氧化镁纳米粉体的制备

以氢氧化镁和草酸为原料,通过控制实验条件制得纳米氧化镁。研究聚乙烯醇(PVA)、聚乙二醇-400,十二烷基硫酸钠和烷基磷酸酯钾盐等分散剂对氧化镁产品粒径的影响,通过X射线衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)对氧化镁产物的物相形貌进行表征。结果表明,以聚乙烯醇为分散剂,通过研磨方式合成出草酸镁前驱体,在600℃煅烧1 h,可制得粒度均匀的球形纳米氧化镁粒子。样品经XRD分析为MgO纯相,TEM图像显示制备的MgO纳米粒子粒径为10~20 nm,颗粒分布较均匀。     

Synthesis and characterization of bimodal mesoporous silica

Mesoporous silica with controllable bimodal pore size distribution was synthesized with cetyltrimethylammonium bromide (CTAB) as chemical template for small mesopores and silica gel as physical template for large mesopores. The structure of synthesized samples were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N₂ adsorption-desorption measurements. The experimental results show that bimodal mesoporous silica consists of small mesopores of about 3 nm and large mesopores of about 45 nm. The small mesopores which were formed on the external surface and pore walls of the silica gel had similar characters with those of MCM-41, while large mesopores were inherited from parent silica gel material. The pore size distribution of the synthesized silica can be adjusted by changing the relative content of TEOS and silica gel or the feeding sequence of silica gel and NH₄OH.     

Structural characteristics of spherical Ni（OH）2 and its charge／discharge process mechanism

Spherical Ni(OH)2 particles were prepared by an aqueous solution precipitation route. The structure of spherical Ni(OH)2 was investigated by scanning electron microscopy and transmission electron microscopy and compared with that of traditional Ni(OH)2. The results show that the spherical nickel hydroxide consists of Ni(OH)2 spheres with a reticulate structure of platelet-like, which is almost arranged radially and the crystalline grains intervene and connect with each other to form a three-dimensional net. The spherical Ni(OH)2 particle is full of pores,crannies between cleave planes. It is supposed that this structure is beneficial to the structural stability for the spherical particles during the charge/discharge processes and can improve the cycle life of the electrode; the pores and the crannies in spherical particles can shorten the proton diffusion distance and speed its velocity, which may result in that the local polarization is lowered. The electrochemical performances of the spherical Ni(OH)2 are improved by enhancing the conducting properties of the crystalline lattice due to its quick proton diffusion.     

Influence of zinc on electrochemical discharge activity of Mg-6%Al-5%Pb anode

Mg-6%Al-5%Pb (mass fraction) anodes with different contents of zinc were prepared by melting and casting. The electrochemical discharge behavior of these anodes in 3.5% NaCl solutions was investigated by galvanostatic test and electrochemical impedance spectroscopy (EIS). The microstructures and the corroded surfaces of these anodes were studied by scanning electron microscopy (SEM) and emission spectrum analysis (ESA). The phase structures and the corrosion products of the anodes were analyzed by X-ray diffraction (XRD). The results show that zinc promotes the grain refinement of Mg-6%Al-5%Pb anode and makes the average discharge potential of Mg-6%Al-5%Pb anode more negative during galvanostatic test. Mg-6%Al-5%Pb anode with the addition of 1% (mass fraction) zinc has the best electrochemical performance. The activation mechanism of zinc to Mg-6%Al-5%Pb anode is as follows: The hydrolyzation of dissolved Zn²⁺ ions reduces the pH value of the solution near the surface of the anode and accelerates the dissolution of Mg(OH)₂ film; The precipitated Zn(OH)₂ with similar structure as Mg(OH)₂ combines with Mg(OH)₂ film easily and makes it break down.     

