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Hardening Mechanism for Nano-multilayer Films
DU Hui-Jing,TIAN Yong-Jun
2006 Vol. 21 (4): 769775
Abstract(
3275 )
PDF(414KB)(
1973
)
The study of the hardening mechanism for the nano-multilayer films is the foundation for the preparation of those films. Several different models were proposed to interpret the super-hard effect in the nano-multilayer films, though they cannot interpret all the phenomena in those films. The progress of the research on the superhardness effect in the nano-multilayer films was reviewed. It shows that all the mechanisms are related to the movement of the dislocation. The difference of the elastic modulus between the two materials plays the important role for the superhadness effect in the nano-multilayer films, while the alternated strain field plays the less important role. The developmental directions and the problems for the nano-multilayer films were also discussed.
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Doping Mechanism and Visible-light Photocatalytic Activity of S-doped TiO2 Nano Powders
ZHOU Wu-Yi,CAO Qing-Yun,TANG Shao-Qiu,LIU Ying-Ju
2006 Vol. 21 (4): 776782
Abstract(
3709 )
PDF(454KB)(
2333
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S-doped TiO2 nanopowders were prepared by a sol-gel method with acid as the catalyst. The results of photocatalytic degradation methylene blue demonstrated that the doped TiO2 exhibited the highest photocatalytic activity when the mole ratio of thiourea and tetrabutyltitanate[Ti(OC4H9)4] was 3.5 and the doped TiO2 was calcined at 500℃ for 2h. The results from the X-ray diffraction (XRD), diffusion reflectance spectra (DRS) and X ray photoelectron spectroscopy (XPS) showed that sulfur doping controlled the increasing of nano TiO2 and restrained the transformation from anatase to rutile. S2- was oxidezed to S4+ during the thermal treatment. The trance of sulfur ions (S4+) substitued partially for the lattice titanium ions (Ti4+), which resulted in the localized crystal deformation of TiO2 and the bandgap between valence band and conduction band narrowed, and the absorption light transferred to visible light region.
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Characterization of Optical Response Properties for a Nanosized TiO2 with Visible-light Response
ZHOU Shi-Feng,HONG Zhang-Lian,ZHAO Fu-Rong,FAN Xian-Ping
2006 Vol. 21 (4): 783788
Abstract(
3386 )
PDF(446KB)(
1870
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Nanosize-TiO2 podwers with visible-light response and photocatalytic capability were synthesized by hydrothermal process with organics as solvents. Results of diffuse reflectance spectra (DRS) for solid TiO2 powders show that the visible light response properties of present nanosize-TiO2 are similar to that of modified TiO2, which have strong visible-light response in visible-light region. On the other hand, UV-Vis absorption spectra of TiO2 suspensions show that the optical properties of present nanosize-TiO2 are similar to that of intrinsic TiO2, and no obvious visible light absorption detected. Such difference in optical properties via DRS and UV-Vis spectra for present nanosize-TiO2 is attributed to the difference status of nanosize-TiO2 existing as solid powder or dilute suspensions. Underthe conditions of extreme dilute suspensions, photon induced electron transition accompanied by phonon excitation may be degenerated while it is not the case for solid powders. For present photocatalyst with high activity under visible light irradiation, it is necessary to combine two methods to evaluate the accurate information of the absorption edge and optical response properties.
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Preparation of Mn3O4 Nano Crystals in Dimethyl Sulfoxide(DMSO) Medium
FAN Wu-Gang,GAO Lian
2006 Vol. 21 (4): 789792
Abstract(
2967 )
PDF(433KB)(
1664
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Nanometer trimanganese tetraoxide nanocrystals were synthesized in DMSO medium with a solvothermal method. The products were characterized by XRD, TEM and FT-IR spectra. The XRD patterns showed that the phase was Mn3O4. The magnetic properties were investigated on a vibrating sample magnetometer (VSM). The results showed that the magnetic performance of the nano Mn3O4 was paramagnetic at room temperature.
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Hytrothermal Synthesis and Gas Sensitivity of One-dimensional ZnO
LIU Rong-Li,XIANG Qun,PAN Qing-Yi,CHENG Zhi-Xuan,SHI Li-Yi
2006 Vol. 21 (4): 793796
Abstract(
3303 )
PDF(578KB)(
1903
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Zn(NO3)2 was used as the raw material to prepare one-dimension ZnO through a hydrothermal technique with CTAB controlling ZnO morphology. The products were characterized by X-ray diffraction(XRD), transmission electron microscope(TEM) and scanning electron microscope(SEM). Gas sensors were made by using the ZnO nanorads and their gas sensitivities were measured. The result shows that the ZnO nanorods have lower working temperature than granulated ZnO and have very good sensitivity to 10ppm trimethylamine (TMA), methanol, ammonia, acetone and ethanol at the working temperature of 170℃. The gas sensitivity mechanism of the ZnO rods was discussed.
