Photocatalytic degradation of metronidazole in aqueous solution by niobate K<Subscript>6</Subscript>Nb<Subscript>10.8</Subscript>O<Subscript>30</Subscript>

The photocatalytic degradation of antibiotic metroni-dazole in aqueous solution by niobate K6Nb10.8O30 photocatalyst that was prepared using a soft-chemical method was studied by Fourier transform infrared spectroscopy and UV-Vis absorption spectrum. Metronidazole is very stable and is difficult to degrade under UV irradiation. K6Nb10.8O30 photocatalyst cannot degrade metronidazole without UV irradiation and shows very high photo-catalytic activity for the degradation of metronidazole under UV irradiation. The photocatalytic degradation rate of metronidazole increased with increasing the dosage of K6Nb10.8O30 photocatalyst. The photocatalytic degradation reaction of metronidazole by nio-bate K6Nb10.8O30 follows the first-order kinetic equation.     

Phase transformation and crystal growth behavior of 8mol% (SmO<Subscript>1.5</Subscript>, GdO<Subscript>1.5</Subscript>, and YO<Subscript>1.5</Subscript>) stabilized ZrO<Subscript>2</Subscript> powders

Nanocrystalline powders of ZrO₂-8mol%SmO_1.5(8SmSZ), ZrO₂-8mol%GdO_1.5 (8GdSZ), and ZrO₂-8mol%YO_1.5(8YSZ) were prepared by a simple reverse-coprecipitation technique. Differential thermal analysis/thermogravimetry (DTA/TG), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to study the phase transformation and crystal growth behavior. The DTA results showed that the ZrO₂ freeze-dried precipitates crystallized at 529, 465, and 467℃ in the case of 8SmSZ, 8GdSZ, and 8YSZ, respectively. The XRD and Raman results confirmed the presence of tetragonal ZrO₂ when the dried precipitates were calcined in the temperature range from 600 to 1000℃ for 2 h. The crystallite size increased with increasing calcination temperature. The activation energies were calculated as 12.39, 12.45, and 16.59 kJ/mol for 8SmSZ, 8GdSZ, and 8YSZ respectively.     

Photoluminescence and cathodoluminescence properties of CaLaGa<Subscript>3</Subscript>O<Subscript>7</Subscript>:Eu<Superscript>3+</Superscript> phosphors

The CaLaGa₃O₇:Eu³⁺ phosphor was prepared by a chemical co-precipitation method. Field emission scanning electron microscopy (FE-SEM), laser particle size analysis, X-ray diffraction (XRD), photoluminescence (PL), and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphor. The results revealed that the phosphor was composed of microspheres with a slight agglomerate phenomenon and was spherically shaped. The average grain size was about 1.0 μm. Eu³⁺ ions, as luminescent centers, substituted La³⁺ ions into the single crystal lattice of CaLaGa₃O₇ with the sites of C_s. Although the CL spectrum was greatly different from the PL spectrum, it had the strongest red emission corresponding to the ⁵D₀ →⁷F₂ transition of Eu³⁺. Under the excitation of UV light (287 nm) and electron beams (1.0–7.0 kV), the chromaticity coordinates of the phosphor were found to be in the nearly red and orange light regions, respectively.     

Synthesis and characterization of wormhole-like mesoporous Ce0.6Zr0.35Y0.05O2 solid solutions

Nanoparticles of Ce0.6Zr0.35Y0.05O2 (CZY) solid solution have been prepared by the CTAB (hexadecyl-trimethyl ammonium bromide), CTAB-EG (ethylene glycol) templating, and CTAB-EG-NaCl (in which the pores of the precursor synthesized by the CTAB-EG method is filled by a certain amount of NaCl) method, respectively. The physical properties of these materials were characterized by means of tech-niques such as X-ray diffraction (XRD), high resolution scanning electron microscopy (HRSEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and N2 adsorp-tion-desorption measurements. The CZY samples synthesized by the above three methods display wormhole-like mesoporous morphology and cubic crystal structures. The materials are narrow in pore size distribution (averaged pore diameter = 5.3―7.1 nm), high in surface areas (95―119 m2/g), and large in pore volumes (0.16―0.18 cm3/g). It has been demonstrated that the introduction of NaCl is capable of retaining the pore structures of solid nanomaterials at high-temperature calcination.     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.     