Preparation of AgSnO2 composite powders by hydrothermal process

Silver-tin oxide powders were synthesized by the hydrothermal method with Ag（NH3）2^＋ solution and Na2SnO3 solution as raw materials and Na2SO3 as reductant. The precipitation conditions of Na2SnO3 solution and the reduction conditions of Ag（NH3）2^＋ were also investigated. The powders prepared were characterized by differential thermal analysis （DTA）, X-ray diffraction analysis （XRD）, scanning electron microscope （SEM） and energy spectrum analysis, The results show that pH value of the solution is a key parameter in the formation of Sn（OH）4 precipitate and the reduction reaction of Ag（NH3）2^＋ can release H^＋ ions, which results in synchronous precipitation of Sn（OH）6^2- as Sn（OH）4. The reduction of Ag（NH3）2^＋ and precipitation of Na2SnO3 occur simultaneously and the coprecipitation of silver and tin oxide is reached by the hydrothermal method. The silver-tin oxide composite powders have mainly flake shape of about 0.3 μm in thickness and there exists homogeneous distribution of tin oxide and silver in the powder synthesized.     

Glass-ceramics made from arc-melting slag of waste incineration fly ash

Grate fly ash and fluidized bed fly ash mixed with glass cullet additive respectively were melted in the electronic arc-furnace. The product, arc-melting slag, was further treated by crushing, pressing and heat treatment in order to make the glass-ceramics. The crystallization behaviors of the produced glass-ceramics were examined by differential thermal analysis (DTA), X-ray diffractometry (XRD) and scanning electron microscopy (SEM). Results show that main crystalline phase of the glass-ceramics from grate fly ash is wollastonite (CaSiO₃) with small amount of diopside (Ca(Mg,Al)(Si,Al)₂O₆), and that from fluidized bed fly ash is diopside (Ca(Mg,Al)(Si,Al)₂O₆). It is found that the glass-ceramics sintered at 850 °C and 1 000 °C from grate fly ash and fluidized bed fly ash respectively have the optimal physical, mechanical and chemical characteristics. Glass-ceramics samples, produced from incinerator fly ash with desirable properties and the low leaching concentration of heavy metals, can be the substitute of nature materials such as marble, granite and porcelain tiles.     

Preparation and optical properties of Er<Superscript>3+</Superscript>: Na<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> transparent glass-ceramics

Na₂O-Al₂O₃-SiO₂ glass-ceramics doped with Er³⁺ ions were synthesized by the conventional melt quenching technique at a low melting temperature. The samples were characterized by differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-vis-NIR scanning spectrophotometry, and fluorescence spectrometry. The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 °C for 2 h. Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu³⁺ are studied in detail.     

Facile Synthesis of 2PbCO3·Pb(OH)2 Microcrystals and Its Catalytic Behavior for Transesterification of Dimethyl Carbonate with Phenol

Polyhedron lead hydroxide carbonate （2PbCO3·Pb（OH）2 ） microcrystals have been prepared in solution phase via a facile method in the presence of surfactant cetyltrimethylammonium bromide （CTAB）. All the samples were characterized by powder X-ray diffraction ,pattern （XRD）, field-emission scanning electron mi- croscopy （FE-SEM）, high-resolution transmission electron microscopy （HRTEM）, and selected area electron diffraction （SAED）. The possible growth mechanism was discussed. 2PbCO3·Pb（OH）2 microcrystals were found to be a novel and efficient catalyst for the synthesis of diphenyl carbonate （DPC） by transesterification of dimethyl carbonate （DMC） with phenol. Compared with some other catalysts, such as AlCl3, ZnCl2, and Mg5（CO3）4（OH）2, 2PbCO3·Pb（OH）2 microcrystals are stable and show relatively high activity at low catalyst amount. When the reaction was carried out at 180 12, with a molar ratio of phenol to DMC of 2：1, a reaction time 14 h, and a catalyst amount 0.2% （molar ratio to phenol）, the selectivity of DPC and methyl phenyl carbonate （MPC） was 14.7% and 78.8%, respectively.     

