|
Developments of Point Defects in ZnGeP2 Crystals
ZHU Chong-Qiang,YANG Chun-Hui,WANG Meng,XIA Shi-Xing,MA Tian-Hui,LU Wei-Qiang
2008 Vol. 23 (6): 10891095
Abstract(
3412 )
PDF(717KB)(
2014
)
ZnGeP2 is a nonlinear optical material which is useful for important applications in the infrared region. A serious limitation to the development of ZnGeP2-based applications is the presence of point defects in the crystals. The latest development of the point defects in ZnGeP2 is summarized in the paper. Firstly, the point defects are studied by electron paramagnetic resonance technique. The dominant point defects in ZnGeP2 are V-Zn acceptor, V0P and Ge+Zn donors, and their energy levels are E(V-Zn)=EC-(1.02±0.03)eV, E(V0P)=EV+(1.61±0.06)eV and E(Ge+Zn)=EV+(1.70±0.03)eV. In addition, the two defects V-3Ge and VPi are observed in electron irradiated and annealed ZnGeP2, respectively. Secondly, the point defects are studied simulatively by full-potential linearized muffin-tin orbital method. The results of the dominant defects and their energy levels are in agreement with the experimental evidences. However, there still exists difference between the theoretical simulation and the actual situation, some results are discrepant with the experimental conclusions. Therefore, it is important to investigate point defects by the combination of experiment and theory.
|
|
Effect of Oxygen Pressure on the Growth Behavior and Optical Properties of ZnO Films
LIU Ming,WEI Wei,QU Sheng-Wei,GU Jian-Feng,MA Chun-Yu,ZHANG Qing-Yu
2008 Vol. 23 (6): 10961100
Abstract(
3392 )
PDF(661KB)(
1941
)
Using a reactive radio-frequent magnetron sputtering method, high c-axis oriented ZnO films were deposited on Si (001) and quartz substrates under various oxygen partial pressures with a total pressure of 0.3Pa. Atomic force microscope, X-ray diffraction, UV-Visible transmission spectroscope and photoluminescence (PL) were used to study the effect of oxygen pressure on the surface morphology and optical properties of ZnO films. It is found that the films have three different growth modes in the range of oxygen pressure from 0.04Pa to 0.23Pa. The critical pressures for the transition of film growth can be taken at 0.04--0.08Pa and 0.16--0.19Pa, respectively. When the oxygen pressure is lower than 0.16Pa, the film grown along +c axis. When the oxygen pressure exceeds 0.19Pa, grains along -c axis growth are dominant in the films. With the increase of oxygen pressure, the transmittance, refraction index, optical band gap, and PL intensity increase. At the oxygen pressure of 0.19Pa, the film has a narrowest PL spectrum with a full width at half maximum of 88 meV at room temperature.
|
|
Preparation and Photoelectric Properties of Al-Ti Codoped ZnO Thin Films with [100] Preferred Orientation
JIANG Min-Hong,LIU Xin-Yu
2008 Vol. 23 (6): 11011105
Abstract(
3319 )
PDF(374KB)(
1850
)
Al-Ti codoped ZnO (ZATO) films with (100) preferred orientation were grown on the glass substrates at room temperature by RF magnetron sputtering. The Al-Ti codoped ZnO ceramic targets used for sputtering were prepared by the conventional solid-state sintering process. The growth mechanism, microstructures and surface figures of ZATO films were investigated by X-ray diffraction (XRD) and scanning electronic microscope (SEM), and its optical and electrical properties were respectively measured using a four-point probe technique and UV-756 spectrophotometer at room temperature. After the ZATO films annealed at 500℃ for 3h, the preferred growth orientation of the films changes from (002) to (100) orientation, and the optic band gap reduces from 3.29eV to 2.86eV, and the average transmittance reduces from 90% to 70%, but the room-temperature resistivity reduces from 1.89×10-2Ω·cm to 1.25×10-3 Ω·cm. And at the same time, there is a super-lattice diffraction ray in the XRD patterns of annealed the ZATO films. The photoluminescence (PL) spectra confirm that there exhibit the near-band-edge (NBE) emission peaks at 380nm, and 410nm, 564nm PL peaks of all the films. After the films are annealed at 500℃ for 3h, the strength of these PL peaks drops, but its positions change little. The above experimental mechanisms were discussed.
|
|
Preparation and Electrical Properties of LiTa3O8 Thin Films
ZHANG De-Yin,HUANG Da-Gui,LI Jin-Hua,LI Kun
2008 Vol. 23 (6): 11061110
Abstract(
3147 )
PDF(542KB)(
1704
)
A novel ferroelectric lithium tantalate LiTa3O8 thin film was prepared on Pt/Ti/SiO 2/Si substrate by sol-gel method using lithium ethoxide and tantalite ethoxide as starting materials. The structure of the LiTa3O8 film is similar to orthorhombic, which is different from LiTaO3 film based on XRD pattern. The SEM image reveals that the LiTa3O8 film crystallized at 750℃ is uniform, smooth and crack-free on the surface with thickness of 1μm. The electrical experiments show that the remanent polarization Pr and coercive field Ec of the LiTa3O8 film polarized at 450kV/cm are 9.3μC/cm2 and 126.8kV/cm, respectively; the leakage current of the LiTa3O8 film is 8.85×10-9A/cm2 at the electric field of 9.5kV/cm, lower than that of LiTaO3 film. The dielectric constant and dielectric loss of the LiTa3O8 film are 58.4 and 0.26, respectively, at frequency of 1kHz. And the crystallization temperature of sol-gel derived LiTa3O8 film is 50℃ higher than that of LiTaO3 film.
|
|
Laser Induced Change in the Electrical and Optical Properties of Amorphous Ge2Sb2Te5 Thin Films
SUN Hua-Jun,HOU Li-Song,WU Yi-Qun,WEI Jing-Song
2008 Vol. 23 (6): 11111114
Abstract(
2907 )
PDF(450KB)(
1804
)
Sheet resistance of laser-irradiated amorphous Ge2Sb2Te5 thin films prepared by magnetron sputtering were measured by the four-point probe method. With the laser power increasing, the sheet resistance undergoes an abrupt change of four orders of magnitude (107-103Ω/□) at about 580mW. X-ray diffraction studies of the three samples before, at and after the abruption point reveal the phase change process of the Ge2Sb2Te5 thin films from amorphous to crystal states. Optical constants of the three samples measured by ellipsometry have relations as follows, namorphous>nintermediate>ncrystalline, kcrystalline>kintermediate>kamorphous, αcrystalline>αintermediate>αamorphous. Based on the above results, the relationship between the electrical/optical properties and the structural state of the Ge2Sb2Te5 thin films is discussed.