Electro-deoxidation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> in molten CaCl<Subscript>2</Subscript>-NaCl-CaO

The electro-deoxidation of V₂O₃ precursors was studied. Experiments were carried out with a two-terminal electrochemical cell, which was comprised of a molten electrolyte of CaCl₂ and NaCl with additions of CaO, a cathode of compact V₂O₃, and a graphite anode under the potential of 3.0 V at 1173 K. The phase constitution and composition as well as the morphology of the samples were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). 3 g of V₂O₃ could be converted to vanadium metal powder within the processing time of 8 h. The kinetic pathway was investigated by analyzing the product phase in samples prepared at different reduction stages. CaO added in the reduction path of V₂O₃ formed the intermediate product CaV₂O₄.     

Synthesis and Structure of Polypyrrole Derivatives／V2O5 Nanocomposites

Poly ( N, N, N-trimethyl ( 2-pyrrol-l-yl ) ethyl ammonium iodide )/V2O5 ( PTPAI/V2O5) nanocomposites were synthesized by sol-gel method. This method involved formation of vanadium pentoxide xerogel in the prcscnce of polypyrrole derivatives solution. X-ray diffraction(XRD) indicated that the polypyrrole derivative particles encapsulated in the fibrous V2O5 network and the layered distance significantly increased from 1. 077 39 to 1. 354 56 nm. The interaction between polypyrrole and V2O5 in the ‘nanocomposites‘ was characterized by IR spectroscopy. The Scanning Electron Microscope(SEM) micrographs reveal the structural contrasts between the hybrid materials and the pristine vanadium oxide xerogel.     

Growth characteristics of directionally solidified Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/YAG/ZrO<Subscript>2</Subscript> ternary hypereutectic <Emphasis Type="Italic">in situ</Emphasis> composites under ultra-high temperature gradient

Oxide eutectic ceramic in situ composites have attracted significant interest in the application of high-temperature structural materials because of their excellent high-temperature strength, oxidation and creep resistance, as well as outstanding microstructural stability. The directionally solidified ternary Al₂O₃/YAG/ZrO₂ hypereutectic in situ composite was successfully prepared by a laser zone remelting method, aiming to investigate the growth characteristic under ultra-high temperature gradient. The microstructures and phase composition of the as-solidified hypereutectic were characterized by using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD). The results show that the composite presents a typical hypereutectic lamellar microstructure consisting of fine Al₂O₃ and YAG phases, and the enriched ZrO₂ phases with smaller sizes are randomly distributed at the Al₂O₃/YAG interface and in Al₂O₃ phases. Laser power and scanning rate strongly affect the sample quality and microstructure characteristic. Additionally, coarse colony microstructures were also observed, and their formation and the effect of temperature gradient on the microstructure were discussed.     

Synthesis and modification of well-ordered layered cathode oxide LiNi<Subscript>2/3</Subscript>Mn<Subscript>1/3</Subscript>O<Subscript>2</Subscript>

Oxalic-acid-based co-precipitation method was employed to prepare LiNi_2/3Mn_1/3O₂ sample with a high-ordered structure. Li⁺, Ni²⁺ and Mn²⁺ acetates were used as starting materials. The influence of the amount of lithium source in the starting materials on Li⁺ content, disorder of Li⁺-Ni²⁺ ions, and electrochemical performance has been investigated. Rietveld refinement shows that the sample prepared with 20% excess Li-source in the starting materials exhibits a perfect ordered structure. A specific discharge capacity is as high as 172 mAh/g at C/20 in the voltage range of 4.35–2.7 V. However, the cyclability is not satisfactory: about 25.3% fade in capacity was observed over 50 cycles. Chemically stable SiO2 was coated on the surface of LiNi_2/3Mn_1/3O₂ particles. A significant improvement in cyclability was attained with 3 wt% SiO2 coating, which is ascribable to the protection of LiNi_2/3Mn_1/3O₂ particles from being dissolved into the electrolyte.     

The electrical property of MnCo<Subscript>2</Subscript>O<Subscript>4</Subscript> and its application for SUS 430 metallic interconnect

The conductivity of MnCo₂O₄ spinel, the best route to form the MnCo₂O₄ protective coating applied by the sol-gel process, and its effect on the intermediate temperature oxidation behavior of SUS 430 alloy, a typical material for the interconnect of solid oxide fuel cell (SOFC), was investigated. The phase structure and surface morphology of the coating and surface oxides were characterized by XRD, SEM and EDS; the “4-probe” method was employed to determine the conductivity of MnCo₂O₄ spinel and the area specific resistance (ASR) of the surface oxides. The conductivity of MnCo₂O₄ spinel is excellent, which is 2 orders of magnitude better than that of MnCr₂O₄ spinel. Long-term thermally cyclic oxidation at 750°C in SOFC cathode atmosphere and ASR measurement have shown that calcined in reducing atmosphere followed by pre-oxidation in the air is the best technique for forming the MnCo₂O₄ protective coating, which enhances the oxidation resistance, and improves the electrical conductivity and adherence of coated SUS 430 alloy significantly. As a result, the MnCo₂O₄ spinel is the most potential candidate for SOFC metallic interconnect protective coating application.     