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Preparation and Dielectric Enhancement of Nickel-coated β-SiC Nanoparticles
ZOU Gui-Zhen,CAO Mao-Sheng,ZHANG Liang,JIN Hai-Bo,XU Hui,WANG Zheng-Ping
2006 Vol. 21 (4): 797802
Abstract(
3233 )
PDF(785KB)(
2800
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A nanoscale core-shell structure of β-SiC P-Ni was prepared at lower temperature by a simple and convenient electroless plating approach. The core-shell nanoparticles were characterized by means of XRD and TEM. The results show that β-SiC nanoparticles (β-SiC P) are coated by a uniform and continuous nickel shell. The mechanism based on the theory of electroless plating and palladium catalysis was discussed in details about core-shell structure of β-SiC P-Ni. Dielectric permittivities of the original silicon carbide nanoparticles (β-SiC P) and nickel-coated β-SiC P in paraffin wax were measured respectively in the GHz frequency range from 8 to 12GHz. The real part and dielectric loss tangent of the nickel-coated β-SiC P were significantly enhanced. The origin of the enhancement was discussed in theory, and also explained by discussing the change of surface electrical conduction behavior of β-SiC P and nickel-coated β-SiC P.
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Enhanced Photoluminescence of Er3+-doped Al2O3 Powders by Y3+
WANG-Hui,LEI-Ming-Kai
2006 Vol. 21 (4): 803808
Abstract(
2759 )
PDF(376KB)(
2094
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The Y3+ co-doping to the 0.1 and 1.0mol% Er3+-doped Al2O3 powders with
the molar ratio of (0~10): 1 for Y3+ and Er3+ was performed in the non-aqueous sol-gel progress using the aluminium isopropoxide Al(OC3H7)3-derived Al2O3 sols with the addition of hydrated erbium nitrate Er(NO3)3·5H2O together with yttrium nitrate Y(NO3)3·5H2O. The effects of Y3+ co-doping on the phase structure and photoluminescence (PL) of the Er3+-doped Al2O3 powders were investigated by X-ray diffraction (XRD) and PL measurement. The Y3+ addition in the Er3+-doped Al2O3 powders suppressed the crystallization of γ-(Er,Al)2O3 and θ-(Er,Al)2O3 phases. The enhancement of the PL properties by Y3+ co-doping is related to Er3+ concentration in the Er3+-doped Al2O3 powders. For the 1mol% Er3+-doped Al2O3 powders, co-doping Y3+ with the concentration up to 10mol% is incorporated in the mixture of γ and θ phases, resulting in an increase of both the intensity and full width at half maximum (FWHM) of PL spectra. The PL intensity for the 1mol% Er3+-doped Al2O3 powders by 10mol% Y3+ co-doping is enhanced by 50 times and almost 10 times higher than that of the 0.1mol%Er3+-doped Al2O3 powders, and the FWHM is enhanced by a gain of 15nm in comparison with those for the 1mol% Er3+-doped powders. However, for the 0.1mol% Er3+-doped Al2O3 powders, no significant change in the intensity and FWHM of PL spectra is observed with all the Y3+ incorporations. The improvement of intensity and FWHM of PL spectra for the Er3+-doped Al2O3 powders by Y3+ co-doping is attributed to the improved dispersion and disordered local structure around Er3+ in the matrix of the Er3+-doped Al2O3 powders, respectively.
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Nano-scale Ce0.8Y0.2O1.9 Powders Prepared by Low Temperature Combustion Synthesis Technique
XU Hong-Mei,YAN Hong-Ge,CHEN Zhen-Hua
2006 Vol. 21 (4): 809814
Abstract(
2614 )
PDF(526KB)(
1917
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Nanocrystalline Ce0.8Y0.2O1.9 solid solution was synthesized by a gel combustion technique using citric acid as reductant and nitrates as oxidants. The effects of processing parameters, such as the amount of citric acid, the pH value of solution, the amount of oxidants on the gel formation and the powders characteristics of the product were investigated by using TG/DTA, XRD, FTIR, Raman and TEM. The stable gel was obtained by controlling the amount of citric acid and the pH value. The nanocrystalline Ce0.8Y0.2O1.9 powders in the range of 5nm to 40nm were obtained by changing the amount of oxidants. The Raman investigation showed that the oxygen vacancy concentration increased with the increase of the amount of oxidants.