|
|
Electrochemically Controlled Ion Separation Performances of Electrodeposited Nickel Hexacyanoferrate Thin Films in Alkaline Earth Metal Solution
JU Jian,HAO Xiao-Gang,ZHANG Zhong-Lin,LIU Shi-Bin,SUN Yan-Ping
2008 Vol. 23 (6): 11151120
Abstract(
3091 )
PDF(651KB)(
1816
)
Nickel hexacyanoferrate (NiHCF) thin films were synthesized on platinum substrates by cathodic deposition and the film-electrode systems were investigated as electrochemically controlled ion separation (ECIS) materials for the selective separation of alkaline earth ions in aqueous nitrate solutions. In 0.1 mol·L-1 Mg(NO3)2, Ca(NO3)2, Sr(NO3)2 and Ba(NO3)2 solutions, cyclic voltammetry (CV) was used to reversibly intercalate and deintercalate alkaline earth cations from the matrix and to investigate the electroactivity, electrochemical behavior and the loading mechanism of NiHCF film electrodes. CV and electrochemical quartz crystal microbalance (EQCM) were used to investigate the ion selectivity of the films in 0.1 mol·L-1 [Mg(NO3)2+Ba(NO3)2] mixture solution. The chemical composition and elemental valence of NiHCF films in reduced and oxidized form were also characterized by X-ray photoelectron spectroscopy (XPS). Experimental results show that the cathodically deposited NiHCF film electrodes have reversible electrochemical behavior in alkaline earth metal solution and display a high Ba2+ selectivity in Mg2+/Ba2+ mixtures. The alkaline earth metal ions can be separated effectively by ECIS processes.
|
|
Preparation of GaN Film and Investigation of Vibrational Spectrum of GaN by DFT
LI En-Ling,WANG Shan-Shan,WANG Xue-Wen
2008 Vol. 23 (6): 11211124
Abstract(
3434 )
PDF(604KB)(
1827
)
Using Ga2O3 as Ga source, the GaN films are successfully deposited on Si (111) substrates by two-step method of sol-gel and high nitridation temperature technique. The as-prepared films were confirmed as single crystalline GaN with wurtzite structure by X-ray diffraction (XRD). The dimension of GaN crystal particulates is smaller than 100nm under the observation of scanning electron microscope (SEM). Moreover, E1 (TO) vibrational mode of GaN are surveyed in IR spectrum of the GaN films. Vibrational frequency of GaN small clusters is calculated using density functional theory (DFT). The results show that the vibrational frequencies of the Ga reached clusters are close to the peaks of the phonon vibration modes of the wurtzite structure GaN, and 2200cm-1 is an intensive vibrational frequency of N--N bond stretch in N reached GaN. FTIR of the sample are analyzed in further.
|
|
Phonon Mode and Electron-phonon Coupling Strengths Controlling the Fluorescence Efficiency of Dy3+-doped Selenide Glasses
YING Xiang-Yue,NIE Qiu-Hua,DAI Shi-Xun,XU Tie-Feng,JIN Zhen-Juan
2008 Vol. 23 (6): 11251130
Abstract(
3033 )
PDF(491KB)(
1756
)
Pure and Dy3+-doped Ge30Ga5Se65 and 0.9Ge30Ga5Se65+0.1CsBr glasses were prepared by conventional melt-quenching method. The intensity parameters, spontaneous emission probability and branching ratio of Dy3+ ions in Ge30Ga5Se65+CsBr glass were calculated by Judd-Ofelt theory. The lifetime of 6H11/2 level at temperatures from 20K to 300K were measured to investigate the temperature dependence of multiphonon relaxation (MPR) rates. The influence of the local phonon mode and electron-phonon (e-p) coupling strength on the 1.72μm fluorescence efficiency of Dy3+-doped selenide glasses was investigated. The frequency of the phonon vibration is changed to 268cm-1 due to the formation of Ga-Br bonds with the addition of CsBr to selenide glasses. The values of e-p coupling strengths in Ge30Ga5Se65 and 0.9Ge30Ga5Se65+0.1CsBr glasses are 0.456 and 0.048, respectively. It is clear that the e-p coupling strengths decrease considerably with the addition of CsBr to Ge30Ga5Se65 glass. This reduced e-p coupling together with a large change in the local phonon mode result in the change of the MPR rate.
|
|
Investigation of High-energy Ball Milling of Al-Y2O3 Mixtures and Solid-state Reaction Synthesis of YAG Ceramics
LI Chang-Qing,ZHANG Ming-Fu,ZUO Hong-Bo,HAN Jie-Cai,MENG Song-He
2008 Vol. 23 (6): 11311134
Abstract(
3313 )
PDF(590KB)(
1789
)
YAG ceramics were fabricated by solid-state reaction method using high pure powders (Al, Y2O3) as starting materials. YAG ceramics were fabricated by vacuum sintering YAG compacts which were calcined from high energy milled Al-Y2O3 powders. Al-Y2O3 powders as-milled were analyzed by DTA-TG, Al-Y2O3 powders, YAG powder and YAG ceramics were characterized by XRD and SEM. The results show that Al powders in Al-Y2O3 powders oxide intensively at 569℃, and continue to react with Y2O3, YAM phase appears after calcined at 600℃, YAP phase emerges with calcination temperature increasing, YAG phase is formed at 1200℃.YAG ceramics are fabricated from YAG compact by vacuum sintering at 1750℃ for 2h, the relative density of YAG ceramics is about 98.6%, the YAG grains grow uniformly with average size of 8-10μm tested by SEM.
