Effect of cobalt loading on reducibility, dispersion and crystallite size of Co／Al2O3 Fischer-Tropsch catalyst

Co/Al2O3 Fischer-Tropsch synthesis catalysts with different cobalt loadings were prepared using incipient wetness impregnation method. The effects of cobalt loading on the properties of catalysts were studied by means of X-ray diffraction (XRD), temperature programmed reduction (TPR), hydrogen temperature programmed desorption (H2-TPD) and O2 titration. Co-support compound formation can be detected in catalyst system by XRD.For the Co/Al2O3 catalysts with low cobalt loading, CoAl2O3 phase appears visibly. Two different reduction regions can be presented for Co/Al2O3 catalysts, which belong to Co3 O4 crystallites (reduction at 320 ““C) and cobalt oxidealumina interaction species (reduction at above 400℃). Increasing Co loading results in the increase of Co3 O4 crystallite size. The reduced Co/Al2O3 catalysts have two adsorption sites, and cobalt loading greatly influences the adsorption behavior. With the increase of cobalt loading, the amount of low temperature adsorption is increased, the amount of high temperature adsorption is decreased, and the percentage reduction and cobalt crystallite size are increased.     

Preparation of BN／SiO2 ceramics by PIP method

The precursor infiltration and pyrolysis(PIP) method for preparation of BN/SiO2 composites was used to improve mechanical properties, dielectric properties and feasibility of high temperature dielectric parts with large dimensions and complex shapes. In the processing procedure, the porous BN ceramic matrix was first successfully prepared by compacting the mixed powders of B and BN and then sintering them at a certain temperature under normal pressure of N2. The polycarbosilane(PCS) solution was vacuum infiltrated into porous BN ceramics at the room temperature and then at 800℃ in the air to depolimerize out amorphous SiO2, and sintered further at 1 300℃ in N2 to get BN/SiO2 composites. The microstructure of materials was studied by means of X-ray diffraction and electron probe micro analysis. The thermo-decomposition mechanism of PCS was investigated by a TG-DTA and infrared (IR) spectrum analysis. The flexural strengths were measured by the three-point bending method. The dielectric constant and the loss tangent were measured by the wave-guide method. The results show BN/SiO2 composites were fabricated. The obtained composites posses a flexural strength of 61.96 - 93.31 MPa, the dielectric constant in the range of 3.50 - 3.78 and the order of magnitude of the loss tangent at 10^-3 , which are good for the high tempera turedielectric parts with large size and complex shapes.     

Reaction products of MgO and microsilica cementitious materials at different temperatures

The paste was prepared by mixing MgO, microsilica and H2O in the presence of water reducer at different reaction ratios and temperatures, and characterized by XRD, DTA, TGA, IR, and solid-state 29Si NMR. The experimental results showed that, besides Mg(OH)2, magnesium silicate hydrate (M-S-H) was formed at a low temperature such as 25 and 50 ℃. At a high temperature of 100 ℃, Mg(OH)2 can be further transformed into M-S-H completely, for instance, within ca. 1 month in an excess of microsilica. The average composition and structure of M-S-H was mainly related to the reaction mixture and curing temperature and was discussed in detail.     

DMAc used as a reducer for preparation of spherical silver nanoparticles with high dispersion

A silver nanoparticle(Ag NP) with good monodispersity was produced by a convenient method for reducing of Ag NO3 with N, N-dimethylacetamide in the presence of polyvinyl pyrrolidone(PVP) as the surface modification agent. The shape and size of the Ag NP with reaction time were taken as variables. The surface plasmon band transition was monitored with reaction mixture time at different temperatures. The Ag NP crystallinity increases with the reaction time, and the reduction efficiency is very low when Ag NP solution is dealt at room temperature even after two days, while it is greatly improved at 160 °C only for 25 min. Ag NP modified by the as-synthesized PVP has a face-centered cubic crystalline structure, in which Ag NP could develop into a spherical morphology with a very narrow size distribution of 2-11 nm. The preparation provides a new reducing agent to form Ag NP with simpler operation and shorter time.     