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Synthesis of Nano Zinc Borate Fire Retardant by Solid State Reaction
HU Yun-Chu,WU Zhi-Ping,SUN Han-Zhou,Zhou Ying,LIU Yuan
2006 Vol. 21 (4): 815820
Abstract(
3566 )
PDF(444KB)(
1905
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There are the handicaps as removing impurity and vaporizing solvent and reunited particle in the rut means of synthesis of zinc borate. These means do not meet the need of preparation of nano zinc borate. In this paper, a new way was researched for the preparation of nano zinc borate from ZnO and H3BO3. The results of XRD and SEM and XPS show that the zinc borate made from ZnO and H3BO3 by solid state rubbing reaction is an amorphism structure. The burning charcoal test indicates that 38.9% of charcoal ratio of poplar wood powder treated with zinc borate made from ZnO and H3BO3 at 1:1 mole ratio, higher than 22.7% of charcoal ratio of the comparison. The compound fire retardant from zinc borate and ammonium polyphosphate has the complex effect of fire retardation. It is 44.5% the charcoal ratio of poplar wood powder treated with the compound fire retardant from zinc borate and ammonium polyphosphate at 50% mass ratio. The complex effect of fire retardation is 22.2%. Solid state reaction is a availability way of preparation of nano salt particle.
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Cubic AlN Synthesized by High Energy Ball Milling and Its Phase Conversion at High Temperature
LI Peng-Liang,ZHOU Jing-En,XI Sheng-Qi
2006 Vol. 21 (4): 821827
Abstract(
3316 )
PDF(508KB)(
1929
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The phase conversion of Al2O3 during high-energy ball milling was investigated. After 20h milling, amorphous and AlN were observed in powders, these were not reported previously. The crystal structure of AlN gained during ball milling is cubic, differs from that of the regular hexagonal AlN synthesized with carbothermal reduction. AlON phase forms by the reaction of cubic AlN and γ-Al2O3 after annealing in N2 atmosphere at the temperature above 500℃. The formation of AlON phase decreases the commencing temperature of AlN.
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Fabrication of Alumina Nano-fibers from PAAO
PAN Jin-Zhi,ZHAO Hong,CHEN Chun-Huan,LI Guo-Jun,REN Rui-Ming
2006 Vol. 21 (4): 828832
Abstract(
3018 )
PDF(767KB)(
2140
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Based on PAAO's unique cellular hexagon morphology and composition, various alumina fibers (nano-belts, nano-rods, and nano-tubes) were fabricated by simply employing a dilute acid etching method. Scanning electron microscope (SEM) incorporated with energy dispersive X-ray spectroscope (EDS) and transmission electron microscope (TEM) were applied to characterize these nano-fibers. It is proved that alumina nano-fibers are formed from the porous layer, while totally different behaviors of the barrier layer and the porous layer are showed during the etching process. The orientated etching, resulted from PAAO's particular morphology and composition, is believed to be the main reason that explains the formation of different alumina nano-fibers.
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Synthesis of Magnesium Borate Nanorods by Sol-Gel Process
JIANG Ji-Wei,WANG Lei,YANG Qing,YANG De-Ren
2006 Vol. 21 (4): 833837
Abstract(
3564 )
PDF(568KB)(
2115
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The magnesium borate (MgB4O7 and Mg2B2O5) nanorods were fabricated with magnesium nitrate, boric acid and citric acid as the starting reagents by the sol-gel method. The structures and morphologies of the nanorods were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). The results show that the products synthesized by calcining were MgB4O7 at 750 ℃ and Mg2B2O5 at 950℃. The ratios of diameter and length of the nanorods can be controlled by adjusting the proportion of Mg(NO3)2 and H3BO3. The self-catalytic mechanism was used to explain the growth of the magnesium borate nanorods.
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Czochralski Growth and Spectral Characteristics of Tm:YAP Single Crystals
LU Yan-Ling,WANG Jun,YANG Yang,LI Sheng-Hua,SUN Bao-De,YUAN Qing-Xi
2006 Vol. 21 (4): 838842
Abstract(
3196 )
PDF(523KB)(
1800
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YAP single crystals doped with 4at%, 8at% and 10at% Tm3+ ions were grown by the Czochralski method with MF induction heating. The segregation coefficient of Tm3+ ion in YAP crystal measured by X-ray fluorescence spectrum technique is about 0.88. Growth striation and structural stress were determined by synchrotron radiation white-beam topography (SRWBT). The absorption spectrum shows two peaks with wavelength of 694nm and 795nm, and the fluorescence peak is about 2.0μm, which suggest that Tm:YAP is one of the most promising mid-infrared laser crystals.