|
|
Fabrication of Transparent Yttria Ceramics through Gel-freezing Dry Method
HUANG Yi-Hua,JIANG Dong-Liang,ZHANG Jing-Xian,LIN Qing-Ling
2008 Vol. 23 (6): 11351140
Abstract(
3300 )
PDF(1516KB)(
1922
)
The effect of gel-freezing dry method (--50℃, 8Pa) was investigated on drying and dewatering on a yttrium hydroxynitrate precursor. Precursor through gel-freezing dry accumulated softly with a clearer card-like figure than that through traditional oven dry. After calcination at 1100℃, the powder through gel-freezing dry method has finer particles, narrower particle distribution and larger surface area than that through oven dry. After dry process, samples were sintered at 1700℃ for 4h in vacuum, transparent polycrystalline ceramics were produced with uniform rystallines. The mean size of crystallines is around 40μm. Relative density of the transparent ceramic eaches 99.6%. After milling and polishing, samples get a high in-line transmittance of 60% at 400nm wavelength, and it also gets a high in-line transmittance ultraviolet wave band, which is similar to single crystalline yttrium oxide.
|
|
Microstructure and Mechanical Properties of Textured Alumina-Zirconia Composites Prepared by Compressive Deformation
WANG Fei,ZHANG Kai-Feng,WANG Guo-Feng
2008 Vol. 23 (6): 11411146
Abstract(
3385 )
PDF(816KB)(
1717
)
3Y-ZrO2/Al2O3 fine-grained composite compacts were prepared by vacuum hot pressed sintering and then compressed at elevated temperatures. The microstructure and mechanical properties of the composites before and after deformation were investigated. Results show that the apparent textured microstructure is observed in the deformed ceramics through XRD and X-ray pole figure measurement. The maximum degree of texture reaches 7.3 times random. As the true strain increases, bending strength, fracture toughness and Vickers hardness increase up to 933.8MPa, 10.4MPa·m 1/2 and 20.4GPa, respectively. When the true strain increases to 1.72, the mechanical properties decrease to some extent. It is concluded that the texture effectively improves the mechanical properties of the composite ceramic, while the coarsening grains and big cavities formed under extremely high strain induce the decrease of mechanical properties.
|
|
Friction and Wear Resistance of Ti3SiC2-SiC Composites
ZHANG Jian-Feng,SHI Lu,WANG Lian-Jun,JIANG Wan,CHEN Li-Dong
2008 Vol. 23 (6): 11471150
Abstract(
3080 )
PDF(822KB)(
1742
)
Ti3SiC2-SiC composites were in situ fabricated by spark plasma sintering technique from the raw powders of Ti, Si, C and small amounts of Al. Pin-disk friction and wear tests were conducted on Ti3SiC2-SiC composites. Testing results indicate that the friction coefficients and wear rates decrease with the increasing SiC contents for the Ti3SiC2-SiC composites against hardened steel, which indicates that the addition of SiC improves the friction and wear resistance of Ti3SiC2-SiC composites. The friction coefficient of Ti3SiC2 is a relatively stable value ranging from 0.8 to 1.0, while that of Ti3SiC2-40vol% SiC composites displays minimum value of 0.5 at stable state. The wear rates decrease one order of magnitude for Ti3SiC2-40vol% SiC compared with monolithic Ti3SiC2. The improvement of the wear resistance of Ti3SiC2-SiC composites is due to the wear mechanism transition and good anti-oxidation of SiC.
|
|
Effect of Sintering Temperature on Microstructure and Properties of Cf/SiC Composites
DING Yu-Sheng,DONG Shao-Ming,GAO Le,HE Ping,ZHANG Xiang-Yu,JIANG Dong-Liang
2008 Vol. 23 (6): 11511154
Abstract(
3457 )
PDF(927KB)(
1789
)
Cf/SiC composites reinforced by carbon fiber were fabricated by hot-pressing. The effects of sintering temperature on the densities, microstructure and mechanical properties were studied. Densities of the Cf/SiC composites are increased with the increase of sintering temperature, and the bending strength and fracture toughness are increased with the sintering temperature increasing from 1800℃ to 1850℃, The highest bending strength and fracture toughness of the composites fabricated at 1850℃ are 500.1MPa and 16.9MPa·m 1/2, respectively. However, when the temperature increases to 1880℃, the mechanic properties of the composite decreases.
|
|
Ablation Performances of the HfC Modified Carbon/carbon Composite Integrated Throat
LI Shu-Ping,LI Ke-Zhi,GUO Ling-Jun,HE Yong-Gang
2008 Vol. 23 (6): 11551158
Abstract(
3472 )
PDF(1468KB)(
1949
)
The carbon felt reinforced HfC-C/C and C/C composite integrated throats were prepared by thermal gradient chemical vapour infiltration process, and their ablation resistance was determined by using an equipment of solid rocket motor under the pressure of 7MPa. The effects of carbon hafnium on ablative properties of the integrated throat were investigated by scanning electron microscope (SEM) and energy dispersive spectroscope (EDS). The results show that the ablation behavior of the HfC-C/C composite integrated throat has characteristic of a steady ablation stage with constant linear ablation rate. Compared with those measured for the C/C composite integrated throat, the linear and mass ablation rates of the HfC-C/C composite integrated throat are decreased by 34% and 13%, respectively.
|
|
Ablation Characteristic of the Pierced C/C Composite Nozzle in a Combustion Gas Generator
CHEN Bo,ZHANG Li-Tong,CHENG Lai-Fei,LUAN Xin-Gang
2008 Vol. 23 (6): 11591164
Abstract(
3498 )
PDF(1657KB)(
1906
)
Ablation property of the pierced C/C composite nozzle was investigated via fire testing by a combustion gas generator which simulated oxy-rich combustion environments of the liquid rocket engine. Ablation mechanisms of the pierced C/C composite nozzle and effects of the combustion gas parameters were discussed. The results show that the linear ablation rate at the throat of the composite nozzle is 0.055±0.029mm/s, and the mass ablation rate is 0.186kg/(m2 ·s). blation behavior of the pierced C/C composite nozzle is directly affected by the compositions, temperature, pressure and the velocity of combustion gases, which shows a non-uniform process. Ablation in the regions ranging from the downstream of the convergent section to the throat is the most severe. Ablation mechanisms of the pierced C/C composite nozzle are cooperation of thermo-chemical ablation and thermo-mechanical erosion. The former is primarily dependent on the combustion temperature and concentrations of H2O and CO2, while the latter is influenced by the pressure and velocity of the combustion gas.
