Aluminum and Activated Alumina Powder Additions on Microwave Synthesis of Al_(4)SiC_(4)

Aiming at improving the properties of magnesia carbon materials,silicon aluminum carbide(Al_(4)SiC_(4))containing materials were prepared using industrial aluminum powder,silicon carbide powder,and graphite as raw materials,and activated alumina powder as an additive,mixing thoroughly,pressing into cylinders and then firing at 1200℃for 30 min in a carbon embedded atmosphere by the microwave method.The effects of the aluminum powder addition(20%and 24%,by mass)and activated alumina powder addition(0,3%,5%and 7%,by mass)on the microwave synthesis of Al_(4)SiC_(4) as well as the effect of the obtained Al_(4)SiC_(4) containing material on the properties of magnesia carbon bricks were studied.The results show that:compared with the samples with 20%aluminum powder,those with 24%aluminum powder generate more Al_(4)SiC_(4).With the activated alumina powder addition increasing from 0 to 7%,the amount of Al_(4)SiC_(4) generated increases first and then decreases.Compared with the sample without activated alumina powder,the samples with activated alumina powder show lower bulk density and higher apparent porosity.With the activated alumina powder addition increasing from 3%to 7%,the bulk density of the samples increases first and then decreases,while the apparent porosity of the samples shows an opposite trend.The optimal additions are 24%aluminum powder and 5%activated alumina powder,and Al_(4)SiC_(4) synthesized in this sample has a hexagonal plate structure.With the synthesized Al_(4)SiC_(4) containing material added,the magnesia carbon brick has slightly increased cold modulus of rupture,basically the same modulus of elasticity and improved oxidation resistance.

Microwave direct synthesis and thermoelectric properties of Mg_(2)Si by solid-state reaction

In order to reduce the oxidation and volatilization caused by Mg element in the traditional methods for synthesizing Mg2Si compounds,Mg2Si thermoelectric materials were prepared by solid state reaction and microwave radiation techniques.Structure and phase composition of the materials were investigated by X-ray diffraction.The electrical conductivity,Seebeck coefficient and thermal conductivity were measured as a function of temperature from 300 to 700 K.It is found that high purity Mg2Si powders can be obtained with excessive content of 8% Mg from the stoichiometric Mg2Si at 853 K and 2.5 kW for 30 min.A maximum dimensionless figure of merit,ZT,of about 0.13 was obtained for Mg2Si at 600 K.

Preparation and characterization of Eu^(3+)-doped CaCO_3 phosphor by microwave synthesis

A Eu^3＋-doped CaCO3 phosphor with red emission was prepared by microwave synthesis. The scanning electron microscopy （SEM） image and laser particle size analysis show that the CaCO3：Eu^3＋ particles are needle-like in the length range of 5.0-10.0 μm. The results of X-ray diffraction （XRD） analysis, Fourier transform infrared spectroscopy （FT-IR）, and Raman spectroscopy indicate that pure aragonite CaCO3：Eu^3＋ is prepared using microwave irradiation and the Eu^3＋ ion as a luminescence center inhabits the site of Ca^2＋. The photoluminescence excitation （PLE） spectrum shows that the strong broad band at around 270 nm and weak sharp lines in 300-550 nm are assigned to the charge transfer band of Eu^3＋-O^2- and intra-configurational 4f-4f transitions of Eu^3＋, respectively. The photoluminescence （PL） spectrum implies that the red luminescence can be attributed to the transitions from the ^5D0 excited level to the ^7FJ （J = 0, 1, 2, 3, 4） levels of Eu^3＋ ions with the mainly electric dipole transition ^5D0 → ^7F2 （614 and 620 nm）, and the Eu^3＋ ions prefer to occupy the low symmetric site in the crystal lattice.

Microwave synthesis of Li_2FeSiO_4 cathode materials for lithium-ion batteries

A novel synthetic method of microwave processing to prepare Li2FeSiO4 cathode materials is adopted. The Li2FeSiO4 cathode material is prepared by mechanical ball-milling and subsequent microwave processing. Olivin-type Li2FeSiO4 sample with uniform and fine particle sizes is successfully and fast synthesized by microwave heating at 700 ℃ in 12 rain. And the obtained Li2FeSiO4 materials show better electrochemical performance and microstructure than those of Li2FeSiO4 sample by the conventional solidstate reaction. ？2009 Yan Bing Cao. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

Synthesis Yttrium Aluminum Garnet Precursor via Homogeneous Precipitation under Microwave Irradiation

