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Drawbacks and Improve Ways of LiNiO2 as a Cathode Material for Lithium Ion Batteries
YE Nai-Qing,LIU Chang-Jiu,SHEN Shang-Yue
2004 Vol. 19 (6): 12171224
Abstract(
2219 )
PDF(591KB)(
2319
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As a cathode material for lithium ion batteries, LiNiO2 has various drawbacks such as difficulty to be synthesized, poor cycling performance and poor thermal stability, which are all related to its crystal structure. Stared from the crystal structure, this paper analyzed the causes that result in these drawbacks and reviewed the improve ways briefly. It was shown that just optimizing the synthesis conditions could only improve the cycling performance to a degree. In order to overcome these drawbacks thoroughly, the most important thing is to stabilize the layered structure of LiNiO2 by part substitution of suitable elements for nickel or/and oxygen.
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Development of Vanadium Oxide in Lithium Ion Batteries
CHEN Chang-Guo,LIU Yu-Ping,LI Lan
2004 Vol. 19 (6): 12251230
Abstract(
2621 )
PDF(412KB)(
1449
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The development of vanadium oxides in lithium ion batteries was summaried. The structure, synthesis methods, electrochemical performances of V2O5, V6 13, VO2, V3O7 and V6O14 in lithium ion batteries were reviewed. The reasons for V4O9, V2O3 excluded from the application in lithium ion batteries were explained. Then the advantage and problem of vanadium oxides as cathode materials of lithium ion batteries were pointed out. Finally the authors considered that those vanadium oxides could be promising as cathode materials of lithium ion batteries.
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Preparation, Properties and Application Prospects of Ferroelectic Nanomaterials
LU Sheng-Guo,LI Biao-Rong,MAK Chee-Leung,WONG Kin-Hung
2004 Vol. 19 (6): 12311239
Abstract(
3244 )
PDF(886KB)(
12968
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The preparation, structure and properties of ferroelectric nanometer sized powders, nanocomposites, and nanoceramics were introduced. The change of structure and properties caused by the reduction of particle size and pertinent mechanisms were discussed. Transparent nanocomposites were expected to be applied as the optical memories, optical computer, etc devices, while the nanoceramics can be widely used to improve the characteristic parameters of current capacitors due to the greatly enhanced dielectric permittivity, breakdown voltage, ageing-resistivity, mechanical strength, etc. Better quality of devices will be obtained by using the nanosized powders.
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Applications of Spray Pyrolysis Technique in Material Science
XU Zhi-Jun,CHU Rui-Qing,LI Guo-Rong,YIN Qing-Rui
2004 Vol. 19 (6): 12401248
Abstract(
5396 )
PDF(514KB)(
2097
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The spray pyrolysis technique is a wonderful method in material science. It possesses many advantages, such as low processing temperature, high homogeneity and purity of products, and so on. The key challenges of spray pyrolysis are control over the morphology and composition of product particles. It has been widely applied in the past few years. In this paper, the spray pyrolysis technique and the applications in production of ceramic powders, films, and fibers were briefly reviewed.
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Growth Elements and Growth Habit of Coordination Polyhedrons of TiC Crystal in Titanium Alloy
JIN Yun-Xue,LI Qing-Fen
2004 Vol. 19 (6): 12491254
Abstract(
2459 )
PDF(590KB)(
1428
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The shape of TiC can be octahedral, facet or/and non-facet dendrite in as-cast Titanium alloys. The growth element and growth habit of TiC6 in titanium alloys were analyzed with the theory of coordination polyhedron through directionally solidified samples. The results indicate that the growth elements of TiC are TiC6 with six coordinations. During the stacking of TiC6 growth element, the growth rates of families {100} and {111} are different, which may easily result in potential nuclei of octahedral TiC surrounded by {111}. During the growing of TiC in the melt, the undercooling and composition at different part of the crystal’s surface vary significantly. Some quadratic dendrites may appear in the direction of <100> and are characterized by facet growth resulting in facet dendritic TiC finally. If a large amount of defects such as screw dislocation are foed on the slowly growing surface of TiC during the growth, the facet will disappear and non-facet dendritic TiC will fo.
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Effect of Precursors on the Hydrothermal Synthesis of KAl(OH)2CO3 Powder
ZHANG Xiang-Feng,WEN Zhao-Yin,GU Zhong-Hua,XU Xiao-He,LIN Zu-Xiang
2004 Vol. 19 (6): 12551259
Abstract(
1943 )
PDF(991KB)(
1278
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KAl(OH)2CO3 powders with different morphology were synthesized by the hy-drothermal method using AlCl3·6H2O, Al(NO3)3·6H2O, Al2(SO4)3·12H2O as the precursors at 120℃ for 24h. The results show that Al(NO3)3·6H2O is the best precursor for the synthesis of KAl(OH)2CO3. The KAl(OH)2CO3 powder synthesized in the hydrothermal aqueous with NO3-concentration of 1.2mol/L possesses particle sizes of less than 20nm, slenderness ratio of less than 5 , and good size distribution.