|
|
In situ Kinetics Study in Chemical Vapor Deposition of Pyrocarbon from Propylene
ZHAO Chun-Nian,CHENG Lai-Fei,ZHANG Li-Tong,XU Yong-Dong,LU Cui-Ying,YE Fang
2008 Vol. 23 (6): 11651170
Abstract(
3309 )
PDF(810KB)(
1765
)
The deposition kinetics of pyrocarbon by chemical vapor deposition (CVD) from propylene was investigated by in situ measurements of deposition rates which were measured by Magnetic Suspension Balance TG system. The gas phase products that collected by a liquid nitrogen cold trap were analyzed by GC-MS. The apparent activation energy is (201.9±0.6)kJ/mol in the range from 850℃ to 1100℃, where dilution ratio α is 4, total pressure is 6kPa and the flow rate of propylene is 20sccm, and the deposition kinetics is controlled by homogenous reactions. The main products of gas phase are single ring aromatic hydrocarbons and polycyclic aromatic hydrocarbons (PAHs) at high and low temperatures, respectively. Through the investigation of dependence of propylene partial pressure (0.3--6.5kPa) on deposition rate in 900℃ and 1000℃, it can be concluded that the decomposition of propylene is a first order reaction. Related to both of the effective reaction time and the flow rate of propylene, the maximum of the deposition rate is found at residence time of 0.6s.
|
|
Research on Thermal Conduction and Mechanical Properties for Carbon Foam
TIAN Zhuo,LI Ke-Zhi,LI He-Jun,SHI Zhen-Hai
2008 Vol. 23 (6): 11711174
Abstract(
3356 )
PDF(486KB)(
1820
)
The phenolic resin foam was prepared by using hollow phenolic resin microspher which was made by microcapsule. And under the protection of Ar, the microcapsules were carbonized at 1000℃ and graphited at 2000℃, then the foam was got. Herein the porosity and the effect of heat treatment temperature on carbon foam were investigated. And the results show that the porosity increasement can reduce the thermal conduction of material, and the low thermal conduction foam is obtained by using this method. However, for the materials with approximative porosity, the thermal conduction is decreased by reducing aperture of material. Finally, the foam material is obtained with density of 0.50g/cm3, thermal conduction of 1.007W/m·K and compressive strength of 8.82MPa.
|
|
Densification and Mechanical Properties of Boron Carbide Ceramics with Addition of Silicon Hexaboride
MA Qian-Cheng,ZHANG Guo-Jun,KAN Yan-Mei,WANG Pei-Ling,XIA Yi-Ben
2008 Vol. 23 (6): 11751178
Abstract(
3860 )
PDF(641KB)(
1862
)
Boron carbide (B4C) ceramics were fabricated by hot-pressing at 2000℃ for 1h with 2wt% and 5wt% SiB6 additives respectively. The effect of addition of SiB6 on sinterability and mechanical properties of B4C ceramics was studied. The results show that B4C ceramics can be fully densified by the addition of SiB6 and thus the mechanical properties of the sintered samples are effectively improved. When 2wt% SiB6 is added, the bulk density of B4C ceramics reaches 2.515g/cm3 which is about 99.5% of the theoretical density, while hardness and flexural strength of the sintered sample are 31.2GPa and 426.6MPa respectively. With the amount of SiB6 increase to 5wt%, the density, hardness and flexural strength of B4C ceramics are reduced to 2.500g/cm3, 29.7GPa and 387MPa respectively. On the other hand, the adding amount of SiB6 does not make a remarkable effect on fracture toughness of B4C samples since the K1C values in both cases are around 3.2MPa·m1/2. The phase assemblages and the reasons induced the changes in mechanical properties of the sintered samples with addtion of SiB6 are also discussed.
|
|
Morphology and Structure of Carbon Nanocoils Synthesized via the Flame Combustion of Ethanol
WANG Lan-Juan,LI Chun-Zhong,GU Feng,ZHOU Qiu-Ling
2008 Vol. 23 (6): 11791183
Abstract(
3094 )
PDF(1761KB)(
1799
)
Carbon nanocoils (CNCs) were in situ synthesized by the flame combustion of ethanol using stannic chloride as catalyst precursor. The morphology and structure of CNCs were characterized by means of scanning electron microscope, transmission electron microscope, X-ray diffraction and Raman spectrum. The coil diameter of the CNCs is calculated to be ca. 100nm and its fiber diameter is 50nm with a pitch of ca. 80nm. The CNC develops along the direction of growth and comprises carbon layers that are peripheral and circulate around the axes of the fiber, similar to a fishbone and the interlayer spacing between carbon sheets is ca. 0.34nm. High-resolution transmission electron micrograph (HRTEM) analyse reveals that the crystal face (101) of SnO2 is the most favored face for carbon precipitation and it is situated on the outer side of the CNCs, while crystal face (110) with the lowest carbon extrusion speed is situated on the inner side. The nonuniformity of the carbon extrusion speed at different crystal faces of the SnO2 grain leads to the helical growth of the coil.
|
|
Microstructure and Properties of Carbon Foams Reinforced by CVD PyC
CHEN Feng,ZHANG Hong-Bo,XIONG Xiang,YAN Zhi-Qiao
2008 Vol. 23 (6): 11841188
Abstract(
3093 )
PDF(1057KB)(
1787
)
Two carbon foams with different bulk density, marked as CF-1and CF-2 were prepared from AR mesophase pitch by self-foaming method at 450℃ under different foaming pressures, 0.1MPa and 3MPa, respectively. Then CF-1 was reinforced by chemical vapor deposition (CVD) PyC for 10h and 70h, getting two carbon foams marked as CF-1-PC1 and CF-1-PC2. The pore structures of four carbon foams were characterized by scanning electron microscope (SEM) and optical microscope (OM), and compressive strength and thermal conductivity were measured in further. The influences of CVD PyC process on carbon foams were investigated. The results show that CVD PyC can widen the ligament of carbon foams and close cracks in pore walls. No obvious interface exists between pitch carbon and PyC. The corresponding bulk density, compressive strength and thermal conductivity of CF-1-PC1 and CF-1-PC2 are 0.196g·cm-3, 1.89MPa, 0.314W·m-1·K-1 and 0.461g·cm-3, 11.93MPa, 1.581W·m-1·K-1, respectively.