The lowly-agglomerated single-phase YAG nanopowders were synthesized for the first time by the microwave homogeneous precipitation in the presence of urea. The composition and transformations during calcination of YAG precursor were analyzed by IR, DTA/TG and XRD. The size and morphology of YAG powders were characterized by LD and TEM methods. Results show that amorphous precursor synthesized under [urea]/[metal ions] molar ratio of 15 crystallizes directly to single-phase YAG at 900degreesC. The size distribution and sinterability of YAG powders are obviously improved by adding (NH4)(2)SO4 into the reaction solution. YAG powders obtained from precursor with the (NH4)(2)SO4 content of 8% have good sinterability and are highly densified at a temperature of 1500degreesC

Electrical Properties and Microwave Synthesis of Mixed Rare Earth Oxide Ln_(0.7)Sr_(0.3-x)Ca_xCo_(0.9)Fe_(0.1)O_(3-δ)

In order to lower the raw materials cost and develop a novel cathode materials for intermediate temperature solid oxide fuel cell(ITSOFC), using mixed rare earth replacing the expensive pure La2O3 as the raw materials, the powders of Ln0.7Sr0.3-xCaxCo0.9Fe0.1O3-δ(Ln = the mixed rare earth, x =0.05, 0. 10, 0. 15) for the applications as the cathode materials were prepared by microwave sintering process. The crystal structure and the particles morphology of the obtained powders were characterized by XRD and SEM, the electrical conductivity of all samples sintered at 1200℃for 3 h was also measured as the function of the temperature from 100 to 800℃by DC four-probe method in air. The experimental results show that due to the influence of mixed rare earth the powders of Ln0.7Sr0.3-xCaxCo0.9Fe0.1O3-δsynthesized at 1200℃for 0.5 h with the mean particle size of 1 ~ 20μm was of perovskite and cubic fluorite phase as well a little SrO phase, the electrical conductivity of the samples decreases with the adding Ca2+ content, and are all higher than 100 S·cm -1from 500 to 700℃when x≤0.10. Ln0.7Sr0.3-xCaxCo0.9Fe0.1O3-δ. can meet the demand of the electrical properties for the cathode materials in ITSOFC.

Synthesis and thermoelectric properties of Mg_2Si_(1-x)Sn_x solid solutions by microwave irradiation

In order to reduce the oxidizing and volatilizing caused by Mg element in the traditional methods for synthesizing Mg2Sil-xSnx （x=0.2, 0.4, 0.6, 0.8） solid solutions, microwave irradiation techniques were used in preparing them as thermoelectric materials. Structure and phase composition of the obtained materials were investigated by X-ray diffraction （XRD）. The electrical conductivity, Seebeck coefficient and thermal conductivity were measured as a function of temperature from 300 to 750 K. It is found that Mg2Si1-xSnx solid solutions are well formed with excessive content of 5% （molar fraction） Mg from the stoichiometric MgESil.xSnx under microwave irradiation. A maximum dimensionless figure of merit, ZT, of about 0.26 is obtained for Mg2Si1-xSnx solid solutions at about 500 K for x=0.6.

Microwave Hydrothermal Synthesis PZT of Nanometer Crystal

It was focused on the applications and developments of microwave hydrothermal synthesis piezoelectric ceramic powder. The microwave hydrothermal vessel was designed and manufactured. The microwave hydrothermal synthesis system was established and the PZT piezoelectric ceramic powder was synthesized. XRD and TEM have been used to characterize the products in detail. The diameter of the PZT powder particle is from 40 to 60 nm.

The Use of Microwave Irradiation for the Rapid Organic Synthesis

Introduction With the development of scientific technology, people continuously search for new methods which can accelerate reactions. Nowadays as a new technology, microwave irradiation has gained much practical importance in chemical reactions. Microwave irradiation has been applied successfully to the areas, such as inorganic synthesis, the prepara-

Rapid Synthesis of Submicrometer-sized Red Phosphor CaS∶Cu^+,Eu^( 2+) in a Microwave Field

The red phosphor materials CaS∶Cu+,Eu 2+ were firstly synthesized in a microwave field, and characterized by XRD、SEM、fluorescent spectroscopy. The experimental results of XRD and SEM show that the phosphors of CaS∶Cu+,Eu 2+ possess a spherical crystallite structure, in the submicrometer(250～500 nm) size range. Compared to the conventional high temperature solid state reaction this new synthetic technique exhibits interesting features, such as rapid reactions without other protective atmosphere,phosphors with high purity, smaller particles,and higher efficient luminescence.