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Preparation and Luminescence Property of (Y,Gd)2O3:Eu Nanopowder by Complex Precipitation
CHEN Ji-Yang,SHI Ying,SHI Jian-Lin
2004 Vol. 19 (6): 12601266
Abstract(
1437 )
PDF(1176KB)(
1550
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(Y,Gd)2O3:Eu phosphors were prepared by the complex precipitation processing using the mixture of ammonium water
and ammonium hydrogen carbonate as complex precipitant. TG-DSC, FT-IR, XRD, SEM, TEM were used to characterize the as prepared
phosphors. The Eu2O3 concentration and calcining temperature have distinctly influence on the X-ray excited luminescence of the as prepared
powders. The resulted (Y,Gd)2O3:Eu powder calcined at 850℃ for 2h has an average particle size of 50nm. The specific surface area
of the weakly agglomerate powder is about 23m2/g. Its X-ray excited luminescence is much stronger than that of the powder prepared by oxalate
precipitation processing.
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Preparation of Porous Glass-ceramic with Controlled Pore Size and Porosity by Adding Porosifier
HE Feng,LIU Chang-Sheng
2004 Vol. 19 (6): 12671276
Abstract(
1847 )
PDF(1581KB)(
1568
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This study presents the manufacture of highly porous biological glass-ceramic with interconnected pores by adding porosifier, and its main crystallized products are fluroapatite and wollastonite. The effects of preparation conditions involving porosifier deformation during pressing (die-pressing technique), particle size and content, and forming pressure on the resultant porosity, pore size as well as structure and mechanical properties were investigated. The experimental results demonstrate that the resultant porous glass-ceramic with a successful control of pore size and 50%~82% volume fraction porosity can be obtained. Macropores with 250~850μm diameter forming through the pyrolysis of porosifier interconnect through the holes with 50~300μm diameter in pore wall. Very little pore volume results from micropores with 2~4μm diameter because of the incomplete sintering of glass particles. Due to plastic deformation under pressure, the green body that is added plastic porosifier stearic acid is with high-strength and can be machined into complex shape, and the sintered products with flat-sphere shape macropores are with high-strength also. On the contrast, because of elastic deformation of rigid porosifier polystyrene under pressure, green body is with low-strength and can’t be machined, and the sintered products with round-sphere shape macropores are with low-strength also. The forming pressure has a strong impact on the properties of samples with plastic porosifier stearic acid, but do not influence the properties of samples with rigid porosifier polystyrene significantly. The total porosity correlates with the weight content of porosifier linearly, so the porosity and pore diameter can be controlled through controlling the porosifier size and its content. The compressive strength increases with increased porosi
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Measurement of Modulus in Ceramic Gelcasting Process by Vane Geometry
DONG Man-Jiang,ZHANG Zhao-Quan,LIU Qian,JIANG Dong-Liang
2004 Vol. 19 (6): 12771281
Abstract(
1974 )
PDF(460KB)(
1428
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A four-blade geometry test fixture was used to capture the evolution moduli of alumina suspensions in gelcasting process in oscillatory measurement. The vane geometry was treated as a couette while the test material moving with the blade formed cylinder-like shearing surface. The diameter of the cylinder was defined as effective diameter of vane and calibrated by comparing the complex modulus G* with data from parallel plate in measuring polyacrylamide solution. Test results show that the effective diameter of the shearing cylinder is smaller than the diameter of the blades . This method provides an convenient way to measure the sol-gel transition in gelcasting process.
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Mechanical Properties and Microstructure of Silicon Nitride Ceramics by Pressureless Sintering
LIU Xue-Jian,HUANG Zhi-Yong,HUANG Li-Ping,ZHANG Pei-Zhi,CHEN Xiao-Yang
2004 Vol. 19 (6): 12821286
Abstract(
2379 )
PDF(965KB)(
1429
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The mechanical properties and microstructure of silicon nitride ceramics with MgO-Al2O3-SiO2 as additives produced by pressless sintering were investigated by XRD, SEM, TEM, EDS, and HRTEM. The relationship among preparation processing, microstructure, and mechanical properties was emphatically discussed. Intensifying blend by planetary blender, silicon nitride ceramics sintered at 1780℃ for 3h has an uniform microstructure with bigger aspect ratio of elongated grains (diameter in 0.3~0.8μm, length in 3~6μm, aspect ratio in 7~10), flexure strength of 1.06GPa, HRA hardness of 92, Hv hardness of 14.2GPa, and fracture toughness of 6.6 MPa·m0.5.
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Imfluence of α-Alumina Seeds on Transformation of Aluminium Hydroxide and Morphology of Alumina Grain in Hot-Pressing
YI Zhong-Zhou,XIAO Bing,YANG Wei-You,XIE Zhi-Peng
2004 Vol. 19 (6): 12871292
Abstract(
2062 )
PDF(786KB)(
1650
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Abrasives as seeds were introduced to the starting materials of aluminium hydroxide by wet-grinding of high-purity alumina milling balls. The phase transformation from aluminium hydroxide to α-Al2O3 was completed at 1100℃ for 2h by seeds added. The size of alumina particle derived from calcined aluminium hydroxide was reduced and narrow particle size distribution was obtained with increasing amount of the seeds. Alumina grain shapes changed with the amount of introduced seeds: equiaxed grains were observed for the samples without seeds introduction, hexagonal platelets were developed after seeds addition. Finally the grain shape showed a trend to elongated grains with seed concentration up to 20wt%.