|
|
Equilibrium Prediction of the Role of Key Species in the Chemical Vapor Deposition of Silicon Carbide
LU Cui-Ying,CHENG Lai-Fei,ZHANG Li-Tong,XU Yong-Dong,ZHAO Chun-Nian
2008 Vol. 23 (6): 11891192
Abstract(
3538 )
PDF(493KB)(
1844
)
Based on Gibbs minimum free energy principle, homogeneous equilibrium calculations were focused by Factsage code for MTS/H2 mixture. An assessment was made to determine the key species to SiC deposition. The results indicate that SiCl2 and C2H2 may contribute to SiC deposition, and their formations are favored high temperature and low pressure. Most of silicon-containing and carbon-containing species are SiCl4 and CH4, at low temperature and high pressure. Other substances such as hydrocarbons, orgamosilicons and silane compounds are probably unimportant for deposition process because of their low concentrations and small surface reactive sticking coefficient. Silicon and carbon are formed independently, based on the fact that there are barely species containing Si--C and Si--Si in gas phase. The ratio of silicon and carbon in sample is determined by their kinetics, respectively.
|
|
Electrochemical Properties of Hybrid Supercapacitor with Nanosized Fe3O4/activated Carbon as Electrodes
DU Xuan,WANG Cheng-Yang,CHEN Ming-Ming,JIAO Yang
2008 Vol. 23 (6): 11931198
Abstract(
3423 )
PDF(627KB)(
1992
)
The supercapacitor using nano-structured Fe3O4 and activated carbon (AC) as electrode materials was developed. Fe3O4 magnetic nanoparticles with average particle size of 36nm were synthesized by microwave method using FeSO4·7H2O and ammonia as the precipitator. Three kinds of supercapacitors, Fe3O4/KOH/Fe3O4, AC/KOH/AC, Fe3O4/KOH/AC, were prepared using 6mol/L KOH as electrolyte. Cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy were used to study the performance of the electrodes and the supercapacitors. The results show that the operating voltage of Fe3O4/KOH/AC hybrid supercapacitor is 1.2V. When the current density is 0.2mA/cm2 and the weight ratio of active materials (Fe3O4/AC) is 1.5, the energy density of hybrid supercapacitor is 9.25Wh/kg, which is 53.4% higher than that of AC/KOH/AC capacitor with the same electrolyte.
|
|
Fabrication and Characterization of High-purity Nanostructured Bulk LaB6 Polycrystal Cathode Material
ZHOU Shen-Lin,LIU Dan-Min,ZHANG Jiu-Xing
2008 Vol. 23 (6): 11991204
Abstract(
2903 )
PDF(1131KB)(
1835
)
La-LaH2 nanopowders were prepared by hydrogen arc plasma method, and then the mixed nanopowders of La-LaH2 and B were in situ sintered by Sparkle Plasma Sintering (SPS) method in oxygen free system. High-purity LaB6 polycrystal nanostructured bulk was successfully synthesized by SPS. The dehydrogenation of LaH2 nanopowders and the reaction equation of sintering LaB6 were studied. The phase and microstructure of LaB6 bulks were characterized by using XRD, SEM, TEM and AFM techniques. The results show that the dehydrogenation temperature of LaH2 nanopowders is 796.4℃. The sintered body is single-phase LaB6, which has a high purity of 99.867%, and its relative densities is up to 99.2%. The hardness and bend strength of the sintered LaB6 are much better than those of LaB6 prepared by other sintering methods. The crystals of LaB6 bulk are equiaxed crystals, the average grain size of the bulks sintered at 50MPa and 1250-1350℃ is about 120nm. The grains are homogeneous and integrated, and the grain size increases with the raising of sintering temperature.
|
|
Synthesis of Microsized Co3O4 Octahedral by High Temperature Gas-solid Hydrolysis
LIU Zhi-Hong,HU Lei,LIU Zhi-Yong,LI Qi-Hou
2008 Vol. 23 (6): 12051210
Abstract(
3132 )
PDF(731KB)(
1727
)
A novel method, involving high temperature gas-solid hydrolysis, was proposed for the preparation of micro-Co3O4 powder. The effects of reaction temperature, crystal water content of CoCl2, the addition of inert dispersate on the product were investigated. The composition,morphology, and particle size of the prepared particle are characterized by X-ray diffraction(XRD), Scanning electronmicroscope(SEM) and Laser particle size analysis. The results indicate that the obtained powder with octahedral crystal structure are surrounded by {111} crystal surfaces. And the size ranges from submicron to micron, the particle size increases with the temperature elevating, the size distribution becomes narrow when CoCl2·2H2O is employed as precursor. The addition of inert dispersate is beneficial to the monodispersity of the obtained powder. The reasons for the formation of octahedral crystal morphology and the influencing factors of the particle size and morphology are also discussed.
|
|
Characteristics of SiC/nano-TiN Aqueous Mixed Slurry and Its Spray Drying Behavior
GUO Xing-Zhong,LI Hai-Miao,ZHU Xiao-Yi,YANG Hui,FU Pei-Xin,GAO Li-Hua
2008 Vol. 23 (6): 12111215
Abstract(
3221 )
PDF(687KB)(
1746
)
The aqueous slurries were prepared usingtetramethyl ammonium hydroxide (TMAH) as dispersant, nano-TiN and submicron SiC powders as starting materials. The dispersion, stabilization mechanism and spray drying behaviors of SiC/nano-TiN aqueous mixed slurry were analyzed. The results show that TMAH can be absorbed on the surface of nano-TiN and SiC particles, and the dispersibility of particles is cooperatively improved by electrostatic and steric effects. The mixed slurry possesses better dispersion and stabilization when pH value is 8 and the amount of TMAH is 0.75wt%, and the SiC/nano-TiN composite powders prepared by spray drying distribute uniformly with good fluidity.