Microwave assisted synthesis, spectroscopic, thermal, and antifungal studies of some lanthanide(Ⅲ) complexes with a heterocyclic bishydrazone

A bishydrazone formed by the condensation of isatinmonohydrazone and salicylaldehyde reacted with lanthanide（Ⅲ） chloride to form complexes of the type [Ln（HISA）2Cl3], where, Ln=La（Ⅲ）, Ce（Ⅲ）, Pr（Ⅲ）, Nd（Ⅲ）, Sm（Ⅲ）, Eu（Ⅲ）, or Gd（Ⅲ） and HISA= [（2-hydroxybenzaldehyde）-3-isatin]bishydrazone. Both reactions were carried out under microwave conditions. The ligand and the metal complexes were characterized on the basis of elemental analysis, molar conductance, magnetic susceptibility measurements, UV visible, infrared, far infrared, and proton NMR spectral data. The ligand acted as neutral tridentate, coordinating through the carbonyl oxygen, azomethine nitrogen, and phenolic oxygen without deprotonation. The ligand and lanthanum（Ⅲ） complex were subjected to X-ray diffraction studies. The X-ray diffraction pattern of ligand exhibited its crystalline nature and that of the lanthanum（Ⅲ） complex indicated its amorphous character. The thermal decomposition behaviour of the complex, [La（HISA）2Cl3], was examined in the temperature range of 40-800 ℃ using TG, DTG, and DTA. The ligand and the metal complexes were screened for their antifungal activities.

Rapid preparation of Mg(B_(1-x)C_x)_2 superconductor using hybrid microwave method

The crystal structure and the superconductivity for samples Mg（B1-xCx）2 （0〈 x 〈0.09） prepared by a hybrid microwave synthesis have been investigated. The starting material B10C is also obtained by using the microwave method. The carbon can distribute uniformly in the Mg（B1-xCx）2 samples because boron and carbon are mixed on an atomic scale in the staring material B10C. The dependences of both lattice parameters and superconducting transition temperature Tc on carbon content accord with those reported in the literature. The upper critical field He2 at 20 K can be enhanced from about 4.3 T for x = 0 to 10 T for x = 0.05. The critical current density Jc of Mg（B0.95 C0.05）2 is 1.05×10^4 A/cm^2 at 20 K and 1 T.

A convenient microwave-assisted synthesis of cinchona alkaloid-derived ligands

An efficient synthesis of cinchona alkaloid-derived ligands based on solvent-free microwave-assisted reaction was described. The coupling of 1,4-dichlorophthalazine or 3,6-dichloropyridazine with quinine, cinchonine or cinchonidine provide bis-or monocinchona alkaloid-derived ligands in moderate to good yields （52-89%） within 15 min under optimum microwave conditions.

Structure and electrochemical properties of LiCoO_2 synthesized by microwave heating

Microwave synthesis method was applied to the fast preparation of LiCoO2. The structure of the synthesized oxides was analyzed by using X-ray diffraction. Only single-phase LiCoO2 was obtained. Electrochemical behaviors of LiCoO2 were investigated by charge-discharge cycling properties in the voltage range of 3.004.35 V（（vs Li）.） The results show that the prepared LiCoO2 powders calcinated at 900 ℃ for 120 min exhibit an initial charge and discharge capacity of 168 and 162 mA·h·g-1 at 0.1C current rate, respectively, as compared to 159 and 154 (mA·h·g-1) of LiCoO2 synthesized by conventional means. In addition, more than 95% of the capacity is retained （even） after 10 cycles. But with the increase of calcinating time, its electrochemical properties deteriorate. Compared with the conventional method, the microwave heating method is simple, fast, and with high energy efficiency.

Microwave Synthesis of Silver Nanoparticles Using Different Pentose Carbohydrates as Reducing Agents

A fast, green and readily reproducible microwave-based method for the production of high quality silver nanoparticles （AgNPs） in high yield is presented. Starch is used as a stabilizing agent with few pentose different reducing carbohydrates as D-ribose, D-arabinose and L-arabinose. From the UV-vis peak profile spectra of the solutions of the silver nanoparticles, the authors have investigated the size of the NPs together with the average diameter, shape, and aggregation state of the colloidal AgNPs. TEM measurements and EDX analysis have confirmed the morphology of our AgNPs.