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Diffusion Behavior in Amorphous Si-B-C System by Molecular Dynamics Simulation
YE Ya-Jing,ZHANG Li-Tong,CHENG Lai-Fei,XU Yong-Dong
2006 Vol. 21 (4): 843848
Abstract(
3135 )
PDF(383KB)(
1779
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Molecular dynamics simulations of amorphous Si-C and Si-B-C systems were carried out in order to investigate the diffusion behavior, and analyze the influence of the addition of B on the thermal stability and creep resistance at high temperature of the amorphous systems. Universal force field was used to describe atomic interactions in the systems at 300K, 773K, 1273K, 1773K and 2073K. MSD curves and diffusion constants at different temperatures were calculated and compared. After the addition of B in the amorphous Si-B-C system, self-diffusion constants of constituent atoms decreased at the same temperature, and increased with temperatures in both the amorphous systems. The results show that self-diffusion of B tends to ascend apparently up to 2073K, which accounts for that phase separation of the amorphous state would take place at about 2073K. Below this temperature, the Si-B-C system will remain the thermal stability and good creep resistance.
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Peparation of Porous Carbon Template with Controllable Channels by Phenolic Resin Pyrolyzing
CUI Zhi-Zhong,LI Di-Chen,QIAO Guan-Jun,LI Ji-Shun
2006 Vol. 21 (4): 848854
Abstract(
3271 )
PDF(1024KB)(
1790
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Porous carbon templates were prepared by pyrolysis of samples. The samples were fabricated by filling mixture of phenolic resin and corn starch into negative molds with network structure manufactured by stereolithography. The network structure generated the channels in pyrolysis process. Thermo-gravimetric analysis (TGA) was applied to reveal the pyrolysis behaviors of photo-curable resin, phenolic resin and corn starch. X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR) and scanning electron microscope (SEM) were employed to characterize and analyze the phase identification and microstructures of the carbon templates. Open porosity and density of the carbon templates were measured by Archimedes principle. The results show that the carbon template is noncrystalline materials. It is in partly graphitized amorphous state, and has a turbostratic structure, and contains minim C-H bonds. With increasing carbonization temperature, the graphitization advances. The pore phase includes channels, macro-pores(d=10~50μm) and micro-pores(d=1~3μm). The channels could prevent the carbon templates from breaking and cracking.
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Effects of Gravity Level on Phase Separation of PbO-B2O3 Glasses
ZHU Dong-Mei,LUO Fa,ZHOU Wan-Cheng,RAY C S,DAY D E
2006 Vol. 21 (4): 855860
Abstract(
2631 )
PDF(798KB)(
1604
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PbO-B2O3 glasses were melted and solidified through drop shaft experiment to explore the phase-separation of the glasses under different gravity conditions. XRD was conducted to determine the phase of samples after phase-separation. The distribution of elements in different samples was compared through EDS analysis and the microstructures were observed by SEM. Results show that both Pb-rich phase and B-rich phase consistently exist in all the glasses no matter how different the gravity level is. For the sample of phase-separation happened under high gravity, the size of separated Pb-rich phase in the top of the sample is much smaller than that in the bottom of the sample, and the homogeneization of elements is the worst due to the difference in density between Pb-rich phase and B-rich phase.
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Preparation and Microwave Absorption Property of BaFe12O19 Encapsulated Porous Glass Particles
ZHANG Yan-Qing,ZHANG Xiong
2006 Vol. 21 (4): 861866
Abstract(
3076 )
PDF(441KB)(
1894
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Barium ferrite encapsulated porous glass particles(BEPG)were prepared with a citrate sol-gel method. The precursors were obtained from barium nitrate,citric acid and porous glass particles and then calcined at 850℃ for 2h with 60℃/h heating rate. The microstructure, complex dielectric constant, complex permeability and microwave absorption of the production were tested by X-ray diffraction, scan election microscope (SEM) and network analyzer. It was found that the BaFe12O19 crystal coated the porous glass particles surfaces well, which in turn exhibited the microwave absorption property. Microwave absorber coating of BEPG with 1.8mm thick was made with latex matrix and the reflection loss was more than -8dB at the range of 5~18GHz. The peak of reflection losses was -15dB at 6 GHz.
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Thermal Stability Investigation of a Newly Developed Sealing Glass as IT-SOFC Sealant
PENG Lian,ZHU Qing-Shan,XIE Zhao-Hui,HUANG Wen-Lai
2006 Vol. 21 (4): 867872
Abstract(
3561 )
PDF(584KB)(
1947
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A sealing glass, based on the SiO2-B2O3-BaO-La2O3-ZrO2-Y2O3 system, was developed for intermediate temperature solid oxide fuel cells (ITSOFCs). The coefficient of thermal expansion (CTE) of the glass is 9.8×10-6/K (RT~631℃), very close to that of 8YSZ electrolyte. The glass shows a very good thermal stability, even after heat-treatment at 700℃ for 300h, little change in CTE detected. The investigations also reveal that the glass is chemically compatible with 8YSZ electrolyte and no obvious interfacial reaction can be observed after the glass contacting with 8YSZ at 700℃ for 300h.