|
|
Preparation and Application of Perovskite Hollow Fiber Oxygen Permeable Membrane
CHEN Xin-Zhi,YU Ling-Hui,LIU Qiao-Sheng,WANG Hai-Hui,LI Zhong
2008 Vol. 23 (6): 12161220
Abstract(
3108 )
PDF(794KB)(
1808
)
The dense perovskite hollow fiber made of BaCo0.4Fe0.4Zr0.2O3-δ (BCFZ) was prepared by phase inversion spinning followed by sintering. The crystal structure and the microstructures of the hollow fiber membrane were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The sintered hollow fiber membrane was also used to construct a reactor for the partial oxidation of methane (POM) to syngas. It is found that the BCFZ itself exhibits low activity for conversion of methane which is lower than 3% without catalysts. After Ni-based catalyst is introduced, the conversion of methane, the CO selectivity and the oxygen permeation flux reach 93%, 80% and 11mL/min·cm2, respectively. It takes only 90min to get the steady state at initial stage in the hollow fiber membrane reactor, which is much shorter than that in the disk-type membrane reactor. The hollow fiber membrane reactor is steadily operated for 40h for the POM reaction.
|
|
Preparation and Oxygen Permeation for SrCo0.8Fe0.2O3-δ Tubular Asymmetric Membrane
FAN Chuan-Gang,HUANG Xiang-Xian,LIU Wei,CHEN Chu-Sheng
2008 Vol. 23 (6): 12211224
Abstract(
3135 )
PDF(535KB)(
1967
)
The tubular asymmetric membrane (TAM) was prepared by co-firing method with dense top layer of SrCo0.8Fe0.2O3-δ(SCF) and porous substrate layer of (SrCo0.8Fe0.2O3-δ)0.85(SrSnO3)0.15 (SCF-SS). Its phase composition, morphology and oxygen permeability were investigated. The results show that SCF layer and SCF-SS layer have desirable compatibility for configuration of asymmetric membrane. The resulting TAM sample sintered at 1150℃ has the dense layer of SCF with thickness of 50μm and the SCF-SS substrate with apparent porosity of 19.3%. The permeation rates of the resulting TAM are 1.91mL·cm-2·min-1 at 900℃ and 1.01mL·cm-2·min-1 at 800℃, respectively, which are 24% and 36% higher than those of the SCF tubular symmetric membrane (TSM) with same size(wall thickness of 1.4mm, outer diameter of 10.3mm, and length of 4.1cm).
|
|
Synthesis of Sn-Substituted ZSM-5/Carbon Zeolite Membrane and Application in Separation of Acetic Acid/water Mixtures by Pervaporation
WANG Xian-Wu,YANG Jian-Hua,LU Jin-Ming,WANG Tong-Hua,WANG Jin-Qu
2008 Vol. 23 (6): 12251230
Abstract(
3178 )
PDF(944KB)(
1978
)
Study on the synthesis and characterization of Sn-ZSM-5 zeolite was carried out. The Sn-ZSM-5 zeolites were prepared from the clear solution of Si(OCH2CH3)4/SnCl4/NaOH/TPABr/H2O by hydrothermal method. SEM, XRD, IR and UV-Vis analysis confirm that Sn atoms are introduced into ZSM-5 zeolite framework. After gained Sn-ZSM-5 zeolites, the carbon tube-supported Sn-ZSM-5 membrane with various Si/Sn ratios are also synthesized by using simple seeded method. The formed Sn-ZSM-5 membranes are found dense and continuous. For 5wt% acetic acid feed, the membrane with Si/Sn of 25 has a total flux of 1.18kg·m-2·h-1 at 90℃ with an acetic acid/water separation selectivity of 4.1.
|
|
PAMAM-SBA-15 Composite in Application of Heavy Metals Ions Adsorption
YU Chi-Chao,ZHANG Ling-Xia,QIN Fei,LI Jiang-Tian,SHI Jian-Lin,YAN Dong-Sheng
2008 Vol. 23 (6): 12311235
Abstract(
3550 )
PDF(480KB)(
1902
)
Using 3-aminopropyltriethoxysilan (APTES) to modify the interior surface of SBA-15 channels, PAMAM of generation 1 and generation 2 were successfully grafted in the meso-channels of SBA-15. The PAMAM-SBA-15 hybrids are employed in the adsorption of heavy metal ions to determine their adsorptive capacity, with the APTES modified SBA-15 as a reference sample. The bonding between PAMAM hybrids and metal ions are proved to be much stronger than that of APTES modified SBA-15 by TG-MS tests. Hybrids are used in deposition solution containing several kinds of heavy metal ions, and the selective adsorption of Pb2+ and Zn2+ is found. After deposition, the concentrations of Pb2+ and Zn2+ are reduced to 0.003mg/L and 0.037mg/L, respectively, which are lower than the national standard of drinking water.
|
|
Preparation and Mechanism Study of Mesoporous Titania Whiskers
HE Ming,XU Li,GU Xiao-Li,LUO Zhen-Yang,LU Xiao-Hua
2008 Vol. 23 (6): 12361240
Abstract(
2972 )
PDF(897KB)(
1857
)
A simple novel procedure for the synthesis of mesoporous titania whiskers from potassium dititanate (K2Ti2O5) was reported. Nanostructure whisker was obtained via controlling mesostructure transition process of the unstable trigonal bipyramidal layered crystal structure of K2Ti2O5 in a hydration step. XRD, TEM and HREM results confirm the existence of nanophase KOH·nH2O inside the inorganic framework. Removing of nanophase KOH·nH2O by acid solution leads to the formation of mesoporous structure with the specific surface area up to 248m2/g. The mesoporous structure of TiO2 whiskers and fibrous morphology can be preserved by calcination at 500℃ with the specific surface area of 139m2/g and the pore diameter of 8.7nm.
|
|
Investigation of HA/chitosan Composite Coatings Prepared by Sol-Gel on Alkali Treated Titanium Surfaces
WANG Ying-Bo,LU Xiong,FENG Bo,QU Shu-Xin,WENG Jie,CHEN Jian-Min
2008 Vol. 23 (6): 12411245
Abstract(
3612 )
PDF(973KB)(
1750
)
Hydroxyapatite/chitosan (HA/CS) composite coatings were prepared on titanium surfaces by hydro-thermal synthesis and Sol-Gel method. The composition, structure, morphology and biocompatibility of composite coatings were characterized. Ti surfaces are convertedinto super-hydrophilic surfaces by alkali treatment, XRD analysis reveals that the coatings are mainly composed of HA and CS and their compositions are determined by TG analysis. SEM observation shows that the coatings with different HA content have different morphologies. Osteoblasts are cultured on the coatings to evaluate their biocompatibility. Alamar Blue assay indicates that cells on the composite coatings has larger proliferation rate than those on pure titanium. Also the ALP activity of the cells on the composite coatings is higher than that on the pure titanium samples. The results demonstrate that as-prepared HA/CS composite coatings have good biocompatibility.
