Effects of temperature and initial molar ratio of Na2O to Al2O3 on agglomeration of fine Al（OH）3 seed in synthetic Bayer solution

Fine Al(OH)3 crystals were aggregated from supersaturated aluminate solution in the batch reaction tanks. By means of laser particle size analyzer and scanning electron microscopy, the influences of temperature and initial molar ratio of Na2O to Al2O3 (αK) on agglomeration of fine seed in Bayer process were investigated. The results show that agglomeration is almost finished in 8 h, and seeds with size less than 2 μm are easily aggregated together, and almost disappear in 8 h under the optimal process condi...     

Influences of seed size and number on agglomeration in synthetic Bayer liquors

By means of Malvern laser particle size analyzer and scanning electron microscopy, the influences of seed size and number on agglomeration in Bayer process were investigated. Agglomeration is almost finished in 8 h, seeds, below 5 μm, especially below 2 μm, gather together rapidly and almost disappear in 8 h. In the same supersaturation of aluminate solution and seed size, the smaller the number of seed is, the bigger the degree of agglomeration is. With the same primary number of seed, the agglomeration of larger seed is superior to that of small seed, and the agglomeration does not happen among the coarse seeds. The agglomeration mainly happens among fine particles, and the combinations among the fine particles are unconsolidated.     

New technique of comprehensive utilization of spent Al2O3 -based catalyst

A new technology was developed to recover multiple valuable elements from the spent Al2O3-based catalyst by X-ray phase analysis and exploratory experiments. The experimental results show that in the condition of roasting temperature of 750 ℃ and roasting time of 30 min, molar ratio of Na2O to Al2O3 of 1.2, the leaching rates of alumina, vanadium and molybdenum in the spent catalyst are 97.2%, 95.8% and 98.9%, respectively. Vanadium and molybdenum in sodium aluminate solution can be recovered by precipitators A and B, and the precipitation rates of vanadium and molybdenum are 94. 8% and 92. 6%. Al（OH）3 was prepared from sodium aluminate solution in the carbonation decomposition process, and the purity of Al2O3 is 99. 9% after calcination, the recovery of alumina reaches 90. 6% in the whole process; the Ni-Co concentrate was leached by sulfuric acid, a nickel recovery of 98. 2% and cobalt recovery over 98.5% can be obtained under the experimental condition of 30% H2SO4, 80 ℃, reaction time 4 h, mass ratio of liquid to solid 8, stirring rate 800 r/min.     

Pressureless reactive sintering mechanism of nanocrystalline Bi2O3-Y2O3 solid electrolyte

The nanocrystalline Bi2O3-Y2O3 solid electrolyte material was synthesized by pressureless reactive sintering process with Bi2O3 and Y2O3 nano mixed powder as raw materials, which was prepared by a chemical coprecipitation process. The study on the behavior of nano δ-Bi2O3 formation and its grain growth showed that the solid solution reaction of Y2O3 and β-Bi2O3 to form δ-Bi2O3occurs mainly in the initial stage of sintering process, and nano δ-Bi2O3 crystal grains grow approximately following the rule of paracurve ((D-D0)2=K.t) during sintering process. After sintered at 600℃ for 2 h, the samples could reach above 96% in relative density and have dense microstructure with few remaining pores, the δ-Bi2O3 grains are less than 100 nm in size.     

Surface Modfication of Fe3O4 Nanoparticles

Nanometer particles are important portion of magnetic fluid. Fe3O4 magnetic nanoparticles were studied in this paper and the surface modification of Fe3O4 nanoparticles was investigated by a series of experiments. Fe3O4 magnetic nanoparticles were synthesized with pH value, temperature, and the dosage of surfactant. The phase, structure, size and magnetism of nanoparticles were tested by X-ray diffration （XRD）, transmission electron microscopy （TEM） and magnetic balance. On the basis of the surface modification coating mechanism, the experimental phenomena and the effects on the variation of size, magnetism and stability of Fe3O4 nanoparticles were theoretically analyzed. X-Ray diffraction spectrum and TEM photograph show that 1） the nanoparticles structure is perfect, 2） the diameter of narnoparticles is small and have good deliquescence, and 3） Sodium oleate is the anion surfactant. Therefore 1） the good condition of surface modification is in an acidic solution, 2） the best temperature of surface modification is at 80 ℃, and 3） the dosage of surfactant should be about 0.6 times of that of Fe^2＋.     