Preparation of Al<Subscript>72</Subscript>Ni<Subscript>8</Subscript>Ti<Subscript>8</Subscript>Zr<Subscript>6</Subscript>Nb<Subscript>3</Subscript>Y<Subscript>3</Subscript> amorphous powders and bulk materials

Amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were successfully fabricated by mechanical alloying. The microstructure, glass-forming ability, and crystallization behavior of amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), and differential scanning calorimetry (DSC). The isothermal crystallization kinetics was analyzed by the Johnson–Mehl–Avrami equation. In the results, the supercooled liquid region of the amorphous alloy is as high as 81 K, as determined by non-isothermal DSC curves. The activation energy for crystallization is as high as 312.6 kJ·mol?1 obtained by Kissinger and Ozawa analyses. The values of Avrami exponent (n) imply that the crystallization is dominated by interface-controlled three-dimensional growth in the early stage and the end stage and by diffusion-controlled two- or three-dimensional growth in the middle stage. In addition, the amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were sintered under 2 GPa at temperatures of 673 K and 723 K. The results show that the Vickers hardness of the compacted powders is as high as Hv 1215.     

Preparation and characterization of porous ceramics prepared by kaolinite gangue and Al(OH)<Subscript>3</Subscript> with double addition of MgCO<Subscript>3</Subscript> and CaCO<Subscript>3</Subscript>

Porous ceramics were prepared from kaolinite gangue and Al(OH)₃ with double addition of MgCO₃ and CaCO₃ by the pore-forming in-situ technique. The characterizations of porous ceramics were investigated by X-ray diffractometry, scanning electron microscopy, and mercury porosimetry measurements, etc. It is found that although the decomposition of MgCO₃ and CaCO₃ has little contribution to the porosity, the double addition of MgCO₃ and CaCO₃ strongly affects the formation of liquid phase, and then changes the phase compositions, pore characterization, and strength. The appropriate mode is the sample containing 1.17wt% MgCO₃ and 1.17wt% CaCO₃, which has high apparent porosity (41.0%), high crushing strength (53.5 MPa), high mullite content (76wt%), and small average pore size (3.24 μm).     

Microstructure and properties of mullite-based porous ceramics produced from coal fly ash with added Al<Subscript>2</Subscript>O<Subscript>3</Subscript>

Using coal fly ash slurry samples supplemented with different amounts of Al₂O₃, we fabricated mullite-based porous ceramics via a dipping-polymer-replica approach, which is a popular method suitable for industrial application. The microstructure, phase composition, and compressive strength of the sintered samples were investigated. Mullite was identified in all of the prepared materials by X-ray diffraction analysis. The microstructure and compressive strength were strongly influenced by the content of Al₂O₃. As the Al/Si mole ratio in the starting materials was increased from 0.84 to 2.40, the amount of amorphous phases in the sintered microstructure decreased and the compressive strength of the sintered samples increased. A further increase in the Al₂O₃ content resulted in a decrease in the compressive strength of the sintered samples. The mullite-based porous ceramic with an Al/Si molar ratio of 2.40 exhibited the highest compressive strength and the greatest shrinkage among the investigated samples prepared using coal fly ash as the main starting material.     

Synthesis of highly ordered SnO2／Fe2O3 composite nanowire arrays by electrophoretic deposition method

Highly ordered SnO2/Fe2O3 composite nanowire arrays have been synthesized by electrophoretic deposition method. The morphology and chemical composition of SnO2/Fe2O3 composite nanowire arrays are characterized by SEM, TEM, EDX, XPS, and XRD. The results show that the SnO2/Fe2O3 composite nanowires are about 180 nm in width and tens of microns in length, and they are composed of small nanoparticles of tetraganal SnO2 and rhombohedral α-Fe203 with diameters of 10-15nm. The SnO2/Fe2O3 composite nanowires are formed by a series of chemical reactions.     