|
|
Blood Compatibility of Titanium Oxide Films Modified by Hydrogen Plasma Reduction
XU Yi,HUANG Nan,SUN Hong
2008 Vol. 23 (6): 12461252
Abstract(
3049 )
PDF(961KB)(
1506
)
Rutile titanium oxide films on silicon substrate were prepared by unbalanced reactive pulsed magnetron sputtering and subsequently modified by hydrogen plasma reduction. The XRD patterns show that the modified titanium oxide films consist of single rutile phase, which is similar to as-deposited films. FTIR results exhibit that no obvious -OH groups exist in the films. XPS spectra display that oxygen deficiency exist in the film after hydrogen plasma reduction. The wettability experiment show that the hydrophilicity of the hydrogen plasma modified Ti-O films decreases slightly. The anticoagulation property of Ti-O films modified at lower temperature in short time (110℃, 15min) is obviously improved, which is related to the content of oxygen deficiency. Consequently hydrogen introducing is an effective way to improve the anticoagulation property of titanium oxide films.
|
|
Photocatalytic Activities of TiO2 Nanopowders by Hydrothermal Synthesis in Different Solution Medium
LI Xiu-Yan,YANG Xian-Feng,WU Ming-Mei
2008 Vol. 23 (6): 12531258
Abstract(
3455 )
PDF(679KB)(
1816
)
TiO2 nanopowders were prepared by hydrothermal synthesis in distilled water, three small organic compounds (n-butyl alcohol, propane diacid and ethylenediamine) and three inorganic acids (HNO3, H2SO4 and HCl) using the titanium n-buoxide as raw material. The product was characterized by powder X-ray diffraction (XRD) and transmission electron microscope (TEM). The effect of different solvent medium on the crystal phase composition, particles size and morphology of the product was investigated. The result shows that anatase TiO2 with non-uniform grain size is obtained in distilled water. The ability to retard the anisotropic growth of anatase is as follows: n-butyl alcohol>propane diacid>ethylenediamine. Under the same experiment condition, rutile, anatase and mixed crystallite of anatase and rutile TiO2 powders are obtained in HCl, H2SO4 and HNO3 medium, respectively. The result of photocatalytic degradation methyl orange shows that the photocatalytic activity of mixed crystallite of anatase and rutile TiO2 powders is higher than that of the pure anatase TiO2 powders. The photocatalytic activity of pure rutile TiO2 powders is worst.
|
|
Study on Synthesis in situ and Photocatalytic Activity of TiO2 Nanotubes Array Films
CUI Yun-Tao,WANG Jin-Shu,LI Hong-Yi,WANG Zhen-Zhen
2008 Vol. 23 (6): 12591262
Abstract(
3166 )
PDF(579KB)(
1825
)
The highly ordered aligned titania nanotubes thin films were successfully prepared by liquid phase deposition (LPD) method. Anodic aluminum oxide (AAO) used as starting material was immersed in an aqueous ammonium hexafluorotitanate ((NH4)2TiF6) solution. The results show that anatase titania can be obtained after the thin films are annealed at 400℃ for 4h. The outside diameter of the titania nanotube is about 150nm and the wall thickness of the nanotubes is approximately 25nm. Moreover, the thickness of titania nanotube array is about 5μm. The annealed TiO2 thin films have good photocatalytic activity on the degradation of methyl blue, i.e., methyl blue can be entirely degradated after 120nm mercury arc irradiation.
|
|
Preparation and Photocatalytic Performance of SiO2-Pillared Layered Titanate
JIANG Fang,SHAO Fei
2008 Vol. 23 (6): 12631266
Abstract(
2937 )
PDF(418KB)(
1712
)
SiO2 pillared layered titanate (SiO2-H2Ti4O 9) was prepared from the layered K2Ti4O9 via a step-reaction method. The influences of alkyl chain length of intercalated alkylamines, washing methods and the hydrothermal time of alkylamine reacted with TEOS on the structure of SiO2-H2Ti4O9 were investigated. The photocatalytic activities of SiO2-H2Ti4O9 were evaluated by photocatalytic oxidation of methylene blue(MB) aqueous solution. The results reveal that the interlayer spacing of alkylamine pre-intercalation samples increases with the increase of the chain length of alkylamines, and the crystallinity of the samples washed with ethanol solution(1:1, v/v) is enhanced compared with anhydrous ethanol. SiO2-H2Ti4O9 treated twice by TEOS at 130℃ has an interlayer spacing of 1.45nm and a specific surface area of 148.4m2/g. SiO2 pillared layered titanate shows a higher efficiency of MB photo-degradation compared with its precursors K2Ti4O9.
|
|
Preparation of Pt/MoO3/ZrO2 Catalyst and its Property of Three-Way Catalysts
WEN Yi-Yun,LIU Zhi-Ming,CAI Li,GUO Jia-Xiu,GONG Mao-Chu,CHEN Yao-Qiang
2008 Vol. 23 (6): 12671271
Abstract(
3013 )
PDF(556KB)(
2211
)
MoO3/ZrO2 was prepared by impregnation method. Its specific surface area, pore size, pore volume and surface acidity were investigated by means of low temperature nitrogen adsorption-desorption and NH3-temperature programmed desorption. By using MoO3/ZrO2 and La2O3/Al2O3 as catalyst support, Pt/MoO3/ZrO2 and Pt/La2O3/Al2O3 catalysts were prepared by wet impregnation method and the activity test of C3H8, CO, NO were also investigated in the simulated automotive gas. The results show that MoO3/ZrO2 has good texture(SBET=106.8m2/g) and surface super-acidity. And the catalysts were also characterized by X-ray diffraction and H2-temperature programmed reduction. Compared with traditional three-way catalyst Pt/La2O3/Al2O3, Pt/MoO3/ZrO2 exhibits lower light-off temperature of hydrocarbon (230℃), carbon monoxide (200℃), and nitrogen oxides (210℃) and wider operational air-to-fuel ratio window, which especially improves C3H8 conversion under higher oxidative conditions. The results also show that Pt on the catalyst support has high dispersion and excellent redox properties.
