry, field-emission scanning electron microscopy, high-resolution transmission electron microscopy, and X-ray diffraction showed that increasing the heating rate from 1 to 20 °C/min promoted the escape of crystalline water from the 318MHCH nanowires. 318MHCH nanowires were dehydrated stepwise to 310MHCH porous nanowires from room temperature to 320 °C, and then to MgO cubic nanoparticles from 420 to 700 °C. The nanowires retained their one-dimensional morphology, until the phase changed to MgO. The immediate collapse of the one-dimensional structure was attributed to the presence of Mg–O/Cl chains.     

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.     

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.     

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.     

Controllable hydrothermal synthesis of star-shaped Sr3Fe2(OH)12 assemblies and their thermal decomposition and magnetic properties

Pure phase star-shaped hydrogarnet Sr₃Fe₂(OH)₁₂ assemblies were synthesized by a mild hydrothermal method (210 °C, 12 h), and the effects of the preparation conditions on the phase composition of the product were investigated. It was found that the impurity phases could be decreased or eliminated by increasing the molar ratio of Sr²⁺ to Fe³⁺, and that high temperatures favored the formation of Sr₃Fe₂(OH)₁₂ and reduced the concentration of CO₃^2–-containing byproducts. The thermal decomposition of the star-shaped Sr₃Fe₂(OH)₁₂ assemblies was examined, and the results showed that the dehydration process at higher temperatures is accompanied by the formation of SrFeO_3–δ. Above 655 °C, a solid state reaction between the SrFeO_3–δ and Sr(OH)₂ or SrCO₃ results in the formation of Sr₄Fe₃O_10–δ.The magnetic properties of the as-synthesized Sr₃Fe₂(OH)₁₂ and of samples calcined at different temperatures were assessed. A sample calcined at 575 °C exhibited greatly enhanced ferromagnetic properties, with a remanent magnetization of 1.28 emu/g and a coercivity of 4522.1 Oe at room temperature.     

Preparation of nano-sized Al2O3–2SiO2 powder by sol–gel plus azeotropic distillation method

Nano-sized amorphous Al₂O₃–2SiO₂ powder was prepared by a sol–gel method coupled with azeotropic distillation. The structure of the powder was investigated by DTS, BET, TEM, FT-IR, TG-DTA and XRD, showing that n-butanol azeotropic distillation could effectively remove water from the aluminosilicate gels and prevent the formation of hard agglomerates in the drying process. The average particle diameter of the powder was about 70 nm. The largest BET specific surface area of the powder was 669 m²/g. To examine the alkali-activation reactivity of the powder, alkali-activation tests were performed with the powder reacting with sodium silicate solution. The synthetic powder was found to be highly reactive.     

Synthesis of mesoporous γ-AlOOH@Fe3O4 magnetic nanomicrospheres

Mesoporous γ-AlOOH@Fe₃O₄ magnetic nanomicrospheres were synthesized using superparamagnetic Fe₃O₄ nanoparticles as the core and aluminum isopropoxide (AIP) as the aluminum source. The obtained magnetic nanomicrospheres were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N₂ adsorption–desorption and vibrating sample magnetometry (VSM). The effects of preparation parameters such as hydrolysis time of AIP, concentration of AIP and coating layer number on microspheres were investigated. The results indicated that the mesoporous γ-AlOOH@Fe₃O₄ magnetic nanomicrospheres consisted of a mesoporous γ-AlOOH shell and a Fe₃O₄ magnetic core. The diameter of γ-AlOOH@Fe₃O₄ nanomicrospheres was about 200 nm, the thickness of mesoporous γ-AlOOH shell was about 5 nm and the average pore size was 3.8 nm. The thickness of the mesoporous γ-AlOOH shell could be controlled via layer-by-layer coating times. The formation mechanism of the mesoporous γ-AlOOH shell involved a “chemisorption–hydrolysis” process.     

Magnetic and electrochemical behavior of rhombohedral α-Fe2O3 nanoparticles with (1 0 4) dominant facets

Uniform rhombohedral α-Fe₂O₃ nanoparticles, ～60 nm in size, were synthesized via a triphenylphosphine-assisted hydrothermal method. Scanning electron micrograph (SEM) and transmission electron micrograph (TEM) analyses showed that the as-synthesized rhombohedral nanoparticles were enclosed by six (1 0 4) planes. The concentration of triphenylphosphine played an important role in morphological evolution of the α-Fe₂O₃ nanoparticles. The as-prepared rhombohedral nanoparticles possessed remanent magnetization M_r of 2.6 × 10^?3 emu/g and coercivity H_C of 2.05 Oe, both lower than those of other α-Fe₂O₃ particles with similar size, indicating their potential applications as superparamagnetic precursor materials. Furthermore, these rhombohedral α-Fe₂O₃ nanoparticles exhibited good sensor capability toward H₂O₂ with a linear response in the concentration range of 2–20 mM.     

Large-scale synthesis of hierarchical MnO2 for benzene catalytic oxidation

Hierarchical sea-urchin-shaped manganese oxide microspheres were synthesized via a facile method based on the reaction between KMnO₄ and MnSO₄ in HNO₃ solution at 50 °C. The average diameter of the microspheres is ∼850 nm. The microspheres consist of a core of diameter of ∼800 nm and nanorods of width ∼50 nm. The nanorods exist at the edge of the core. The Brunauer–Emmett–Teller surface area of the sea-urchin-shaped microspheres is 259.4 m²/g. A possible formation mechanism of the hierarchical sea-urchin-shaped microspheres is proposed. The temperature for 90% conversion of benzene (T_90%) on the hierarchical urchin-shaped MnO₂ microspheres is about 218 °C.     