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Effects of α-Al2O3 Seeds on the Phase Transformation and Microstructure of Alumina
LI Jiang,PAN Yu-Bai,NING Jin-Wei,HUANG Li-Ping,GUO Jing-Kun
2004 Vol. 19 (6): 12931297
Abstract(
1921 )
PDF(869KB)(
1381
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Nanometer NH4Al(OH)2CO3 precursor was synthesized from NH4Al(SO4)2 and NH4HCO3. The effect of α-Al2O3 seeds (-150nm) on the phase transformation and micrograph of alumina was studied. The results show that under the conditions of adding a small quantity of α-Al2O3 seeds, the nucleating temperature can be lowered, the transition rate enhanced effectivelly, the transition of Al2O3 from θ to α phase can be completed at a lower temperature, and the grain accumulation can also be influnced to a certain extent.
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Fluorine Doping of LiNi3/8Co2/8Mn3/8O2 Cathode Material for Lithium-ion Batteries
LI Jian-Gang,WAN Chun-Rong,YANG Dong-Ping,YANG Zhang-Ping
2004 Vol. 19 (6): 12981306
Abstract(
2085 )
PDF(1053KB)(
1984
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The layered LiNi3/8Co2/8Mn3/8O2-yF_y(y=0, 0.05, 0.10, 0.20) samples were prepared by using the co-precipitated hydroxide as precursor, and characterized by means of XRD, XPS, SEM, cyclic voltammetry, charge/discharge tests, DSC etc techniques. The results show that fluorine doping can not induce the valence change of transition metal ions in LiNi3/8Co2/8Mn3/8O2-yFy samples. The samples with y=0.05, 0.10 show better cycling performance with no expense of capacity compared with undoped one, 97.5%, 96.2% capacity retention respectively after 30 cycles can be reached. The ch lattice expanding of samples with y=0.05, 0.10 reduces from 2.06% of undoped one to 1.017%, 1.018% respectively when lithium is de-intercalated, contributing to the improvement of structure stability and electrochemical cycle character. However, the sample with y=0.20 exhibits lower capacity and faster capacity fading upon cycling, due to high cation disordering and internal impedance. Fluorine doping also accelerates agglomeration of particles of the samples, enhancing operability of electrode preparation of the cathodes. In addition, fluorine-doped samples have better thermal stability than LiNi3/8Co2/8Mn3/8O2.
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Effects of Ultrasound on the Microstructure and Electrochemical Behavior of Ti/SnO2+Sb2O3/PbO2 Electrodes
WANG Ya-Qiong,TONG Hong-Yang,XU Wen-Lin,WANG Peng
2004 Vol. 19 (6): 13071312
Abstract(
1982 )
PDF(656KB)(
1433
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The morphology and microstructure of the electrodes under ultrasound were observed and analyzed by means of ESEM and XRD. The effects of ultrasonic irradiation time on the electrochemical active surface of the Ti/SnO2+Sb2O3/PbO2 electrodes in 1.0mol/L H2SO4 solutions were studied by cyclic voltammetry. The experimental results show that the ultrasound has the influence on the morphology and microstructure of the electrodes surfaces. Under ultrasound for 20min, the cyclic voltammetric peak current density is about two times as high as that of the anode without ultrasonic irradiation. The voltammetric charge of the electrodes increases firstly as the time under ultrasound increases, after ultrasonic irradiation 20min, and the voltammetric charge decreases with increasing ultrasonic irradiation time. The voltammetric charge is the highest under the condition of ultrasonic irradiation for 20min, which means that the electrochemical active surface of the electrodes is the largest at the ultrasonic irradiation time.
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0.80Pb(Mg1/3Nb2/3)O3-0.20PbTiO3 Ceramics Prepared by Semichemical Method
CUI Bin,TIAN Chang-Sheng,SHI Qi-Zhen
2004 Vol. 19 (6): 13131321
Abstract(
2156 )
PDF(761KB)(
1291
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A semichemical method (SCM) was developed for synthesizing 0.80Pb(Mg1/3Nb2/3)O3-0.20PbTiO3 (PMNT) with pure perovskite phase. The influences of the chemical reactivities of the partial starting materials, such as soluble Mg-salts instead of MgO, Pb-salts instead of PbO and Ti(OC4H9)4 instead of TiO2 and crystalline of pure perovskite phase of PMNT on the formation of perovskite phase were investigated in detail. The influences of technological parameters, such as calcining temperature, sintering temperature and soaking time, on the phase content, and dielectric properties were investigated systematically. The results show that Mg-salts are effective for the formation of perovskite phase, especially Mg(NO3)2 and/or Mg(AC)2 instead of MgO in a molecular grade. Almost pure perovskite phase can be obtained by both using Mg(NO3)2 and Ti(C4H9O)4 instead of MgO and TiO2 respectively. The optimum preparation parameters are the calcining condition of 850℃/2h and the sintering condition of 950℃/2h. The semichemical method has many advantages of not only simple preparation process, lowing calcining and sintering temperatures, shorting reacting time, but also preparing ceramics with excellent dielectric properties. The sintered ceramics having clear crystal boundaries, large-sized crystal grains and high density, and pure perovskite phase of PMNT were successfully prepared by the SCM.