|
|
Performance of Mullite Matrix Microwave Absorber Coatings Fabricated by Plasma Spraying Technology
JIANG Li,YUAN Xiao-Jing,ZHA Bai-Lin,HOU Gen-Liang,WANG Han-Gong
2008 Vol. 23 (6): 12721276
Abstract(
3336 )
PDF(802KB)(
1896
)
The clusters of mullite matrix (steatite, carbon) composite absorber powders were produced by using spraying spheroid granulator, and the composite powders were used to fabricate composite microwave absorber coatings by plasma spraying technique. The results show that during the plasma spraying, the carbon is oxidized, and the steatite is decomposed to enstatite and quartz for the high temperature plasma gas. The experiments show that the mean adhesive strength of coatings decreases with the coating thickness increasing, which reaches 2MPa with thickness of 0.8mm. The crack extracted the coatings rupture surface with wavelet maximum module exists in the glass phase interface. For these coatings, with the coatings thickness increasing, the reflectivity coefficient transforms to low frequency; while with the complex permittivity of enstatite increasing, it decreases and transforms to high frequency. The reflectivity coefficients of the coatings with thickness of 0.8mm are all below -5dB in the frequency range from 15GHz to 18GHz.
|
|
Synthesis and Characterization of N-doped Pink ZnO Nanocrystalline by Combustion Method
WU Jia-Qing,ZHENG Min
2008 Vol. 23 (6): 12771282
Abstract(
3559 )
PDF(848KB)(
1816
)
N-doped ZnO (NZO) nanocrystallines were synthesized by combustion method using urea as main fuel, surfactant as assistant fuel and zinc nitrate as oxidant. The effects of calcination temperature and molar ratio of urea to zinc nitrate on the properties of the synthesized samples were investigated. The variation of adiabatic flame temperature (Tad) with the various fuel-to-oxidizer molar ratios value was calculated theoretically according to the thermodynamic principle. XRD, FTIR, SEM and XPS were used to characterize the properties of the samples respectively. The experimental results show that perfect pink powders with standard cubic ZnO crystal phase are obtained at 800℃ when molar ratio of the urea to zinc nitrate is 4.920 and the concentration of the zinc nitrate is 60g/L. The average primary granularity of the as-synthsized sample is about 30nm estimated according to Scherrer Equation. XPS analysis indicates that the nitragen concentrantion in the N-doped ZnO sample is 1.02%. And the obtained N-doped ZnO film has perfect ultraviolet prevention ability.
|
|
Synthesis of Core/Shell Calcium Carbonate Peanut-like Assemblies in Polyacrylamide Aqueous Solution
JIANG Xi-Hua,ZHENG Ming-Bo,CHEN Hui-Qin,PAN Li-Jia,TAO Jie,CAO Jie-Ming
2008 Vol. 23 (6): 12831286
Abstract(
3134 )
PDF(792KB)(
1812
)
Peanut-like CaCO3 assemblies with core-shell structure were obtained in polyacrylamide aqueous solution. The as-prepared products were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), and X-ray diffraction (XRD). The results indicate that the peanut-like CaCO3 assemblies has some hollows. The shell of the CaCO3 assemblies is composed of calcite rhombohedras, and the core of the CaCO3 assemblies is composed of rod-like aggregates which are assembled by small particles and the core has a radially outward growth structure. The radially outward structure of the core is explained by the fractal growth theory, and the formation of Core/Shell structure is explained by the Ostwald ripening theory.
|
|
Low-temperature Cofiring Behavior of ZMT3/NZC Sandwich Structure Composites
LIU Xiang-Chun,TIAN Chang-Sheng
2008 Vol. 23 (6): 12871292
Abstract(
3353 )
PDF(979KB)(
1739
)
A novel zero-shrinkage-difference technique was introduced to eliminate the camber or cracks in cofired composites without the degradation, A sandwich structure of (Zn0.7Mg0.3)TiO3(ZMT3) dielectric/(Ni0.8Zn0.12Cu0.12)Fe1.96O4(NZC) ferrite multilayer composite was designed and prepared by using tape-casted technique, with ZMT3 as interlayer, and NZC as top and bottom layers. The produced sandwich structure shows no camber and cracks after being co-sintered. The cofired samples exhibit good dielectric performance (εr=12, tanδ=9.84×10-4), and low firing characteristics (900℃). Due to their dielectric performance, low firing characteristics, and realizable co-firing compatibility, the sandwich structure of ZMT3 dielectric/NZC ferrite multilayer composite can serve as the promising medium materials in the multilayer LC filter.
|
|
Research on Low-temperature Sintering of Ca0.3(Li1/2Sm1/2)0.7TiO3 Microwave Dielectric Ceramics
LI Yue-Ming,SONG Ting-Ting,YOU Yuan,HU Yuan-Yun,LIU Wei-Liang,TANG Chun-Bao
2008 Vol. 23 (6): 12931297
Abstract(
3077 )
PDF(686KB)(
2028
)
The NCB(Na2O-CaO-B2O3)-doped Ca0.3(Li1/2Sm1/2)0.7TiO3(CLST) ceramics were fabricated via the traditional ceramic process. The relation between NCB dopant contents and the crystal structure, microstructure, sintering behavior, and dielectric properties of CLST ceramics were investigated systematically. The results indicate that the second phases are not found when NCB dopant contents are in the range from 1wt% to 15wt% and the major phase of CLST ceramics is still orthorhombic perovskite. With the increase of NCB content, the densification temperature and bulk density of CLST ceramics decrease, the dielectric constant εr and the product of quality factor and resonance frequency Qf value also decrease, and the temperature coefficient of resonant frequency τf increases to positive. NCB can effectively decrease the sintering temperature of CLST from 1300℃ to 900℃. The sample of CLST with 12.5wt% NCB sintered at 900℃ for 5h still has excellent dielectric properties: εr=73.7, Qf=1583GHz, τf=140.1×10-6/℃, which satisfies the design demand of high dielectric constant and multilayer microwave components.
|
|