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Synthesis and Electrochemical Performance of Spinel Li4Ti5O12 Electrode Material
RUAN Yan-Li,TANG Zhi-Yuan,PENG Qing-Wen
2006 Vol. 21 (4): 873879
Abstract(
2853 )
PDF(465KB)(
1841
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Spinel lithium titanium composite oxides (Li4Ti5O12) were synthesized by three methods. The effects of the synthesis conditions on the properties of as-synthesized cathode materials were investigated. The crystal structure and the electrochemical performance were characterized by XRD, SEM, LSD, CV, AC impedance and galvanostatically charge-discharge experiments. The results demonstrated that pure Li4Ti5O12 powders could be prepared in short time by using organic solvent. Glucose was added to improve the conductivity of Li4Ti5O12, and the powders showed a good lithiumation performance. The reversible capacity of the material, more than 160mAh·g-1, was delivered at room temperature and 0.2C rate, and the charge-discharge efficiency was almost 100%. After 44 cycles, there was no obvious capacity fade. The charge and discharge results of Li4Ti5O12/LiFePO4 indicated that Li4Ti5O12 was a good candidate material of negative electrode for lithium-ion battery.
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Structure and Characterization of LiFe0.99M0.01PO4/C Electrodes
YANG Shu-Ting,LI Ting-Ju
2006 Vol. 21 (4): 880884
Abstract(
3117 )
PDF(421KB)(
1786
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In latest studies we confirmed that the PAM (polyacrylamide) templated LiFePO4/C composite was nano-structured with better rate property and higher specific capacity, compared with the undoped LiFePO4. In this article we further synthesized metal ions doped phosphates by this templating method, and all the capacities of those LiFe0.99M0.01PO4/C (M=Nd3+、Co3+、Cr3+、Mn3+) composites were enhanced. When discharging at C/3 rate the capacity of LiFePO4/C composite was only 108mAh·g-1, while those of the doped LiFe0.99M0.01PO4/C were respectively 140, 129, 120 and 115mAh·g-1. And the cycliabilities were also stable. Researches show that the conductivities of those doped materials are improved by 5~7 magnitude, which are close to those in references. XRD patterns show that those doped materials still remain their ordered olivine structure.
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Phase Transition and Grain Growth Kinetics of V2O5 and B2O3 Doped Zinc Titanate Ceramics
LIU Xiang-Chun,ZHAO Li-Li,GAO Feng,YAN Xiao-Bin,TIAN Chang-Sheng
2006 Vol. 21 (4): 885892
Abstract(
3016 )
PDF(806KB)(
1902
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Zinc titanate ceramics were prepared by the conventional mixed-oxide method combined with a chemical processing. The effects of V2O5-B2O3 additives on the low-temperature sintering behavior and phase structures of zinc titanate ceramics were investigated; and phase transition mechanism and grain growth kinetics were discussed. The results show that the densification temperature of zinc titanate ceramics can be reduced from 1100 to below 900℃ by V2O5-B2O3 addition. The temperature of complete phase transition from hexagonal ZnTiO3 phase to cubic Zn2TiO4 is lowered from 945 to 930℃ for V2O5-B2O3 co-doped samples. Exaggerated grain growth found is in V-rich region in high-V content samples and disappeared with B2O3 content increasing, at the same time, the grains become uniform. V2O5-B2O3 additive increases the diffusion rate of structure unit and accelerates grains growth. The Tradition Phenomenological Rate Equation (TPRE) model is well fit for characterizing the grain growth kinetics of V2O5-B2O3 co-doped zinc titanate ceramics. According to TPRE, the grain growth activation energy calculated is 315.5kJ/mol, the grain growth expression is shown as G=K0[texp(-315.5×103/RT)]1/7. The Q value decreases for V0-doped zinc metatitanate-based ceramics in microwave region as compared to single-phase hexagonal ZnTiO3 ceramics. The value of dielectric constant depends on the amount of rutile phase from the decomposition of hexagonal ZnTiO3 phase and the bulk density of ceramics.
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Preparation of TaC Anti-ablation Materials by Liquid Precursor
XIANG Hua,XU Yong-Dong,ZHANG Li-Tong,CHENG Lai-Fei
2006 Vol. 21 (4): 893898
Abstract(
3055 )
PDF(634KB)(
1774
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Tantalum carbide materials were prepared by liquid precursor conversion, and the phase compositions and the microscopic structures of samples were characterized by XRD and SEM, respectively. Ta2O5 crystals are formed inside samples by 900℃ treatment, and after 1600~2000℃ high temperature treatment, the samples can almost be converted into tantalum carbide materials whose particles disperse homogeneously throughout the carbon matrix. As temperatures elevate, the graphitization degree of matrix increases and the grain size of tantalum carbide obviously enlarges, all of these are in favor of improving the anti-ablation properties of materials.