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Formation and Properties of the BSTN Composite Ceramics with Perovskite and Tungsten Bronze Phases
ZHOU Zong-Hui,DU Pi-Yi,WENG Wen-Jian,HAN Gao-Rong,SHEN Ge
2004 Vol. 19 (6): 13221328
Abstract(
1848 )
PDF(306KB)(
1263
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Special compositions of Ba0.7Sr0.3·(1-y)TiO3·yNb2O5 were designed for preparing the BSTN system by the traditional ceramic method. The composite ceramics in which the two phases of the perovskite (BST) and the tungsten bronze (SBN) coexist were successfully prepared by this composition controlled in the excessiveness of some components. XRD and LCR were used to measure the structure and dielectric constants of the composite ceramics. It is found that, in the perovskite (BST) structured system of BSTN ceramics, the second phase SBN starts to appear when the excessive content of Nb2O5 is up to about 6mol%. Similarly, in the tungsten bronze (SBN) structured system, the second phase of BST can also begin to form while the excessive content of (BaO+SrO) is up to about 11mol%. However, both the perovskite and the tungsten bronze phases formed in a system exhibit the different minorities of Nb2O5 and TiO2 solved respectively with changing the excessiveness. Especially in the case of the two phases being equivalent to each other in BSTN composite ceramics, Nb2O5 is hardly to be solved into the perovskite phase due to shortage of Nb2O5 and excessiveness of TiO2 in composition. However, a few of TiO2 is easily to be solved in the tungsten bronze phase due to excessiveness of TiO2.There is a dual characteristic shown by the perovskite phase and the tungsten bronze phase in temperature dependence curve of dielectric constant in the BSTN. The Curie temperature of the tungsten bronze phase decreases with the increase in solubility of TiO2 in the phase structure. Conversely, the Curie temperature increases with increasing perovskite phase due to the primary effect of the tungsten bronze phase being restricted by a lot of perovskite. The lowest transition temperature between ferroelectric and paraelectric phases in the BSTN is at about 200℃ and it is 90℃ lower than that of the SBN without TiO2 solved in the present work.
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Effects of Sm Doping on the High Temperature Thermoelectric Properties of Ca3Co4O9+δ-based Compounds
WANG Dong-Li,CHEN Li-Dong,BAI Sheng-Qiang,LI Jian-Guo
2004 Vol. 19 (6): 13291333
Abstract(
1970 )
PDF(323KB)(
1279
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Ca3-xSmxCo4O9+δ(x=0, 0.15, 0.3 and 0.45) polycrystalline samples were prepared by using sol-gel process followed by SPS sintering. Their thermoelectric properties were carefully studied from room temperature to 1000K. The substitution of Sm for Ca results in the increase of both Seabeck coefficient and electrical resistivity, which could be attributed to the decrease of carrier concentrations. The Sm substituted samples (x=0.15, 0.3) have lower thermal conductivity than Ca3Co4O9+δ due to their lower electronic and lattice thermal conductivities. The dimensionless figure of merit ZT reaches 0.3 at 1000K for the sample of Ca2.7Sm0.3Co4O9+δ.
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Synthesis and Property of La2O3-doped MoSi2
GAO Jian-Ying,JIANG Wan,WANG Gang
2004 Vol. 19 (6): 13341338
Abstract(
1899 )
PDF(892KB)(
1282
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La2O3-doped MoSi2 was synthesized by self-propagating high-temperature synthesis. The morphology of the combustion product was investigated by using scanning electron microscopy. The fracture toughness at room temperature was measured by Anstis’ mode and the responded microstructure was analyzed by using SEM. The results show that the addition of La2O3 as a doping agent significantly influences the thermodynamics and kinetics of combustion process when compared with the combustion synthesis of molybdenum disilicide alone. The addition of La2O3 can obviously decrease the particle size of the combustion product, and the addition of La2O3 can obviously toughen the matrix.
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Dielectric Properties of Ba0.5Sr0.5TiO3 Ceramics Sintered by Pulse Electric Current Sintering
SHEN Cai,LIU Qing-Feng,LIU Qian
2004 Vol. 19 (6): 13391344
Abstract(
2188 )
PDF(961KB)(
1507
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Cu2+, La3+ and (Cu2+, La3+ ) co-doped BST ceramics were fabricated from the powder prepared by using barium nitrate, strontium nitrate, copper nitrate, lanthanum nitrate,tetra-n-butyl titanate, and ammonium hydroxide via a citrate-nitrate combustion process. Pulse electric current sintering (PECS) was carried out to obtain the compact crystalline BST. The effects of Cu2+, La3+ doping and (Cu2+, La3+) co-doping on the dielectric property of BST were investigated. It showed that Cu2+, La3+ doping and (Cu2+, La3+) co-doping in BST bulk could dramatically modify the homogeneous of grain sizes in the sintered samples. The dielectric test showed that the Cu doping decreased not only loss tangent, but also the dielectric constant, while La doping and (La, Cu) co-doping decreased the loss tangent, but increased the dielectric constant at 25℃ to some degree.