ZnO films on transferable and low thermal resistance graphite substrate grown by ultrasonic spray pyrolysis

ZnO thin films were deposited on graphite substrates by ultrasonic spray pyrolysis method with Zn(CH 3 COO) 2 ·2H 2 O aqueous solution as precursor. The crystalline structure, morphology, and optical properties of the as-grown ZnO films were investigated systematically as a function of deposition temperature and growth time. Near-band edge ultraviolet(UV) emission was observed in room temperature photoluminescence spectra for the optimized samples, yet the usually observed defect related deep level emissions were nearly undetectable, indicating that high optical quality ZnO thin fi lms could be achieved via this ultrasonic spray pyrolysis method. Considering the features of transferable and low thermal resistance of the graphite substrates, the achievement will be of special interest for the development of high-power semiconductor devices with suffi cient power durability.     

Study on crystallization and microstructure of Li2O-Al2O3-SiO2 glass ceramics

Lithium aluminosilicate （LAS） glasses are generally difficult to prepare because of their high melting temperature. In this study, the preparation of LAS glasses was achieved at a relatively low melting temperature. The batch containing MgO-ZnO-LiEO- Al2O3-SiO2 was melted in a platinum crucible at 1550℃ for 2 h and was then followed by two- or three-step heat treatment processes for nucleation and crystal growth. The characterizations were carried out by differential thermal analysis, X-ray diffraction, infrared spectroscopy, scanning electron microscopy, and UV-Vis-NIR scanning spectrophotometry. The hexagonal stuffed β-eucryptite solid solution crystallized at 840-960℃. Most of the hexagonal β-eucryptite solid solution transformed into the tetragonal β-spodumene solid solution at 1100℃. Almost all the aluminum atoms entered into the tetrahedral sites in the aluminosilicate network of the 6- eucryptite/β-quartz solid solution. All of the Al atoms did not belong to the aluminosilicate network of the β-spodumene solid solution. The glass ceramic with a mean grain size of 10-20 nm is transparent, the transmittance reaches -85% in the visible light wavelength.     

Synthesis,Characterization and Formation Mechanism of Friedel’s Salt（FS:3CaO·A12O3·CaCl2·10H2O） by the Reaction of Calcium Chloride with Sodium Aluminate

The synthesis of Friedel’s salt(FS: 3Ca O·A12O3·Ca Cl2·10H2O) by the reaction of calcium chloride with sodium aluminate was investigated. Factors affecting the preparation of Friedel’s salt, such as reaction temperature, initial concentration, titration speed, aging time and molar Ca/Al ratio were studied in detail. XRD, SEM images and particle size distribution show that the reaction temperature, aging time and molar Ca/Al ratio have significant effect on the composition, crystal morphology, and average particle size of the obtained samples. In addition, the initial Ca Cl2 concentration and Na Al O2 titration speed do not significantly influence the morphology and particle size distribution of Friedel’s salt. With the optimization of the operating conditions, the crystals can grow up to a average size of about 28 um, showing flat hexagonal(or pseudohexagonal) crystal morphology. Moreover, two potential mechanisms of Friedel’s salt formation including adsorption mechanism and anion-exchange mechanism were discussed. In the adsorption mechanism, Friedel’s salt forms due to the adsorption of the bulk Cl- ions present in the solution into the interlayers of the principal layers, [Ca2Al(OH-)6·2H2O]+, in order to balance the charge. In the anion-exchange mechanism, the free-chloride ions bind with the AFm(a family of hydrated compounds found in cement) hydrates to form Friedel’s salt by anion-exchange with the ions present in the interlayers of the principal layer, [Ca2Al(OH-)6· 2H2O]+-OH-.     