Synthesis of LiCo<Subscript>0.3</Subscript>Ni<Subscript>0.7</Subscript>O<Subscript>2</Subscript> as cathode materials for lithium ion batteries by citric acid-assisted sol-gel method

The synthesis process of LiCo0.3Ni0.7O2 was investigated by FT-IR, mass spectroscopy, elemental analysis, SEM, BET, TG/DTA and XRD in this paper. The results revealed that lithium and transition metal ions were trapped homogeneously on an atomic scale throughout the precursor. Li2CO3, NiO and CoO are the intermediate products obtained after decomposition of the precursor and Li2CO3 undergoes direct reactions with NiO and CoO to form LiCo0.3Ni0.7O2. Moreover, the kinetics of formation of LiCo0.3Ni0.7O2 by dtrate sol-gel method is faster than the case of the conventional solid-state reaction between lithium carbonate and corresponding reactants. The single phase of LiCo0.3Ni0.7O2 was synthesized at temperature as low as 550℃. The discharge capacity of LiCo0.3Ni0.7O2 increases from 127 to 185 mAh/g as the caldnation temperature increasing from 550 to 750℃. After 100 cycles, the discharge capacity of the sample calcined at 750℃ is 155 mAh/g. The electrochemical study shows that the LiCo0.3Ni0.7O2 has high discharge capacity and good cycling behavior for lithium ion batteries.     

Synthesis, Characterization and Calorimetry of Ni（C4H8N2O3）2Cl2

A coordination complex was synthesized from NiCl2 and dipeptide glycylglycine（GG）. It was characterized by element analysis, NMR and TG methods, and then was determined to be Ni（C4HsN2O3）2Cl2. Using an isoperibolic reaction calorimeter, the standard molar enthalpy of formation of Ni（GG）2Cl2（solid） has been determined to be -（1 674.66±2.02） kJ · mol^-1 at 298.15 K.     

Photoluminescence and cathodoluminescence properties of a novel CaLaGa307：Dy3＋ phosphor

A single host white emitting phosphor, CaLaGa3O7:Dy3+, was synthesized by chemical co-precipitation. Field emission scanning electron microscopy, X-ray diffraction, laser particle size analysis, and photoluminescence and cathodoluminescence spectra were used to investigate the structural and optical properties of the phosphor. The phosphor particles were composed of microspheres with a slight tendency to agglomerate, and an average diameter was of about 1.0 μm. The Dy3+ ions acted as luminescent centers, and substituted La3+ ions in the single crystal lattice of CaLaGa3O7 where they were located in Cs sites. Under excitation with ultraviolet light and a low voltage electron beam, the CaLaGa3O7:Dy3+ phosphor exhibited the characteristic emission of Dy3+ (4F9/2-6H15/2 and 4F9/2-6H13/2 transitions) with intense yellow emission at about 573 nm. The chromaticity coordinates for the phosphor were in the white region. The relevant luminescence mechanisms of the phosphor are investigated. This phosphor may be applied in both field emission displays and white light-emitting diodes.     

Synthesis and Magnetic Properties of Spin-Liquid Tb2Ti2O7

Polycrystalline samples of a novel spin-liquid compound Tb2Ti2O7 were prepared by a standard solid-state reaction. X-ray diffraction at room temperature confirms that the synthesized compound of Tb2Ti2O7 is single phase with cubic unit cell constant a0 of 1.015 44 nm. Magnetic susceptibility measurements in the temperature range between 100 and 300 K give an effective moment of 9.44 μB and Curie-Weiss temperature of 12.68 K, respectively, indicating the dominance of antiferromagnetic interactions. However, below 50 K, the magnetic behavior of Tb2Ti2O7 deviates from Curie-Weiss law, whose origin remains suspicion.     

Preparation of high emissivity NiCr<Subscript>2</Subscript>O<Subscript>4</Subscript> powders with a spinel structure by spray drying

Spray-drying was used to produce the high emissivity NiCr₂O₄ powders with a spinel structure. Preliminary investigations focused on fabricating the high emissivity powders for infrared radiation coatings and finding the relationship between microstructure and emissivity. The NiCr₂O₄ powders were characterized for composition, microstructure, and infrared emissivity by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared radiant instrument, and Fourier transform infrared spectra (FT-IR). Thermogravimetry and differential thermal analysis show that the appropriate baking temperature for NiCr₂O₄ powder preparation is about 1200°C. The emissivity measurement and FT-IR spectra show that, because of the special spinel structure, the NiCr₂O₄ powders have a high emissivity about 0.91. Spray-drying is a suitable method to produce the high emissivity ceramic powders.     

A new PAA Sol-gel method to synthesis the spinel LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> Material for Li-ion battery

A PAA sol-gel method, which is based on the chelate effect of PAA polymer, was developed for the synthesis of the spinel LiMn₂O₄ material. The pyrolysis process of the PAA-nitrate mixture precursor was investigated by TG and DTA analysis. It is found that the structure and electrochemical properties of the material are sensitive to the atmosphere employed in the synthesis process. Preliminary results show that the material thus prepared has a good electrochemical performance even at high charge and discharge current. Foundation item: Supported by the National Science Foundation of China (No. 29833090) Biography: Zhan Hui (1973-), female, Ph.D. research direction relectrochemistry.