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Preparation and Properties of Titanium Diboride Ceramic Matrix Reinforced by Carbon Nanotubes
ZHANG Xing-Hong,HONG Chang-Qing,HAN Jie-Cai,ZHANG He-Xin,MENG Song-He,QU Wei
2006 Vol. 21 (4): 899905
Abstract(
3419 )
PDF(1956KB)(
2020
)
TiB2-xwt%CNTs-5wt%Ni (x=0.1, 0.3, 0.5, 1, 4) composites reinforced by carbon nanotube were fabricated by hot-pressing sintering and the prepared conditions, mechanical properties and microstructure were also investigated. XRD and SEM were used to analyze the phase and fracture surface. The results show that the hardness, bending strength and fracture toughness of the composite reinforced by carbon nanotube are increased distinctly. When the carbon nanotube content is 0.5wt%, the bending strength attains 496MPa; moreover the value of hardness and fracture toughness reaches 20.5GPa and 7.25MPa·m1/2 respectively. The analysis of fracture photograph reveals that the carbon nanotube mainly distributes at the TiB2 grain boundary. The main toughing mechanisms of the TiB2-CNTs-Ni composite are CNTs pulled-out and CNTs bridging.
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Preparation of Si-Al-Zr-O Composite Ceramics with Ultra Fine Grains by in situ Controlled Crystallizing from the Amorphous Bulk
TAN Xiao-Ping,LIANG Shu-Quan,LI Shao-Qiang,TANG Yan
2006 Vol. 21 (4): 906912
Abstract(
3125 )
PDF(942KB)(
1843
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The homogeneous SiO2-Al2O3-ZrO2(SAZ) sol was prepared at 1650~1700℃ and transparent amorphous bulk was obtained by controlling the cooling process. The bulk was treated at 950℃ for 2h to nucleate and at 1100~1250℃ for 1h to crystallize, and SAZ composite ceramics with ultra fine grains were prepared. The effects of heat treatment on the structure and properties of the composite caramics were analyzed by using DSC, IR, XRD, SEM and Vickers indentation techniques. The results show that crystallization of SAZ amorphous bulk begins with t-ZrO2 at about 950℃ and completes at about 1100℃. The main phases are mullite, t-ZrO2. With the increase of crystallization temperatures, the gains grow rapidly from 10~40nm to 0.5μm, and the transformation of zirconia from tetragonal into monoclinic occurs. The values of microhardness and fracture toughness are largest at 1150℃, those are 12.6GPa and 4.32MPa·m1/2 respectively.
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Porous Silicon Nitride Ceramics Prepared by Carbothermal Reduction Method
SHAN Shao-Yun,YANG Jian-Feng,GAO Ji-Qiang,ZHANG Wen-Hui,JIN Zhi-Hao
2006 Vol. 21 (4): 913918
Abstract(
3292 )
PDF(579KB)(
1967
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Porous silicon nitride ceramics with high porosity and uniform pore structure were prepared by carbothermal reduction reaction between low-cost silicon dioxide and activated carbon. The influence of SiO2 particle sizes on their microstructures was investigated. Microstructures and mechanical properties of porous silicon nitride ceramics were studied by XRD, SEM and three-point bending measurement. XRD analysis showed that only β-Si3N4 phase, minor of α-Si3N4 phase and glass phase Y8Si4N4O14 were detected. SEM analysis showed that porous silicon nitride ceramics obtained were composed of rod-like β-Si3N4 grains and uniform pores. Porous silicon nitride ceramics with different porosities and good mechanical properties were fabricated by changing SiO2 particle sizes.
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Mechanism Investigation of Grain Boundary Reoxidation of Barium-lanthanum Titanate Ceramics
PU Yong-Ping,CHEN Shou-Tian,LANGHAMMER H. T.,MAKOVEC D.
2006 Vol. 21 (4): 919926
Abstract(
3285 )
PDF(881KB)(
1895
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BaTiO3 ceramics doped with different La concentrations were sintered under a reducing atmosphere of H2/Ar (1:99), subsequently, reoxidized in oxygen partial pressure P O2=260Pa(mixture with Ar and O2 gas).The behaviour of oxygen in the reoxidation process was investigated by an oxygen coulometry. The microstructure of the raw sintered and reoxidized samples were analysed via TEM. Temperature dependence of resistivity and complex impedance spectroscopy of reoxidized samples at different maximum temperature were measured. Results showed that three oxygen uptake peaks with different onset temperature could be observed during the heating circle. Peak I (onset about 250℃) was attributed to the filling up of oxygen vacancy. Peak II and III were related to the oxidizing of reduced phase. Respectively, Peak II (onset about 800℃) was the formation of oxidized phase at the vicinity of the grain boundaries, which was controlled by grain boundary diffusion. Peak III (onset about 1250℃) was the oxidized phase expanding towards the grain centre and controlled by oxygen bulk diffusion, meanwhile, the rich-Ti phase Ba6Ti17O40 was precipitated. During the transformation from reduced phase to oxidized phase the development of two potential barriers at grain boundaries resulted in the strong PTCR effect.