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Kinetics of Chemically Activated Combustion Synthesis α-Si3N4 under Controlled Temperature
CHEN Song-Lin,YANG Yun,LIN Zhi-Ming,LI Jiang-Tao,ZHAO Hai-Lei,SUN Jia-Lin
2004 Vol. 19 (6): 13451352
Abstract(
1938 )
PDF(480KB)(
1056
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Combustion synthesis of α-Si3N4 was carried out through a chemical activation method under controlled temperature. Temperature profile analysis was carried out to determine the kinetics of combustion synthesis of α-Si3N4. The kinetic parameters included the combustion wave velocity, the rate of temperature increase, the adiabatic temperature rise, the inert temperature rise time and the inert temperature decay time, as well as the convention ratio of Si to Si3N4. Two methods, i. e., temperature profile analysis method and wave velocity method were used to calculate the activation energy of combustion reaction of silicon in pressurized nitrogen. The kinetics analysis will provide guideline for understanding the reaction mechanism and optimizing the processing parameters.
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Preparation and Characterization of Zn and Mg Doped Bioactive Glasses
DU Rui-Lin,CHANG Jiang
2004 Vol. 19 (6): 13531358
Abstract(
2193 )
PDF(640KB)(
1764
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Mg is a modifier of Si--O network in sol-gel bioactive glasses, and Zinc is an essential trace element in human body and has a stimulatory effect on bone formation. In this work, a CaO-SiO2-P2O5 bioactive glass (58S) used as the based glass, Mg doped glass (58S0.5M) and Zn doped glass (58S0.5Z) were prepared by the sol-gel technique , and the phase composition and the mechanical strength of the glass cuboids were evaluated. In addition, the in vitro bioactivity of the glasses was tested by immersion in simulated body fluid (SBF). The results indicated that 58S0.5M and 58S0.5Z were all amorphous even calcined at 800℃, and the incorporation of Mg and Zn improved bending strength due to the higher bond energy of Mg--O and Zn--O as compared to Ca--O. The in vitro study showed that all glasses could induce hydroxyapatite (HA) formation, but 58S0.5M and 58S0.5Z revealed a slower deposition of HA at the early stage of the immersion. After prolonged soaking, a thick layer of HA was formed on all glasses, which suggested that Mg and Zn inhibited the HA nucleation at the early stage, but did not affect the deposition of HA in long term soaking in SBF.
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BMP Releasing Kinetics and Osteogenesis Capacity of BMP/α-Tricalcium Phosphate Bone Cement
YANG Wei-Zhong,ZHOU Da-Li,YIN Guang-Fu,YIN Shao-Ya,ZHENG Chang-Qiong,GAO Li-Da
2004 Vol. 19 (6): 13591366
Abstract(
2000 )
PDF(867KB)(
1391
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A novel BMP/α-TCP composite bone cement was developed by bone tissue engineering approach. The releasing behavior of BMP from the composite was investigated in vitro through protein releasing testing, compressive strength measurement and XRD analysis. With the help of histological study and X radiographic examination, the skull defect of rabbit was repaired by the novel composite bone cement, and α-TCP bone cement was discussed as the control. Results in simulate body environment show that the rules of BMP releasing from BMP/α-TCP composite agree with Higuchi equation, which indicate that BMP releasing accords with diffusion model. The setting time of the bone cement is not influenced by the combination of BMP and α-TCP. After BMP releasing, the compressive strength of materials increases with time, and the value reaches the level hardened pure α-TCP bone cement at fourth week. The crystalline phase of materials is transferred into hydroxyapatite (HA) with time increasing. Animal experiments confirm the strong osteogenesis capacity of the novel bone cement. Rabbit skull defect can be well healed with the materials in short period.
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Synthesis and Luminescent Properties of Eu3+ Doped Strontium Borate Phosphors
WANG Hai-Ying,WANG Ru-Ji,ZHANG Yue,LI Ya-Dong
2004 Vol. 19 (6): 13671372
Abstract(
2065 )
PDF(367KB)(
1616
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Eu3+ doped borate phosphors (SrB4O7, SrB2O4, Sr2B2O5, Sr3B2O6) were prepared by solid state reaction and sol-gel technique, respectively. The luminescent results showed that the four kinds of phosphors have different luminescent properties. The Sr2B2O5:Eu3+, Sr3B2O7:Eu3+ phosphors have the red emission at 610nm, the SrB2O4:Eu3+ phosphor has the orange emission at 593nm, however the SrB4O7:Eu3+ phosphor displays the emission peaks of Eu2+ ion, all that result from the different Eu-O coordination environment. The optimal doping concentration of phosphors is 2%.
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Encapsulation Study of Persistent Luminescent Pigment of Alkaline Earth Aluminate
LU Xing-Dong,SHU Wan-Gen,TAN Ai-Dong,ZHOU Wen-Hua
2004 Vol. 19 (6): 13731378
Abstract(
2127 )
PDF(434KB)(
1674
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Silica encapsulation was studied on the particle surface of aluminate-based luminescent pigment by using TEOS as the raw materials. The encapsulated particles were analyzed by SEM, diameter testing, BET surface area measurement and XPS, a dense SiO2 film formed on particle surface with the thickness of 14nm. The anti-water property and luminescent characteristics measurement show that encapsulated particles have a better anti-water performance and similar luminescent properties to non-encapsulated particles. Moreover, the encapsulation procedure was analyzed and the process parameters’ effect on coating film was also researched. The results show that the encapsulation procedure is actually a kind of sol-gel procedure of SiO2·nH2O on the surface of particles and its process is optimized as following: pH of encapsulation solvent is about 10, encapsulation temperature is at 80℃ and reaction time is about 3.0.