Calculation of Apparent Activation Energy of Coal Oxidation at Low Temperatures by Measuring CO Yield

By analyzing previous studies on activation energy of coal oxidation at low temperatures, a theoretical calculation model of apparent activation energy is established. Yield of CO is measured by using the characteristic detector of coal oxidation at 30-90 ℃. The impact of parameters, such as airflow and particle size, on activation energies is analyzed. Finally, agreement was obtained between activation energies and the dynamic oxygen absorbed in order to test the accuracy of the model. The results show that： 1） a positive exponential relation between concentration of CO and temperature in the process of the experiment is obtained： increases are almost identical and the initial CO is low; 2） the apparent activation energies increase gradually with the sizes of particle at the same airflow, but the gradients increase at a decreasing rate; 3） the apparent activation energies increase linearly with airflow. For the five coal particles, the differences among the energies are relatively high when the airflow was low, but the differences were low when the airflow was high; 4） the optimum sizes of particle, 0.125-0.25 ram, and the optimum volume of airflow, 100 mL/min, are determined from the model; 5） the apparent activation energies decrease with an increase in oxygen absorbed. A negative exponential relation between the two is obtained,     

Preparation and characterization of calcium aluminate by chemical synthesis

Saturated Ca（OH）2 and AlCl3 solutions were used to synthesize calcium aluminate hydrate precipitates at room temperature; high purity calcium aluminate powders with stable phases were made by calcination of the precursors at a temperature as low as 1100℃. PSD and BET analysis revealed the particles with sizes ranging from submicrometer to several micrometers and with a specific area of 13 m^2/g. The measurement of hydraulic exotherm revealed that the exothennal rate is in peak for about 2 h. The exothermal quantities are 449.24 J/g at 12 h and 488.38 J/g at 24 h. Its strength development is quick and the 1 day curing strength is almost equal to 100% of the 3 days curing strength in the mortar test.     

Design,preparation, and structure of particle preforms for Si3N4（p）/Si3N4 radome composites prepared using chemical vapor infiltration process

A particle preform was designed and prepared by conglomerating and cold-pressed process, which was condensed by chemical vapor infiltration （CVI） process to fabricate silicon nitride particles reinforced silicon nitride composites. The conglomerations are of almost sphericity after conglomerated. There are large pores among the conglomerations and small pores within themselves in the preform according to the design and the test of pore size distribution. The pore size of the preform is characterized by a double-peak distribution. The pore size distribution is influenced by conglomeration size. Large pores among the conglomerations still exist after infiltrated Si3N4 matrix. The conglomerations, however, are very compact. The CVI Si3N4 looks like cauliflowershaped structure. 2008 University of Science and Technology Beijing. All rights reserved.     

Preparation and densification of BaTiO3 nanopowder by sol—gel autoigniting synthesis

Autoigniting synthesis of gel from Ba(NO3)2,TiO(NO3)2 and C6H8O7.H2O aqueous solution was investigated at an initial temperature of 600℃ and tetragonal BaTiO3 nanopowder with particle size of 80nm was prepared.It is indicated that the specific surface area of the combustion product before and after calcination is 14.74m^2/g and 12.49m^2/g,respectively.The combustion wave is composed of solid phase reaction zone and gaseous phase flame reaction zone.The combustion flame temperature is 1123K derived from thermo couple measurement.The characteristics and densification behavior of the sol-gel autoigniting synthesized BaTiO3 nanopowder were in vestigated.     

Factors affecting ice crystal purity during freeze concentration process for urine treatment

Freeze concentration has great potential in treating wastewaters containing soluble pollutions. It is important for freeze concentration process to produce ice crystals with large size and high purity. In this work raw urines of 4660-7914 mg/L in COD, 512.71-872.41 mg/L in NH3-N and 22600-28800 μs/cm in electric conductivity were studied. Urines were frozen by a digital refrigerated circulator bath. Ice crystals were purified by ice-water steep and vacuum filtration. The COD, NH3-N, and electric conductivity levels of the melted ices were measured to reflect ice crystal purity. Effects of coolant temperature, ice crystal shape, initial solution temperature, solution concentration, ice seeding, re-crystallization process and crystallization time on ice crystal purity were analyzed. The results show that an appropriate coolant temperature, suspended ice crystals, an initial solution temperature of about 6 ℃, introduction of seed ice, addition of re-crystallization process, and crystallization time of less than 30 min are in favor of producing ice crystals with high purity. Under such conditions, more than 99 percent of inorganic salts, COD and NH3-N sources in raw urine could be removed.     

Effects of drying method on preparation of nanometer α-Al2O3

Ammonium aluminum carbonate hydroxide （AACH） precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.     