Octacalcium phosphate fiber synthesized by homogeneous precipitation method

Calcium phosphate fiber was synthesized by homogeneous precipitation method using urea as precipitation agent. Effects of the reactant concentration and hydrothermal temperature on the calcium phosphate morphology and composition were studied using SEM, FTIR and XRD. It is found that fine octacalcium phosphate(OCP)fiber can be synthesized when the reactant concentrations are 0.167 mol/L for Ca(NO3)2, 0.1 mol/L for (NH4)2HPO4, and 0.6-0.7 mol/L for (NH2)2CO, respectively, with the initial reactant solution pH value around 2.2, hydrothermal temperature 90 ℃ and termination reaction at pH value around 5.0. At very low urea concentration, the product size distribution is highly inhomogeneous, however, at an excessively high concentration the product becomes larger and shorter and a mixture of OCP and hydroxyapatite (HA). Increasing the hydrothermal temperature is favorable to the fast precipitation of OCP, higher productivity and finer product.     

Magnetic Properties of γ-Fe2O3 Nanoparticles Prepared by Laser Ablation

A new method of preparing nanoparticles by pulsed-laser ablation of a tiny wire was reported, and pure maghemite （ γ-Fe2 O3 ） nanoparticles were synthesized by this method in a mixed gas flux of N2 and O2 at atmospheric pressure. The obtained γ-Fe2 O3 nanopartiles were in the range of 5 to 80 run in diameter and largely spherical in shape. Structural characteristics and morphologies of the nanoparticles were characterized by XRD and TEM , respectively. Moreover, magnetic properties of the obtained 7- Fe, O3 nanopartiles in the temperature range of 300 to 773 K were investigated. The experimental results demonstrate that the squareness value of the hysteresis loop decreases with increasing temperature. Both the coercivity and the saturation magnetization of the γ-Fe2 O3 nanoparticles show a constantly decrensing trend with increasing temperature up to the occurrerwe of the transformation from γ-Fe2O3 to α-Fe2O3. Especially, at the temperature of 773 K, the γ-Fe, O3 begins to transform to the α-Fe2 O3 phase and the hysteresis loop becomes unclosed .     

Fabrication and its characteristics of low-temperature polycrystalline silicon thin films

In order to reduce the cost of solar cells or flat-panel display, it is very important to synthesis poly-crystalline silicon films on low cost substrate such as glass at low temperature. In this work, electron cyclotron resonance (ECR) plasma enhanced chemical vapor deposition (PECVD) system was successfully applied to synthesize poly-Si thin-film on common glass substrate using H2 as the plasma source and SiH4 (Ar:SiH4=19:1) as the precursor gas at low temperature. Since the multicusp cav- ity-coupling ECR plasma source was adopted to provide active precursors, the growth temperature decreased to lower than 200℃. In the plasma, the electron temperatures kTe are ~2―3 eV and the ion temperatures kTi≤1 eV. This leads to non-remarkable ion impacts during the film deposition. The characteristic of poly-Si films was investigated. It was shown that the crystalline fraction Xc of the films can be up to 90% even deposit at room temperature, and the film was (220) preferably oriented. The growth behaviors of the film between the interface of glass and Si films were also discussed in detail.     

Conversion and reaction kinetics of coke oven gas over a commercial Fe-Mo/Al_2O_3 catalyst

Producing methanol from coke oven gas(COG) is one of the important applications of COG. Removal of sulfur from COG is a key step of this process. Conversion and reaction kinetics over a commercial Fe-Mo/Al2O3 catalyst(T-202) were studied in a continuous flow fixed bed reactor under pressures of 1.6-2.8 MPa, space time of 1.32-3.55 s and temperatures of 240-360 °C. Though the COG contains about 0.6 mol/mol H2, hydrogenation of CO and CO2 is not significant on this catalyst. The conversions of unsaturated hydrocarbons depend on their molecular structures. Diolefins and alkynes can be completely hydrogenated even at relatively low temperature and pressure. Olefins, in contrast, can only be progressively hydrogenated with increasing temperature and pressure. The hydrodesulfurization(HDS) of CS2 on this catalyst is easy. Complete conversion of CS2 was observed in the whole range of the conditions used in this work. The original COS in the COG can also be easily converted to a low level. However, its complete HDS is difficult due to the relatively high concentration of CO in the COG and due to the limitation of thermodynamics. H2 S can react with unsaturated hydrocarbons to form ethyl mercaptan and thiophene, which are then progressively hydrodesulfurized with increasing temperature and pressure. Based on the experimental observations, reaction kinetic models for the conversion of ethylene and sulfur-containing compounds were proposed; the values of the parameters in the models were obtained by regression of the experimental data.     

