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 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.

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 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 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.

Microwave Synthesis of Cathode Material Li_xMn_2O_4 for Lithium-ion Battery

LiMn 2O 4 was synthesized rapidly by microwave heating.The product phases of the microwave synthesis and conventional solid-state synthesis were comparatively invesitigated.The capacity of microwave synthesis product decreases relatively slow.The lithium ion can be inserted into and extracted from the spinel framework structure fluently after cycling.But the capacity of the conventional solid-state synthesis product is more remarkably lowered.The spinel framework structure was destroyed which hindered the lithium ion from inserting and extracting.The influential factors of the process parameters are discussed such as heat preservation time, pre-heating at 400℃ for 24h and coupled agent.

Microwave Synthesis and Crystal Structure of Bis{2-[(2,4-dichloro-phenylimino)methyl]-4,6-diiodo-phenol}-copper(Ⅱ)

Bis{2-[（2,4-dichloro-phenytimino）-methyl]-4,6-diiodo-phenol}-copper（II） （1） has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 14.7558（17）, b = 20.770（2）, c = 20.3260（19） A, β = 90.6110（10）°, V= 6229.2（11） A3 and Z = 8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[（2,4-diehloro-phenylimino）-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.

Microwave Synthesis and Photocatalytic Properties of CeVO 4/FeVO4 Nanocomposites

In this paper, CeVO4/FeVO4 nanocomposites were prepared by direct feeding microwave synthesis method with nine water iron nitrate (Fe(NO3)3•9H2O), cerium nitrate hexahydrate (Ce(NO3)3•6H2O) and ammonium metavanadate (NH4VO3) as raw material and Sodium Dodecyl Sulfate (SDS) as surfactant. Then X-Ray Diffractometer (XRD) and Scanning Electron Microscopy (SEM) were used to observe the CeVO4/FeVO4 nanocomposites. SEM image showed that the as-prepared CeVO4/ FeVO4 nanocomposites calcined at 773 Kis formated of small particles aggregation irregular sheet structure. We studied the photocatalytic activity of the as-prepared samples by using degradation of methyl orange in visible light. The results showed that the photocatalytic activity of CeVO4/FeVO4 nanocomposites were very well. It found that when the catalyst calcined at 773 K was 0.10 g, and 0.5 mL hydrogen peroxide joined as well as, pH was 2.0, the degradation ratio of catalyst for methylene orange of 100 mL 5 mg/L reached 98.63% in 40 min.

Microwave synthesis and enhancement of thermoelectric performance in Hf_(x)Ti_(1-x)NiSn_(0.97)Sb_(0.03)half-Heusler bulks

We obtained TiNiSn-based half-Heusler Hf_(x)Ti_(1-x)NiSn_(0.97)Sb_(0.03)bulks with 85%-96%relative densities via 5-min microwave synthesis and 20-min microwave sintering in sealed vacuum.The phase composition and microstructure of samples were characterized by X-ray diffractometer(XRD)and scanning electron microscopy(SEM).Thermoelectric(TE)properties were measured,i.e.,Seebeck coefficient(S),electrical resistivity(ρ),and thermal conductivity(κ)through Seebeck coefficient/resistance analysis system(S/RAs)and laser flash thermal analyzer(LFT).The results show that the nearly single phase exists after microwave sintering.The grain sizes and the number of grain boundaries decrease with increase in Hf-doping amount due to an increase in point defects.The matrix grains for Hf_(0.1)Ti_(0.9)NiSn_(0.97)Sb_(0.03)are~10μm.The nanoscle pores and precipitates are present as second phases in matrix grain.The real composition for Hf_(0.1)Ti_(0.9)NiSn_(0.97)Sb_(0.03)matrix grain is Hf_(3.51)Ti_(28.76)-Ni_(34.76)Sn_(31.55)Sb_(1.43).The variation trends of electrical resistivity,Seebeck coefficient,power factor,and thermal conductivity were analyzed in detail.The maximum figure of merit(ZT)of 0.46 is obtained for Hf_(0.1)Ti_(0.9-)NiSnSn_(0.97)Sb_(0.03)at 723 K.The innovation route exhibits advantages for predation of TE bulks when compared to the conventional methods,especially in terms of efficiency while it still maintains TE performance.

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-

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.

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.

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.