Capture of phosphates in surface water by TiO2 nanoparticles under UV irradiation

The capture of orthophosphates and total phosphorus from the Pudong Canal river in the Pudong District of Shanghai by TiO₂ nanoparticles is studied using a rotating photoreactor and the nano-TiO₂ photocatalyst Degussa P25. The effects of UV irradiation intensity in a range of 20–74 mW/cm², the loading of the TiO₂ nanoparticles in a range of 0.05–0.1 g/L, irradiation time up to 4 h, and pH values in a range of 2–10.5 on the capture efficiency are investigated. The results show that the capture of orthophosphates and total P are significantly enhanced by UV irradiation; at a loading of 0.1 g/L and an irradiation intensity above 36 mW/cm², orthophosphates and total phosphorus are rapidly captured by TiO₂ nanoparticles, causing an observed reduction from 0.4 mg/L down to 0.02 mg/L. pH values in a range of 2–10.5 have little effect on the capture efficiency of orthophosphates and total phosphorus.     

Emission of organic carbon,elemental carbon and water-soluble ions from crop straw burning under flaming and smoldering conditions

Emissions from major agricultural residues were measured using a self-designed combustion system. Emission factors (EFs) of organic carbon (OC), elemental carbon (EC), and water-soluble ions (WSIs) (K⁺, NH₄⁺, Na⁺, Mg²⁺, Ca²⁺, Cl⁻, NO₃⁻, SO₄^2–) in smoke from wheat and rice straw were measured under flaming and smoldering conditions. The OC₁/TC (total carbon) was highest (45.8% flaming, 57.7% smoldering) among carbon fractions. The mean EFs for OC (EF_OC) and EC (EF_EC) were 9.2 ± 3.9 and 2.2 ± 0.7 g/kg for wheat straw and 6.4 ± 1.9 and 1.1 ± 0.3 g/kg for rice straw under flaming conditions, while they were 40.8 ± 5.6 and 5.8 ± 1.0 g/kg and 37.6 ± 6.3 and 5.0 ± 1.4 g/kg under smoldering conditions, respectively. Higher EC ratios were observed in particulate matter (PM) mass under flaming conditions. The OC and EC for the two combustion patterns were significantly correlated (p < 0.01, R = 0.95 for wheat straw; p < 0.01, R = 0.97 for rice straw), and a higher positive correlation between OC₃ and EC was observed under both combustion conditions. WSIs emitted from flaming smoke were dominated by Cl⁻ and K⁺, which contributed 3.4% and 2.4% of the PM mass for rice straw and 2.2% and 1.0% for wheat straw, respectively. The EFs of Cl⁻ and K⁺ were 0.73 ± 0.16 and 0.51 ± 0.14 g/kg for wheat straw and 0.25 ± 0.15 and 0.12 ± 0.05 g/kg for rice straw under flaming conditions, while they were 0.42 ± 0.28 and 0.12 ± 0.06 g/kg and 0.30 ± 0.27 and 0.05 ± 0.03 g/kg under smoldering conditions, respectively. Na⁺, Mg²⁺, and NH₄⁺ were vital components in PM, comprising from 0.8% (smoldering) to 3.1% (flaming) of the mass. Strong correlations of Cl⁻ with K⁺, NH₄⁺, and Na⁺ ions were observed in rice straw and the calculated diagnostic ratios of OC/EC, K⁺/Na⁺ and Cl⁻/Na⁺ could be useful to distinguishing crop straw burning from other sources of atmospheric pollution.     

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.     

Microstructure and mechanical properties of ZrO2 (Y2O3)–Al2O3 nanocomposites prepared by spark plasma sintering

Zirconia (yttria)–alumina ceramic nanocomposites were fabricated from different powders by spark plasma sintering (SPS). One powder was a commercially available nanocomposite powder TZP-3Y20A, consisting of 3 mol% yttria-stabilized zirconia (3-YSZ) reinforced with 20 wt% alumina, and the other, used as a comparison, was a conventional mechanically mixed powder 3YSZ-20A, a blend made of 3 mol% yttria-stabilized zirconia powder ZrO₂ (3Y) and 20 wt% α-alumina powder. The effect of the sintering temperature on the densification, the sintering behavior, the mechanical properties and the microstructure of the composites was investigated. The results showed that the density increased with increasing sintering temperature, and thus, the mechanical properties were strengthened because of the increased densification. The nanocomposite powder TZP-3Y20A was easily sintered, and good mechanical properties were achieved as compared with the powder from the conventional mechanically mixed method, the maximum flexural strength and fracture toughness of which were 967 MPa and 5.27 MPa m^1/2, respectively.     

Capuli cherry-mediated green synthesis of silver nanoparticles under white solar and blue LED light

In this article, the Capuli (Prunus serotina Ehrh. var. Capuli) cherry extract was used for the synthesis of silver nanoparticles (AgNPs) in the presence of white/visible solar and blue light-emitting diode (LED) light. For the characterization of the extract and the AgNPs, Fourier transform infrared spectroscopy and ultraviolet–visible spectroscopy were employed, along with hydrodynamic particle size analysis, transmission electron microscopy and X-ray diffraction. The Ag nanospheres obtained using white light were 40–100 nm in diameter and exhibited an absorption peak at λ_max = 445 nm, whereas those obtained using blue LED light were 20–80 nm in diameter with an absorption peak at λ_max = 425 nm. Thermal analysis revealed that the content of biomolecules surrounding the AgNPs was about 55–65%, and it was also found that blue LED light AgNPs (56.28%, 0.05 mM) had a higher antioxidant efficacy than the white solar light AgNPs (33.42%, 0.05 mM) against 1,1-diphenyl-2-picrylhydrazyl. The results indicate that obtaining AgNPs using a blue LED light may prove to be a simple, cost-effective and easily reproducible method for creating future nanopharmaceuticals.