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Comparison and Discussion on the Adsorption Capacity of Several Compounds with Layered Structure
YE Ying,YANG Shui-Jie,ZHENG Li-Bo,SHEN Zhong-Yue,JI Shan-Shan,HUANG Xia
2004 Vol. 19 (6): 13791385
Abstract(
2284 )
PDF(480KB)(
1679
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Pillared montmorillonite (P-MMT), organic montmorillonite (O-MMT), layered double hydroxide (LDH) and layered double oxide (LDO) were prepared. Their adsorption performance on Cr (VI) was measured. The result shows that adsorbent capability (AC) of P-MMT and O-MMT is 8.9 and 3.7 mg/g respectively; both of them can be attributed to physical adsorption. Their surface characters, i.e., hydrophilic P-MMT versus hydrophobic O-MMT, are quite possibly responsible for the difference in AC. LDO’s AC on Cr (VI) is 73 mg/g at room temperature, much higher than that of the other materials. After the adsorption, LDO’s XRD pattern changes apparently, similar to the one of LDH. This demonstrates that LDO took anions from the solution to recover the crystal structure of LDH, and that the adsorption is chemical one. Theoretical AC of LDO on Cr (VI) calculated from the reaction formation is 152 mg/g. pH variation during the adsorption was observed. pH of the solution increased rapidly at the first few minutes, slowly from 5 to 180 minute, decreased a bit after that. The first two phases indicate the adsorbing progress, and the last one is quite possibly related with the interference of dissolved CO2. There are two ways to restrain the activity of CO2, increasing Cr (VI) content and/or decreasing CO2 content. In the solution being boiled and isolated from air, LDO’s AC on Cr (VI) can be as high as 157.1 mg/g. The part above the theoretical AC can regard as the contribution of physical adsorption.
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Deposition of High Quality TiN Thin Films with Nano-structure
YAN Peng-Xun,WU Zhi-Guo,XU Jian-Wei,ZHANG Yu-Juan,ZHANG Wei-Wei,LIU Wei-Min
2004 Vol. 19 (6): 13861390
Abstract(
2022 )
PDF(677KB)(
1426
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Nano-structure TiN thin films with excellent properties were deposited on the silicon wafer and stainless steel substrate under room temperature by a filtered cathode arc plasma technique. The structure and morphology of the films were characterized by atomic force microscopy (AFM) and small angle X-ray diffractometer (XRD), and it’s hardness and elastic mouldness were measured by nano-indenter. Research results show that the TiN thin films are highly uniform, very smooth, dense and droplet-phase-free. The average grain size of the films is 50nm, and it’s hardness is up to 50GPa that is about two times of that deposited by conventional CVD and PVD techniques. XRD analysis demonstrates that the diffraction peaks of the TiN films move to small angle, and the films display a preferred orientation along plane (111).
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Preparation and Characterization of Nanocrystalline Electrochromic NiO Thin Films Prepared by Sol-Gel Method
WANG Lian-Chao,MENG Fan-Li,SUN Yu-Feng,HUANG Xing-Jiu,LIU Jin-Huai
2004 Vol. 19 (6): 13911396
Abstract(
2332 )
PDF(652KB)(
1890
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A precursor solution was prepared by dissolving nickel chloride salt and citric acid in butanol and ethanol. The solution was refluxed under continuous stirring and adding predetermined amount of water (solution in solvent). The thin films were deposited by dip-coating methods. The thin films were analyzed by TG, DSC, TEM, SEM, XRD and cyclic voltammetry. The influence of heat treatment temperature on film transmittance in the range of 350 nm to 850 nm was discussed. Results show that the thin film can transform from amorphous into cubic-NiO nanocrystalline by means of heat treatment. The results of cyclic voltammetry of the films, carried out in an electrochemical cell with three electrodes and 0.1mol/L KOH electrolyte ,show that the NiO thin film treated at 350℃ for 30min has a good electrochromic performance. As given voltage, the films reversibly change their colors from transparent to brown, and their transmittance can modulate from 80% to 30%. The cyclic voltammeter results also show that the film is quick to reach its electrochromic stable condition.
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Synthesis and Hydrophilicity of TiO2 Thin Films from Aqueous TiOSO4 Solution
LUO Zhong-Kuan,SONG Li-Xin,LI Ming,LIU Jian-Hong,CAI Hong-Hua
2004 Vol. 19 (6): 13971401
Abstract(
1895 )
PDF(533KB)(
1618
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TiO2 thin films synthesized from aqueous TiOSO4 solution were characterized by X-ray diffractometry (XRD), atomic force microscopy (AFM) and UV-Vis transmittance measurements. The photoinduced hydrophilicity of the TiO2 thin films was investigated. Results show that the as-synthesized TiO2 thin films have good hydrophilicity; the hydrophilicity can be improved by increasing annealing temperatures at 100-500℃.