Super-capacitive Properties of Thick RuO2·xH2O Electrodes:Effect of Thickness,Binder and Carbon Black Addition

Hydrous ruthenium oxide,RuO2·xH2O,was synthesized through a sol-gel reaction of ruthenium chloride aqueous solution.The annealed RuO2·xH2O powders are aggregate of very small particles in nano-size of 70-80 nm and have abundant porous structure as observed by SEM.The effect of electrode thickness,PTFE binder and carbon black addition on the super-capacitive properties of thick RuO2·nH2O electrodes was investigated.At low scan rate of 5 mV/s,the specific capacitance of RuO2·xH2O (SCR,based on the weight of RuO2·xH2O only) for pure RuO2·xH2O and RuO2·xH2O-PTFE-CB electrodes can reach 665 F/g.Increasing electrode thickness and mixing PTFE into RuO2·xH2O lead to a degradation of SCR and rate capacity.By adding carbon black into RuO2·xH2O-PTFE mixture,the rate capacity of the thick electrode (RuO2·xH2O-PTFE-CB) can be improved close to the thick pure RuO2·xH2O electrode.However,mixing with PTFE and carbon black leads to a loss of the overall mass-specific capacitance.The reason for the dependence of SCR and rate capacity on electrode thickness,binder and carbon black addition was discussed based on the relation between the resistance and utilization rate of electrodes.     

Preparation and characterization of nanometer-sized barium titanate powder by complex-precursor method

A new complex-precursor method was proposed to prepare nanometer-sized BaTiO3 powder. Firstly,Ti2O（O2）2（ta）24-complex ions were prepared by the reaction of H2O2,Ti^4＋ and ta^3-（ta=[C6H6O6N]^3-） with a desirable amount of surface active agent,and then the Ba2[Ti2O（O2）2（ta）2]·2H2O precursor was obtained by reaction between [Ti2O（O2）2（ta）2]^4-and Ba^2＋. Finally,the precursor was annealed at 800 ℃ for 2 h to obtain BaTiO3 powder. The morphology,the particle size distribution,the purity and the molar ratio of Ba to Ti of BaTiO3 powder were investigated systematically by TEM,XRD,IR,Raman and chemical analysis,respectively. The results show that the BaTiO3 powders with the grain size of about 40 nm have a tetragonal crystalline structure at room temperature and a spherical morphology.     

Mixed H2/H∞ State Feedback Attitude Control of Microsatellite Based on Extended LMI Method

For the appearance of the additive perturbation of controller gain when the controller parameter has minute adjustment at the initial running stage of system,to avoid the adverse effects,this paper investigates the mixed H_2/H_∞ state feedback attitude control problem of microsatellite based on extended LMI method.Firstly,the microsatellite attitude control system is established and transformed into corresponding state space form.Then,without the equivalence restriction of the two Lyapunov variables of H_2 and H∞performance,this paper introduces additional variables to design the mixed H_2/H_∞ control method based on LMI which can also reduce the conservatives.Finally,numerical simulations are analyzed to show that the proposed method can make the satellite stable within 20 s whether there is additive perturbation of the controller gain or not.The comparative analysis of the simulation results between extended LMI method and traditional LMI method also demonstrates the effectiveness and feasibility of the proposed method in this paper.     