Facile Synthesis of 2PbCO3·Pb(OH)2 Microcrystals and Its Catalytic Behavior for Transesterification of Dimethyl Carbonate with Phenol

Polyhedron lead hydroxide carbonate (2PbCO3·Pb(OH)2) microcrystals have been prepared in solution phase via a facile method in the presence of surfactant cetyltrimethylammonium bromide (CTAB). All the samples were characterized by powder X-ray diffraction pattern (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED). The possible growth mechanism was discussed. 2PbCO3·Pb(OH)2 microcrystals were found to be a novel and efficient catalyst for the synthesis of diphenyl carbonate (DPC) by transesterification of dimethyl carbonate (DMC) with phenol. Compared with some other catalysts, such as AlCl3, ZnCl2, and Mg5(CO3)4(OH)2, 2PbCO3·Pb(OH)2 microcrystals are stable and show relatively high activity at low catalyst amount. When the reaction was carried out at 180℃, with a molar ratio of phenol to DMC of 2:1, a reaction time 14h, and a catalyst amount 0.2% (molar ratio to phenol), the selectivity of DPC and methyl phenyl carbonate (MPC) was 14.7% and 78.8%, respectively.     

Structure and Electric Conductivity of Ce-doped Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> Electrolyte Synthesized by Reverse Titration Chemical Coprecipitation

Ce-doped Bi₂O₃ nanopowders were prepared by reverse titration chemical coprecipitation from Bi³⁺ and Ce⁴⁺ containing aqueous solution. Techniques of X-ray diffraction (XRD), transmission electron microscopic (TEM) and Fourier transform infrared spectroscopy (FTIR) were employed to characterize the as-synthesized materials. The XRD patterns indicated that the peaks can be easily indexed to β-Bi₂O₃ and no diffraction peaks of Ce or other impurity phases were detected in the prepared samples. The calculated average crystalline size decreased from 31.72 to 11.96 nm when the Ce content increased from 1 wt% to 10 wt%. The morphology changed from flake-like into the spherical-like with increase in Ce content. The electric conductivity of Ce-doped Bi₂O₃ electrolyte was also investigated by two probe DC method. Conductivity analysis exhibited that the rate of conductivity increased with increasing Ce²⁺ ratio, when the Ce concentration was up to 5 wt%, the as-synthesized Ce-doped Bi₂O₃ electrolyte showed the maximum value of conductivity(0.295 S·cm^–1).     

Synthesis of mesoporous chromium aluminophosphate (CrAlPO) via solid state reaction at low temperature

Mesoporous chromium aluminophosphate（CrAlPO）was successfully synthesized via solid state reaction（SSR）route at low temperature in the presence of a cationic surfactant cetyltrimethyl ammonium bromide（CTAB）and inorganic sources such as AlCl₃·6H₂O,CrCl₃·6H₂O and NaH₂PO₄·2H₂O.Characterizations by means of powder X-ray diffraction（XRD）,N₂ adsorption-desorption,high resolution transmission electron microscopy（HR-TEM）,scanning electron micrography（SEM）,energy dispersion spectroscopy（EDS）,thermo-gravimetry（TG）,Fourier transform infrared spectroscopy（FT-IR）,and ultraviolet visible light spectroscopy（UV-Vis）were carried out to understand both the pore characteristics and electron transition route of these obtained materials.The experimental results show that the meso-CrAlPO materials with various Cr/Al molar ratios possess a mesostructure and a specific surface area of 193 to 310 m² /g corresponding to an average pore size of 5.5 to 2.2 nm,respectively.The maxium content of Cr in meso-CrAlPO materials synthesized via SSR route can achieve 16.7wt%,being significantly higher than that of the meso-CrAlPO prepared via a conventional sol-gel route.Meanwhile,the formation mechanism of the meso-CrAlPO was also proposed.     