Effects of temperature and initial molar ratio of Na2O to Al2O3 on agglomeration of fine AI(OH)3 seed in synthetic Bayer solution

Fine AI(OH)3 crystals were aggregated from supersaturated aluminate solution in the batch reaction tanks.By means of laser particle size analyzer and scanning electron microscopy,the influences of temperature and initial molar ratio of Na2O to A12O3 (αK) on agglomeration of fine seed in Bayer process were investigated.The results show that agglomeration is almost finished in 8 h,and seeds with size less than 2 μm are easily aggregated together,and almost disappear in 8 h under the optimal process conditions.In the aluminate solution with the same moderate initial αK,when the reaction temperature reaches 75 ℃,the secondary nucleation does not occur,and the effect of agglomeration is better.And at the same reaction temperature,when the initial αK is 1.62,the initial supersaturation of aluminate solution is moderate,the binders on the surfaces of the seed are enough to maintain the agglomeration process,and the agglomeration degree is better.From SEM images,agglomeration mainly occurs in the fine particles,the combinations among the fine particles are loose and the new formed coarse crystal shapes are irregular.     

Luminescent properties of BaO-La2O3-B2O3 glasses with dopant

The luminescent properties of glasses synthesized in air atmosphere by conventional high temperature process were stud{ed. The emissions spectra of Eu^2 and Eu^3 were observed in BaO-La2O3-B2O3-Eu2O3 glasses.The results show that the broad emission peaks at 430 nm correspond to 5d→4f emission transition of Eu^2 , the sharp emission peaks at 592, 616, 650 and 250 nm correspond to 5^D0→1Fj(j=1--4) emission transition of Eu^3 ,respectively, which indicates that the BaO-La2O3a-B2O3-Eu2O3 glass can convert ultraviolet and green omponents of sunlight into blue and red light so as to increase the intensity of blue and red light, respectively. The luminescent in--tensity of Eu^2 increases with increasing the molar ratio of Tb^3 in BaO-La2O3-B2O3-Eu2O3a-Tb4O3 glasses, whereas the luminescent intensity of Eua^3 decreases. So the luminescent intensity of Eu(Ⅲ,Ⅱ) is influenced by Tb^3 .These phenomena can be explained by electron transfer mechanism; Eu^3 (4f6) Tb^3 (4f^8)→Eu^2 (4f′) Tb^4 (4f′). Taking advantage of the luminescent properties of BaO-La2O3-B2O3-Eu2O3 glasses, light-conversion glass for agriculture can be produced.     

Preparation of LiFePO4 for lithium ion battery using Fe2P2O7 as precursor

In order to obtain a new precursor for LiFePO4, Fe2P2O7 with high purity was prepared through solid phase reaction at 650 ℃ using starting materials of FeC2O4 and NH4H2PO4 in an argon atmosphere. Using the as-prepared Fe2P2O7, Li2CO3 and glucose as raw materials, pure LiFePO4 and LiFePO4/C composite materials were respectively synthesized by solid state reaction at 700 ℃ in an argon atmosphere. X-ray diffractometry and scanning electron microscopy（SEM） were employed to characterize the as-prepared Fe2P2O7, LiFePO4 and LiFePO4/C. The as-prepared Fe2P2O7 crystallizes in the Cl space group and belongs to β-Fe2P2O7 for crystal phase. The particle size distribution of Fe2P2O7 observed by SEM is 0.4-3.0 μm. During the Li^＋ ion chemical intercalation, radical P2O7^4- is disrupted into two PO4^3- ions in the presence of O^2-, thus providing a feasible technique to dispose this poor dissolvable pyrophosphate. LiFePO4/C composite exhibits initial charge and discharge capacities of 154 and 132 mA·h/g, respectively.     

Synthesis of γ-Al2O3 nanoparticles by chemical precipitation method

Highly pure active γ-Al₂O₃ nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al₂O₃ nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor Al(OH)₃ sols are produced by using 0.1 mol/L Al(NO₃)₃ · 9H₂O and 0.16 mol/L (NH₄)₂CO₃ · H₂O reaction solutions, according to the volume ratio 1.33, adding 0.024% (volume fraction) surfactant PEG600, and reacting at 40 °C, 1 000 r/min stirring rate for 15 min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80°C for 8 h, final calcined at 800 °C for 1 h in the air, and high purity active γ-Al₂O₃ nanoparticles can be prepared with cubic in crystal system, O _H ⁷ -FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131. 35 m²/g in BET specific surface area, 7 – 11 nm in pore diameter, and not lower than 99.93% in purity. Foundation item: Project(03JJY3015) supported by the Natural Science Foundation of Hunan Province     