Chemical Synthesis and Magnetic Properties of Nanocrystalline (La_(0.67-X)Gd_X)Sr_(0.33)MnO_3 Using Amorphous Molecular Alloy as Precursors

A new route to synthesize nanosized crystalline of(La 0.67–X Gd X )Sr 0.33 MnO 3 (X=0.05,0.10, 0.15,0.20)perovskite-type complex oxides at calcination temperature of 600-1000°C using the amorphous molecular alloy as precursors was reported.The precursor could be completely decomposed into complex oxide at temperature below 500°C according to the TGA and DTA results.XRD demonstrates that the decomposed species is composed of perovskite-type structure at calcination temperature of 600°C for 2 h.The particle size that depends on the calcination temperature of the precursor is in a range of 30-120 nm as determined by transmission electron microscopy(TEM).This method is effective and can be easily quantitatively controlled to synthesize nanosized perovskite-type complex oxides.The magnetic properties of(La 0.67–X Gd X )Sr 0.33 MnO 3 nanocrystalline were preliminary studied.     

Spontaneous combustion tendency of fresh and pre-oxidized sulfide ores简

Three representative sulfide ore samples were collected from typical metal mines,and their corresponding pre-oxidized products were obtained under nature environment.The thermal behaviors of each sample at heating rates of 5,10,15 and 20 °C/min in air flow from ambient temperature to 800 °C were studied by simultaneous thermal analysis and the TG/DSC curves before and after the pre-oxidation were compared.By the peak temperature of DTG curves,the whole reaction process for each sample was divided into different stages,and the apparent activation energies were calculated by the Ozawa-Flynn-Wall method.The results show that the reaction process of each sample after pre-oxidation is more complex,with quicker reaction rates,fewer heat production quantities,and higher or lower ignition-points.The apparent activation energies decrease from 364.017-474.228 kJ/mol to 244.523- 333.161 kJ/mol.Therefore,sulfide ores are more susceptible to spontaneous combustion after the pre-oxidation.     

Effect of water washing pre-treatment on the properties of glass-ceramics from incinerator fly ash using electronic arc furnace

Production of glass-ceramics by sintering the molten slag obtained from electric arc furnace treatment of fly ash was investigated. The effect of washing pretreatment prior to melting the fly ash on the microstructure and properties of the glass-ceramics was examined. The results show that washing pretreatment of fly ash can decrease alkali metal chloride and increase network former in fly ash, which results in the increase of peak crystallization temperature of parent glass and strengthening of properties of bending strength and chemical stability of the glass-ceramics. The optimal heat treatment temperature for parent glass of washed fly ash is 1 173 K, at which the crystalline phase of glass-ceramics is composed of gelignite (Ca2Al2SiO7) and akermanite (Ca2MgSi2O7). Glass-ceramics produced at optimal heat treatment temperature are excellent in term of the physical and chemical properties and leaching characteristics, indicating attractive potential as substitute of nature materials.     

Impedance Spectroscopy of Ion Beam Mixed Cu/BaTiO_3PTCR Ceramics

The positive temperature coefficient resistance ( PTCR) barium titanate ceramic samples have been prepared by the standard solid-state reaction method, and the ceramic samples have been treated by depositing copper films with magnetron sputtering method. The metallic copper films deposited on the ceramic substrates have been mixed at room temperature with argon ions in energy of 400 keV. Ion beam mixing induced modification of PTCR behavior of the ceramics was studied by using the ac complex impedance method and the resistance vs. temperature measurements . The results showed that room temperature resistance dramatically decreased and Curie point shifted toward higher temperature side for the ion beam mixed samples.     

Reactive Hot-press Sintering of Al-B₄C Composites at Relative Low Temperature

A new process of reactive hot-press sintering with boron carbide(B4C) and aluminum powders was proposed to overcome difficulties in the sintering of dense B4C ceramic materials.The B4C powder with different content of pure metallic aluminum particle were milled,hot-pressed and sintered at 1600 ℃ for 1 hour.The mechanism of sintering at relative low temperature was analyzed.The phase constitution of the composites was determined.Effects of Al content on the hardness and fracture toughness of the composites were discussed.The results show that thermite reaction procedure in B2O3+Al was the mechanism of sintering at relative low temperature,B4C,Al2O3 and metallic aluminum are the major constituents of the composites.The microhardness of the composites decreases with the increasing of Al content,but the fracture toughness increase obviously.The composite with 5wt% Al content has the best microhardness and fracture toughness in all the composites.