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Preparation and Tribological Properties of C/SiC Friction Materials
FAN Shang-Wu,XU Yong-Dong,ZHANG Li-Tong,CHENG Lai-Fei,LOU Jian-Jun
2006 Vol. 21 (4): 927934
Abstract(
3209 )
PDF(755KB)(
2086
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The cost effective and high performance carbon/silicon carbide aircraft friction materials were prepared by the combination of chemical vapor infiltration (CVI) and reactive melt infiltration (RMI). The tribological properties of the as-manufactured C/SiC composites were measured under the simulated conditions of normal landing of the aircraft. The test results indicate the more excellent tribological properties of C/SiC composites than that of C/C composites. The average coefficients of kinetic friction and static friction are about 0.34 and 0.41, respectively, the wet fading ratio is about 2.9%, the linear wear rate is less then 1.9μm·cycle-1, and the coefficient of friction is stable. The surface microstructure and wear debris on wear-induced surfaces of C/SiC disks were investigated by optical microscope and SEM. The results indicate that the main wear mechanism of the C/SiC composites is the grain-abrasion. The wear resistance is improved due to the enhanced in-plane shear strength derived from the fiber bundle vertical to the friction surface.
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Preparation of Si3N4/SiO2 Composites with Pressureless Sintering
XU Chang-Ming,WANG Shi-Wei,HUANG Xiao-Xian,GUO Jing-Kun
2006 Vol. 21 (4): 935938
Abstract(
2944 )
PDF(396KB)(
1846
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Si3N4/SiO2 composites were prepared with pressureless sintering. It was found that the Si3N4 particle was effective to suppress the crystallization of cristobalite in the Si3N4/SiO2 composites and contributed to the improvement of the mechanical properties. After sintered at 1370℃ for 2h, the flexural strength of the composites with 5vol% Si3N4 addition reached 96.2MPa, the fracture toughness was 2.4MPa·m1/2. The dielectric constant and loss tangent of the composites was 3.63~3.68 and 1.29~1.75×10-3, respectively.
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Relationship of Composition and Microstructure to Sr/Ba Ratio of BSTN Composite Ceramics
ZHOU Zong-Hui,CHENG Xin,DU Pi-Yi
2006 Vol. 21 (4): 939945
Abstract(
3275 )
PDF(614KB)(
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In our previous work, the BSTN composite ceramics in which two phases of the perovskite (BST) and the tungsten bronze (SBN) coexist were successfully prepared in situ by controlling excess components in BaO-SrO-TiO2-Nb2O5 system. What the formation, microstructure and properties of BST and SBN mainly depend on Sr/Ba ratio is well known. The Sr/Ba ratio may affect the structure and properties of the composite ceramics, too. In this paper, the effects of Sr/Ba ratio on the phase composition and microstructure of the composite ceramics were investigated in detail. X-ray diffractometry (XRD) and scanning electron microscope (SEM) were used to characterize the phase composition and microstructure of the composite ceramics. The results show that the Sr/Ba ratio increases in the perovskite phase and keeps almost constant in the tungsten bronze phase with increasing the content of strontium in the two-phase-coexistence composite BSTN system. The constant Sr/Ba ratio in the tungsten bronze phase is about 0.667. The crystal lattices of the perovskite phase in composite system are larger or smaller respectively than them in pure (1-x)BaO· xSrO·TiO2 system when the Sr/Ba ratio is respectively <0.667 or >0.667. The crystal lattices of the perovskite phase in both systems show the same crystal lattices when the Sr/Ba ratio is 0.667. Affected by the ratio of Sr/Ba required in the tungsten bronze phase in the composite system, the contents of the perovskite phase decreases while the tungsten bronze phase increases with increasing ratio of Sr/Ba. For the same reason, the average grain size of the perovskite phase and the density of the composite ceramics decrease as the ratio of Sr/Ba increases. If the substitution of ions can take place both in the two phases in a composite system with two phases, the substitution will take place first in the phase with higher solubility of ions while it will be restrained in the other phase.
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Properties and Microstructure of ZrB2/C Composites
LI Xiu-Tao,SHI Jing-Li,GUO Quan-Gui,ZHAI Geng-Tai,LIU Lang
2006 Vol. 21 (4): 946952
Abstract(
3047 )
PDF(1514KB)(
1836
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ZrB2/C composites were prepared by a hot-pressing method. The influence of dopants on the flexural strength, thermal conductivity, electrical resistivity and microstructure of these composites was investigated. Results show that the flexural strength and thermal conductivity increase with increasing ZrB2 content up to a maximum of 131MPa and 161W/m·K at 10% addition, respectively. But the electrical resistivity reduces rapidly with increasing the concentration of ZrB2. Correlations between the content of dopant and properties and microstructure of ZrB2/C composites were also discussed.