Preparation of Sialon powder from coal gasification slag

X-ray fluorescence spectrometry(XRF),X-ray powder diffractometry(XRD) and scanning electron microscopy(SEM) were used to characterize the chemical composition,phase constituent and microstructure of the coal gasification slag.Sialon powders were synthesized by carbothermal reduction and nitridation using the coal gasification slag as raw materials.The experimental results showed that glass and amorphous carbon were the main phases,quartz and calcite as minor crystalline phases were also presented in porous coal gasification slag.Main constituents of coal gasification slag were SiO2,Al2O3,CaO and residual carbon.Sialon powder with Ca-α-Sialon as main crystalline phase can be synthesized when coal gasification slag powders were reduced and nitrided at 1500 ℃ for 9 h using nitrogen flow of 500 ml/min.The coal gasification slag is a valuable and economic starting material for preparing Sialon powders.     

Effect of heat-treatment on crystalline phase and UV absorption of 60CeO2-40TiO2 thin films by magnetron sputtering

60CeO2-40TiO2 thin films were deposited on soda-lime silicate glass substrates by R.F. magnetron sputtering. The effects of heat-treatment on the UV-absorption of the thin films were studied on the 60CeO2-40TiO2 thin film with the largest UV cut-off wavelength. The sample films with CeO2:TiO2=60:40 were heated at 773 K, 873 K, 973 K for 30 min. These films are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy and spectrometer (XPS). XRD analysis proves that the addition of TiO2 to CeO2 changed the crystalline state of CeO2. But the UV absorption effect of CeO2-TiO2 films with CeO2 crystallite phase is inferior to that of the amorphous phase CeO2-TiO2 films. XPS analysis also indicates that the amorphous phase CeO2-TiO2 films have the most Ce3+ content in these films. Amorphous phase and crystalline phase of the CeO2-TiO2 films have different effects on UV absorption of the thin films.     

Preparation of basic magnesium carbonate and its thermal decomposition kinetics in air

The thermal decomposition process of basic magnesium carbonate was investigated. Firstly, Basic magnesium carbonate was prepared from magnesite, and the characteristics of the product were detected by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Subsequently, the thermal decomposition process of basic magnesium carbonate in air was studied by thermogravimetry-differential thermogravimetry (TG-DTG). The results of XRD confirm that the chemical composition of basic magnesium carbonate is 4MgCO₃·Mg(OH)₂·4H₂O. And the SEM images show that the sample is in sheet structure, with a diameter of 0.1–1 μm. The TG-DTG results demonstrate that there are two steps in the thermal decomposition process of basic magnesium carbonate. The apparent activation energies (E) were calculated by Flynn-Wall-Ozawa method. It is obtained from Coats-Redfern’s equation and Malek method that the mechanism functions of the two decomposition stages are D3 and A1.5, respectively. And then, the kinetic equations of the two steps were deduced as well.     

Facile synthesis of nanocrystalline Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> thin film

A novel and facile synthesis route for the manufacture of transparent and uniform self-assembled nanocrystalline Cr2O3 (nc-Cr2O3) thin films with different morphology was reported, utilizing chromium nitrate as the inorganic source and triblock copolymer F127 as the morphology-directing agent by the evaporation-induced assembly (EIA) method. X-ray powder diffraction (XRD), thermogravimetry-differential scanning calorimetry (TG-DSC), N2-sorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the as-prepared nc-Cr2O3 thin films. The Cr2O3 thin film with different morphology was obtained by changing the relative humidity. The possible formation mechanism of the nc-Cr2O3 thin films with different morphologies was discussed.     