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Highly Crystalline AlN Particles Synthesised by SHS Method
FU Ren-Li,CHEN Ke-Xin,ZHOU He-Ping,Ferreira J. M. F
2004 Vol. 19 (6): 14021406
Abstract(
2038 )
PDF(693KB)(
1077
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Aluminium nitride (AlN) powders were prepared by self-propagating high-temperature synthesis (SHS). Aluminium and AlN powder mixtures with weight ratios of about 60/40, in the presence of 3wt% NH4F and 3wt% carbon powders were ignited in a nitrogen atmosphere of 8 MPa, resulting in highly crystalline AlN particles with regular hexagonal morphology. The microstructure development during the reaction and the influence of additives of NH4F and carbon were determined by SEM/EDS and XRD analysis of the resulting products. For the samples with NH4F and carbon, the combustion temperature could be kept on a high level for longer times compared to the sample without NH4F and carbon. This indicates that an after-burning phenomenon has occurred; Carbon apparently enhances vapour transport through a mechanism that involves reduction and then removal of the surface oxide layer of the particles during after-burning.
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Preparation and Characterization of Hollow Superparamagnetic Fe3O4 Nanospheres
MA Wen-Zhe,QIAN Xue-Feng,YIN Jie,ZHU Zi-Kang
2004 Vol. 19 (6): 14071410
Abstract(
2148 )
PDF(407KB)(
1228
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Hollow superparamagnetic Fe3O4 nanospheres were prepared by co-precipitating iron (Ⅱ) and iron (Ⅲ) chloride salts in the presence of sodium hydroxide at 80℃. Triblock copoly-mer F127 was used as template. The nanospheres were characterized by XRD and TEM. The experimental results show that the Fe3O4 hollow nanospheres are uniform and well dispersed, the diameter is from 55 to 75nm and the shell thickness is about 7nm.
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Monodentate Ligand-assisted Hydrothermal Synthesis of CdS Nanorods
NIE Qiu-Lin,YUAN Qiu-Li,XU Zhu-De
2004 Vol. 19 (6): 14111414
Abstract(
1924 )
PDF(886KB)(
1205
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Semiconductor CdS nanorods were successfully synthesized by the hydrothermal method with monodentate ligand methylamine as assistant. The obtained CdS nanorods were characterized by using TEM, XRD, Raman, and PL techniques respectively. Effects of the concentration of methylamine on the morphologies of CdS nanocrystals were investigated. It was found that CdS nanocrystals synthesized displayed nano-particle, short nanorod, and long nanorod shape when the concentration of methylamine was 1, 5, and 20wt% in the hydrothermal process, respectively. This indicated that the type of ligand, i.e. bidentate or monodentate ligand, was not the critical factor for the formation of one dimention CdS nanocrystals in the hydrothermal process. Based on the experimental results, a complex structure-controlling mechanism was proposed.
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Upconversion Luminescence Research of Er3+-doped Oxyfluoride Tellurite Glasses
XU Shi-Qing,ZHANG Jun-Jie,DAI Shi-Xun,SUN Hong-Tao,HU Li-Li,JIANG Zhong-Hong
2004 Vol. 19 (6): 14151418
Abstract(
2264 )
PDF(292KB)(
1234
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The absorption spectra and upconversion luminescence spectra of Er3+-doped oxyfluoride tellurite glasses were investigated, and upconversion luminescence mechanisms of Er3+ in oxyfluoride tellurite glasses were analyzed. The results show that the intense green (524 and 545nm) and red (655nm) emissions corresponding to the 2H9/2→4I15/2, 2H11/2→4I15/2, 4S3/2→4I15/2, and 4F9/2→4I15/2 transitions of Er3+ ions, respectively, can be simultaneously observed at room temperature under 975 nm diode laser excitation. With increasing PbF2 concentrations, the intensity for the green emissions increases slightly, while the red emission intensity enhances much larger than the green emission intensities. There are two basic upconversion mechanisms: excited state absorption and energy transfer, and a two-photon upconversion process is assigned to the intense green and red emission, respectively.
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Etching Morphology and Symmetry of TeO2 Crystal
FANG Ya-Ke,SANG Wen-Bin,MIN Jia-Hua
2004 Vol. 19 (6): 14191422
Abstract(
2050 )
PDF(376KB)(
1209
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The etching morphologies of TeO2 crystal on (110) and (001) faces were observed by means of chemical etching and analyzed with the theory of symmetry group. The morphologies of etch pits are very special compared with the tetragonal system crystal with 422 point group. The morphologies of etch pits by theoretical analysis are in conformity with the experiment. It shows that the patterns of etch pits consist of {110} planes. It is clear that the habitual plane of TeO2 crystal is {110} plane.
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Synthesis of Polycrystalline GGG by Carbonate Co-precipitation Method for Crystal Growth
PIAO Xian-Qing,LIU Jing-He,SUN Jing
2004 Vol. 19 (6): 14231426
Abstract(
2168 )
PDF(285KB)(
1190
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Gd3Ga5O12 (GGG) precursor was synthesized by a co-precipitation method using ammonium hydrogen carbonate as precipitator. TG-DTA and IR spectra indicated that the precursor was alkaline and the weight loss during calcination was 28.06%. The results of XRD analysis indicated that the polycrystalline powder was well-crystallized after calcination at 1000℃C for 3h. Compared with the solid-state reaction, the carbonate co-precipitation had the merits of short reaction period, well-crystallization, low calcining temperature, and less volatilization. As a result, the volatilization and disproportion of Gd2O3 and Ga2O3 could be well controlled during crystal growth and the optical quality of single crystal was also improved.