Microwave synthesis of single-phase nanoparticles made of multiprincipal element alloys

Metal nanoparticles of multi-principal element alloys(MPEA)with a single crystalline phase have been synthesized by flash heating/cooling of nanosized metals encapsulated in micelle vesicles dispersed in an oil phase(e.g.,cyclohexane).Flash heating is realized by selective absorption of a microwave pulse in metals to rapidly heat metals into uniform melts.The oil phase barely absorbs microwave and maintains the low temperature,which can rapidly quench the high-temperature metal melts to enable the flash cooling process.The precursor ions of four metals,including Au,Pt,Pd,and Cu,can be simultaneously reduced by hydrazine in the aqueous solution encapsulated in the micelle vesicles.The resulting metals efficiently absorb microwave energy to locally reach a temperature high enough to melt themselves into a uniform mixture.The duration of microwave pulse is crucial to ensure the reduced metals mix uniformly,while the temperature of oil phase is still low to rapidly quench the metals and freeze the single-phase crystalline lattices in alloy nanoparticles.The microwave-enabled flash heating/cooling provides a new method to synthesize single-phase MPEA nanoparticles of many metal combinations when the appropriate water-in-oil micelle systems and the appropriate reduction reactions of metal precursors are available.

Microwave Accelerated Synthesis of 2,2',3,3'-Biphenyltetracarboxylic Dianhydride

Polyimides have been widely used in aerospace and mi- croelectronics due to their excellent mechanical properties and thermo oxidative stability^[1]. However, most of aromatic polyi- mides are severe difficult to process because of their bad solu- bility in common solvents and intractable in their fully imidized forms, which restrict their applications and developments^[2,3]. Therefore, many investigations were focused on improving the dissolvability of polyimides and it was found that the excellent solubilizing units could be obtained from substituted biphenyls^[4-7]. Biphenyltetracarboxylic dianhydrides（BPDAs） are the most important monomers for the synthesis of these compounds. Among them, the synthesis of 2,3,3＇,4＇-/3,3＇,4,4＇- biphenyltetracarboxylic dianhydride has been widely investi- gated, but only a few literatures reported the synthesis of 2,2＇,3,3＇-biphenyltetracarboxylic dianhydride（i-BPDA）^[8-10].

Space-confined microwave synthesis of ternary-layered BiOCl crystals with high-performance ultraviolet photodetection

In recent years,two-dimensional(2D)ternary materials have attracted wide attention due to their novel properties which can be achieved by regulating their chemical composition with a very great degree of freedom and adjustable space.However,as for the precise synthesis of 2D ternary materials,great challenges still lie ahead that hinder their further development.In this work,we demonstrated a simple and reliable approach to synthesize 2D ternary-layered BiOCl crystals through a microwave-assisted space-confined process in a short time(<3 minutes).Their ultraviolet(UV)detection performance was analyzed systematically.The photodetectors based on the as-obtained BiOCl platelets demonstrate high sensitivity to 266-nm laser illumination.The responsivity is calculated to be8 A/W and the response time is up to be18 ps.On the other hand,the device is quite stable after being exposed in the ambient air within 3 weeks and the response is almost unchanged during the measurement.The facile and fast synthesis of single crystalline BiOCl platelets and its high sensitivity to UV light irradiation indicate the potential optoelectronic applications of 2D BiOCl photodetectors.

Single Step Microwave Assisted Synthesis and Antimicrobial Activity of Silver, Copper and Silver-Copper Nanoparticles

Copper and silver nanoparticles were synthesized and characterized in two minutes at 175°C in a one-step synthesis using a modified polyol (ethylene glycol) method and a microwave heating process. We successfully synthesized spherical Silver (Ag) and Copper nanoparticles (CuNP) with a crystallite size of less than 10 nm, as well as irregular silver-copper nanoparticles (AgCuNP) with a crystallite size of less than 15 nm, as confirmed by X-Ray Diffraction (XRD) and High-Resolution Transmission Electron Microscopy (HRTEM). The successful synthesis of AgCuNP with 1:1 molar ratio and constituted by 51.74% of copper and 48.26% of silver was corroborated using the Energy Dispersive X-ray (EDX) mapping technique. The AgNP and AgCuNP exhibited more stability in suspension, in comparison to CuNP, as observed by continuously monitoring the absorbance with UV-Vis spectroscopy for 12 days. Furthermore, the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of AgNP, CuNP, and AgCuNP were determined, against Gram-negative and Gram-positive bacteria, and yeast. The obtained MIC and MBC values indicate that AgCu nanoparticles exhibited bactericidal properties greater than its constituents. On the contrary, antifungal activity of AgCuNP against yeast was not observed.

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

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.