Electrochemical behavior of K3Fe（CN）6 in water-in-oil microemulsion

A water-in-oil (W/O) microemulsion composed of Triton X-100, n-hexanol, n-hexane and water solution with hydrochloric acid was prepared. K₃Fe(CN)₆ was added in as a water-soluble electroactive probe, and its electrochemical behavior was investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). It is found that the H⁺ concentration of the water phase has a great effect on the conductivity of the W/O microemulsion, and hence influences the electrochemical behavior of K₃Fe(CN)₆. When the pH value of water phase is about 7, the electrical conductivity of the W/O microemulsion is only 1.2×10⁻⁶ S/cm, and K₃Fe(CN)₆ almost cannot react at the glassy carbon electrode. But when the H⁺ concentration is more than 3 mol/L, the W/O microemulsion has a good electrical conductivity and K₃Fe(CN)₆ shows good electrochemical performance in it. The results of CV and EIS studies indicate that the electrochemical behavior of Fe(CN)₆ ³⁻/Fe(CN)₆ ⁴⁻ in the W/O microemulsion is different from that in the aqueous solution. This may be due to the unique liquid structure of the W/O microemulsion and the unique mass transfer in the W/O microemulsion. Foundation item: Projects(20673036, J0830415) supported by the National Natural Science Foundation of China; Projects(05JT1026, 2007JT2013) supported by the Science Technology Project of Hunan Province, China     

Antibiotic properties of Al2O3 doping silver

The preparation technique and properties of Ag-type inorganic antibiotic material carried by Al₂O₃ were studied. The results show that the material has good antibiotic and safety properties, the acute toxicity taken by stomata is LD ₅₀>8 000 mg/kg (little and big white rats), and the normal quantity in subacute toxicity test is 80 mg/(kg · d). The better mass fraction of doping Ag₂O in antibiotic material carried by Al₂O₃ is 4%–8%, and the optimal sintering temperature is from 1 000 °C to 1 100 °C. Foundation item: Project (2002AA327090) supported by National High Technology Research and Development Program of China     

Influence on performance and structure of spinel LiMn2O4 for lithium-ion batteries by doping rare-earth Sm

The spinel LiMn₂O₄ used as cathode materials for lithium-ion batteries was synthesized by mechano-chemistry fluid activation process, and modified by doping rare-earth Sm. Thesting of X-ray diffraction, cyclic voltammograms, charge-discharge and SEM was carried out for LiMn₂O₄ cathode materials and the modified materials. The results show that the cathode materials doped rare earth Li _x Mn_2−y Sm _z O₄ (0.95⩽x⩽1.2, 0⩽y⩽0.3, 0⩽z⩽0.2) exhibit standard spinel structure, high reversibility of electrochemistry and excellent properties of charge-discharge. In EC: DMC(1 : 1)+1 mol/L LiPF₆ electrolyte with discharge capacity more than 130 mA · h/g, and its capacity is deteriorated less than 15% after 300 cycles at room temperature and less than 20% after 200 cycles at 55°C. At the same time, Crystal Field Theory was applied to explain the function and mechanism of doped rare earth element. Foundation item: Project (02JJY2081) supported by the Natural Science Foundation of Hunan Province     

Pressureless sintered 3Y-TZP/20%Al2O3 composite ceramic

Nanometer 3Y-TZP/20%Al₂O₃ (mass fraction) composite powders prepared by the chemical coprecipitation method were pressureless sintered at 1550 °C for 2 h. Effects of calcining temperatures at 800 °C, 1 000 °C, and 1 200 °C on phase structure, relative density, and Vicker’s hardness of the sintered bodies were studied. The results show that 1 000 °C was the optimal calcining temperature, and the powder calcined was composed of tetragonal zirconia with the Scherrer crystalline size of 6.3nm. The relative density was up to 98.5% under pressureless sintering, and the sintered body was t-ZrO₂ (without m-ZrO₂)+α-Al₂O₃ with the average size of 0.4 μm. Foundation item: State Key Laboratory for Powder Metallurgy(No.9706-36) Biography of the first author: YIN Bang-yao, born in 1966, majoring in advanced ceramic materials.     

Leaching kinetics of low grade zinc oxide ore in NH3-NH4Cl-H2O system

The leaching kinetics of low grade zinc oxide ore in NH3-NH4Cl-H2O system was studied. The effects of ore particle size, reaction temperature and the sum concentration of ammonium ion and ammonia on the leaching efficiency of zinc were examined. The leaching kinetics of low-grade zinc oxide ore in NH3-NH4Cl-H2O system follows the kinetic law of shrinking-core model. The results show that diffusion through the inert particle pores is the leaching kinetics rate controlling step. The calculated apparent activation energy of the process is about 7.057 kJ/mol. The leaching efficiency of zinc is 92.1% under the conditions of ore particle size of 69μm, holding at 80℃ for 60 min, sum ammonia concentration of 7.5 mol/L, the molar ratio of ammonium to ammonia being 2：1, and the ratio （g/mL） of solid to liquid being 1：10.