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Spectroscopic Properties of Cr,Yb:YAG Crystals
XU Xiao-Dong,ZHAO Zhi-Wei,SONG Ping-Xin,ZHOU Guo-Qing,DENG Pei-Zhen,XU Jun
2004 Vol. 19 (6): 14271430
Abstract(
2502 )
PDF(279KB)(
1056
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Cr,Yb:YAG laser crystals codoped with 10 at% Yb and different concentration Cr were grown by the Czochralski method. The absorption spectra, fluorescence spectra, and fluorescence lifetimes of Cr,Yb:YAG crystals were investigated at room temperature. With the increase of Cr concentration in Cr,Yb:YAG crystals, the absorption coefficient at 1.03μm increases, and the fluorescence intensity and lifetime decrease, the energy transfer efficiency from Yb3+ to Cr4+ increases and the quantum efficiency in Cr,Yb:YAG crystals decreases. The optimum Cr concentration for Cr,Yb:YAG crystals was estimated.
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Sintering of β-Si3N4 Powder Derived by SHS
JIANG Jiu-Xin,WANG Pei-Ling,CHENG Yi-Bing,CHEN Wei-Wu,ZHUANG Han-Rui,YAN Dong-Sheng
2004 Vol. 19 (6): 14311435
Abstract(
2357 )
PDF(533KB)(
1255
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The sintering of β-Si3N4 powder synthesized by self-propagating high-temperature synthesis was studied with the addition of MgO, Al2O3, Y2O3 as sintering additives. MgO was found to be the effective sintering aids, and β-Si3N4 could be densified at 1600℃ under 20MPa with the addition of 10wt% MgO. XRD results showed that the additives did not react with β-Si3N4, existing in glassy phase of the sintered sample, with the exception of Al2O3, which reacted with β-Si3N4 to form β -Sialon phase. The samples with MgO added had better mechanical properties than that of samples doped with Y2O3 and Al2O3.
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Rapid Fabrication of Nano-structured Ti5Si3-TiC Composites by Spark Plasma Sintering
WANG Lian-Jun,JIANG Wan,BAI Sheng-Qiang,WANG Gang,CHEN Li-Dong
2004 Vol. 19 (6): 14361440
Abstract(
1997 )
PDF(984KB)(
1066
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Nano Ti5Si3-TiC composites were in situ fabricated through spark plasma sintering (SPS) technique using Ti and SiC powders without any additive. The phase constituent of the samples was analyzed by X-ray diffraction techniques and microstructures were observed by scanning electron microscope and transmission electron microscope. The fracture toughness at room temperature was also measured by indentation tests. The results show that the Ti5Si3-TiC composite can be fabricated by means of the reactive sintering method in a relatively short time (8 min) and at a lower temperature (1260℃), with a fine microstructure (TiC grain size <200nm).
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Preparation and Gas-sensing Properties of Zinc Oxide Nano-powders by Microwave Hydrolysis
XU Jia-Qiang,WANG Huan-Xin,ZHANG Jian-Rong,SHEN Jia-Nian
2004 Vol. 19 (6): 14411445
Abstract(
2275 )
PDF(518KB)(
1518
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ZnO nano-powders were prepared by using microwave hydrolysis and constant temperature hydrolysis methods, using Zn(CH3COO)2·2H2O as the starting material. In order to improve gas sensitivities, ZnO nano-powders doped with Pt of Pd were also prepared by using the microwave hydrolysis method. Their phase constitution and crystal structure were characterized by TEM and XRD analyses, and their gas sensitivities were measured. results show that the microwave hydrolysis method is better than the canstant temperature hydrolysis method, for obtaining ZnO nano-powders. The ZnO nanopowders prepared by using the two methods possess higher sensitivities to ethanol and gasoline, and the ZnO nanopowders doped with Pt or Pd can enhance their selectivities to ethonal and gasoline, respectively.
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Preparation of Micro-arc Discharge Oxidized Coating on Hot-dip Aluminized Stainless Steel Sheet
YANG Zhong-Shi,JIA Jian-Feng,TIAN Jun,HE De-Yan
2004 Vol. 19 (6): 14461450
Abstract(
2488 )
PDF(479KB)(
1167
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A new method of surface treatment for austenitic stainless steel sheets was developed to improve their mechanical performance. An aluminium layer was firstly formed on the surface of stainless steel by immersing the sheet into a 760℃ molten aluminium bath for 8 min. The aluminized stainless steel sheet was then treated by micro-arc discharge oxidation. The structure of the resultant compound coating was analyzed by using X-ray diffraction, scanning electron microscopy with energy dispersive spectrometer and Vickers micro-hardness tester. The results show that a ceramic coating composed mainly of α-Al2O3 and γ-Al2O3 is formed on a medium intermetallic compound layer and the content of γ-Al2O3 is higher than that of α-Al2O3. The micro-hardness of the compound coating shows a gradation from the coating surface (800HV) to the substrate (230HV) through the medium intermetallic compound layer (250~600HV).
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