Microwave Synthesis of CdTe/TGA Quantum Dots and Their Thermodynamic Interaction with Bovine Serum Albumin

The thioglycollic acid（TGA） as a capping agent, CdTe/TGA quantum dots（QDs） with excellent properties were synthesized under microwave irradiation. The TGA/Cd/Te molar ratios, reaction time, temperature and p H are the crucial factors for properties of QDs. The QDs were characterized by UVvis absorption and fluorescence spectra, transmission electron microscopy and Fourier transform infrared spectroscopy. The experimental results show that when the p H value is 11.5 and molar ratio of TGA：Cd：Te is 1.2：1：0.4 at 100 ℃ heating for 15 min, the resulted QDs exhibit a high fluorescence quantum yield of 78%. The fluorescence full width at half maximum（FHMW） of QDs is around 23 nm. The products are spherical with average size of 3-5 nm. There is a strong coordination effect between TGA and Cd2＋. Moreover, the results of interaction between as-made QDs and bovine serum albumin（BSA） suggest that the QDs-BSA binding reaction is a static quenching. The negative values of free energy（△G〈0） suggest that the binding process is spontaneous, △H〈0 and △S〈0 show that hydrogen bonds and van der Waals interactions play a major role in the binding reaction between QDs and BSA.

The Microwave Synthesis and Photocatalytic Activity of W6+-Doped TiO2 Nanocomposite

W6+-doped TiO2 was prepared by sodium tungsten (VI) and titanium sulfate with sodium dodecyl sulfate as surfactant under microwave irradiation. The samples were characterized by X-ray diffraction (XRD) and Scanning electron micrograph (SEM). The results showed that the as-prepared nanocomposite of inventory molar ratio of 2% calcined at 500°C for 2 h was anatase. The SEM showed that the majority of the catalyst was a relatively flake structure, and some fine particles attached to it. We also studied the photocatalytic activity of the as-prepared samples by using degradation of methyl orange. The factors including inventory molar ratio and concentration of W6+-doped, calcined temperature, amount of hydrogen peroxide and acidity of solution were investigated. When the catalyst was 1.0 g/L, pH was 2, C(H2O2) was 3 mL/L, the degradation rate of TiO2 for methyl orange of 20 mg/L reached 79.63% in 40 min.

Microwave assisted synthesis,spectroscopy and biochemical aspects of lanthanum(Ⅲ) and praseodymium(Ⅲ) complexes with oxadiazole functionalised dithiocarbazinates

The new lanthanum (Ⅲ) and praseodymium (Ⅲ) complexes of the general formula [Ln(L)3] (Ln=La(Ⅲ) or Pr(Ⅲ); LK=potassium salt of dithiocarbazinates) were prepared by both, conventional thermal and by the use of microwave technology. Elemental analyses, electrical conductance, magnetic moment and electronic, infrared, far-infrared, 1H and 13C NMR spectral studies were used to characterize the complexes. The molecular weights of few complexes were determined by FAB-mass spectra. Nephelauxetic ratio, covalency parameter and bonding parameter for these complexes were also calculated. The probable structures of the complexes were proposed. The antifungal and antibacterial activities of the complexes were evaluated. The activities were correlated with the structures of the compounds.

Microwave synthesis of La_(1-x)Sr_xCo_(1-y)Fe_yO_3 cathode materials for solid oxide fuel cells

La1-xSrxCo1-yFeyO3 cathode materials for solid oxide fuel cells were prepared by the microwave synthesis method.The reaction mechanism was studied using a thermal analysis method.The influences of microwave synthesis conditions were examined and the characteristics of the samples were determined by X-ray diffraction and scanning electron microscopy.It was found that the optimum conditions were the microwave power of 800 W and the reaction time of 40 min.Samples with perosvkite-type crystal structure were obtained.The samples consist of uniformly distributed internal particles and the particle size is less than 1 μm.

Synthesis of Phosphors(Ce_(0.67)Tb_(0.33))MgAl_(11)O_(19) and BaMgAl_(10)O_(17)∶Eu^(2+) by Microwave Irradiation Technique and Their Luminescent Properties

The phosphors(Ce 0 67 Tb 0 33 )MgAl 11 O 19 (P G) and BaMgAl 10 O 17 ∶Eu 2+ (P B) have been synthesized using the microwave irradiation technique. The data of X ray powder diffraction( d values and I/I 0 values) are basically coincided with the data of JCPDF 36 73 and 26 163 cards. The calculated cell dimensions are a =0 5582 nm, c =2 1884 nm for P G, and a =0 5616 nm, c =2 2614 nm for P B. The excitation spectra and the emission spectra of the phosphors were measured. The chromatic coordinates are x =0 316, y =0 565 for P G, and x =0 156, y =0 106 for P B. The relative luminescent intensity is about 88%(P G) and 80%(P B), respectively, compared with the same commercial phosphors. The phosphors were also detected by scanning election microscope.