Preparation of Bauxite Ceramic Microsphere

Ceramic microspheres were prepared by using Chinese bauxite as raw materials through the centrifugal spray drying method. The control technology of microsphere size, degree of sphericity was researched. The ceramic microspheres were sintered by a double sintering process. The microstructure and composition of ceramic microsphere were investigated by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and X-ray energy spectroscopy. The results show that the degree of sphericity of the ceramic microsphere was good and the particle size was 10-100 μm. The XRD analysis reveals that the main crystalline phase of the ceramic microsphere was a-Al2O3 and mullite （3Al2O3·2SiO2）. The product can be used as reinforced material for composite material, especially for antiskid and hard wearing aluminum alloy coating.     

Preparation of microsized single-crystalline Co_3O_4 by high-temperature hydrolysis

Microsized single-crystalline Co3O4 has been synthesized by high-temperature hydrolysis of CoCl2·2H2O at 600 °C.The samples were characterized by powder X-ray diffraction(XRD),scanning electron microscopy(SEM) and transmission electron microscopy(TEM).The results reveal that the as-prepared powders are microsized single-crystalline Co3O4 with cubic spinel structure.An increase in the high-temperature hydrolysis time results in the evolution of particle shapes from cube to quasi-sphere,and then to octahedron...     

Catalytic graphitization of Mo-B-doped polyacrylonitrile （PAN）-based carbon fibers

A novel carbon fiber pretreatment was proposed. Polyacrylonitrile (PAN)-based carbon fibers were first anodized in H₃PO₄ electrolyte to achieve an active surface, and then coated with Mo-B catalysts by immersed the carbon fibers in a uniformly dispersed Mo-B sol. The as-treated carbon fibers were then graphitized at 2 400 °C for 2 h. The structural changes were characterized by X-ray diffractometry (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and high-resolution transmission electronic microscopy (HRTEM). The results show that much better graphitization can be achieved in the presence of Mo-B, with an interlayer spacing (d ₀₀₂) of 0.335 8 nm and a crystalline size (L _c) of 28 nm.     

Structure and Properties of the Lithium Aluminosilicate Glasses with Yttria Addition

The structure and properties of lithium aluminosilicate glasses containing Y 2 O 3 were investigated by X-ray diffraction(XRD),scanning electron microscopy(SEM),differential thermal analysis (DTA)and Raman spectroscopy.Effects of yttria on the viscosity of LAS glasses were investigated,and found that the introduction of yttria effectively decreased the viscosity of LAS glasses.In Raman spectra of initial glasses it is shown the starting glasses are in almost complete disorder,since all bands are weak and broad.In the spectra of heat-treated specimens some new narrow bands appear and increase in intensity,and the frequency changes with varied yttria addition.The DTA and XRD results show that yttria controlled the crystallization of LAS glasses by increasing the crystallization peak temperature(T p ),however,the main crystalline phase of glass-ceramics wasβ-spodumene.     

Synthesis and characterization of triclinic structural LiVPO4F as possible 4.2 V cathode materials for lithium ion batteries

A potential 4.2 V cathode material LiVPO4F for lithium batteries was prepared by two-step reaction method based on a carbon-thermal reduction （CTR） process. Firstly, V2O5, NH4H2PO4 and acetylene black are reacted under an Ar atmosphere to yield VPO4. The transition-metal reduction is facilitated by the CTR based on C→CO transition. These CTR conditions favor stabilization of the vanadium as V^3＋ as well as leaving residual carbon, which is useful in the subsequent electrode processing. Secondly, VPO4 reacts with ElF to yield LiVPO4F product. The property of the LiVPO4F was investigated by X-ray diffractometry （XRD）, scanning electron microscopy （SEM） and electrochemical measurement. XRD studies show that LiVPO4F synthesized has triclinic structure（space group p I ）, isostructural with the naturally occurring mineral tavorite, EiFePO4-OH. SEM image exhibits that the particle size is about 2μm together with homogenous distribution. Electrochemical test shows that the initial discharge capacity of LiVPO4F powder is 119 mA·h/g at the rate of 0.2C with an average discharge voltage of 4.2V （vs Ei/Li^＋）, and the capacity retains 89 mA·h/g after 30 cycles.