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Montmorillonite Assembled with Nano-SiO2-particles for Gasoline Desulfurization
ZHAO Shao-Yun,CHEN Ai-Ping,LIU Wei,CHEN Xiao-Ping
2006 Vol. 21 (4): 953957
Abstract(
2672 )
PDF(489KB)(
1674
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Montmorillonite (MMT) is a natural layer-layer material. The template-directed method was used to assemble the nano-SiO2-particles within the layers of MMT. And a desulfurizer for gasoline was developed through loading the transition metal oxide on Si/MMT. The modified montmorillonite was characterized by XRD, TG, TEM, FT-IR and N2 adsorption-desorption. The results of gasoline desulfurization show that nano-particle assembled montmorillonite is an excellent selective adsorbent and its desulfurization ratio is increased by 52% than Na-MMT. The SiO2 pillared montmorillonite modified with rare earth oxides and transition metal oxides nano-particles shows an excellent heat-stability.
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Novel Biodegradable Scaffold of Calcium Phosphate Cement
WEI Jie,LIU Chang-Sheng,HONG Hua,YUAN Yuan,CHEN Fang-Ping
2006 Vol. 21 (4): 958964
Abstract(
3345 )
PDF(1326KB)(
2092
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A novel porous scaffold of calcium phosphate cement with porosity-controllable, pore size-controllable and morphology-controllable was prepared and cell culture with scaffold was studied, also, the biodegradation of the porous scaffold in SBF was investigated. The results reveal that the compressive strength of the porous bone cement can reach 4MPa, the porosity of the scaffold can reach 70%, abundant micropores are on the wall of the macroposes and the pores are interconnected with each other, the cultural cell are attached, dispersed and preferentially proliferated on the surface of the scaffolds materials. The biodegradation ratio increases with the increasing of porosity and decreasing of Ca/P ratio of the calcium phosphate cement. The scaffolds not only have good biocompatibility but also biodegradation. The novel new type of biodegradable Ca-P materials can be used as scaffolds for bone defect repair and tissue engineering.
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Structure and Photo Absorption Property of Coupled Semiconductor ZnFe2O4-TiO2/SiO2
ZHAO Chun,ZHONG Shun-He
2006 Vol. 21 (4): 965971
Abstract(
3084 )
PDF(460KB)(
1877
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ZnFe2O4-TiO2/SiO2 photocatalysts were prepared by a sol-gel method. Their crystal structure, surface compositions and photo absorption properties were investigated by techniques of differential thermal-thermal gravimetric analysis (DTA-TG), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, temperature programmed reduction (TPR) and ultraviolet-visible diffuse reflectance spectroscopy (UV-Vis DRS). The results show that ZnFe2O4 crystallites are highly dispersed on the surface of photocatalysts; a few of Fe3+ ions are embedded in the lattice of TiO2 through the couple of TiO2 and ZnFe2O4. Simultaneously, the excess Zn2+ ions on the surface are gathered to form ZnO. The phase transition of TiO2 starts from bulk and extends to surface with the increase in content of ZnFe2O4. The dispersity of active species, such as TiO2 and ZnFe2O4, is enhanced for the addition of SiO2 and the crystal sizes of TiO2 are smaller than 10nm. The UV absorption limit of photocatalyst tends to bathochromic shift and the percent absorption of visible light is obviously increased by the coupling effect of TiO2 and ZnFe2O4.
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Effects of Surfactants on Dispersion Properties of Nano-Sb2O3 and Nano-Sb2O3/Mica
FENG Li,LIU Jiong-Tian,WANG Jian-Huai,WANG Bin-Guo,SONG Shuo-Jiang
2006 Vol. 21 (4): 972978
Abstract(
2819 )
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1695
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The Sb2O3/mica nanoparticles were prepared by using layered mica as the micro-reaction cell and characterized by means of XRD and TEM. The effects of surfactants on the particle properties and particle-size distributions for both nano-Sb2O3 and Sb2O3/mica nanoparticle were investigated and compared. The results show that after modified by CTAB, Sb2O3 nanoparticles assembled uniformly between mica layers, have a good dispersion property and a narrow size distribution around 5nm, 30nm less than that of Sb2O3 nanoparticles prepared without the addition of mica.
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Characterization and Properties of Si3N4p/Si3N4 Radome Material Prepared by Chemical Vapor Infiltration
LIU Yi,LIU Yong-Sheng,ZHANG Li-Tong,CHENG Lai-Fei,XU Yong-Dong
2006 Vol. 21 (4): 979985
Abstract(
2993 )
PDF(804KB)(
1735
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normalsize Abstract: Si3N4p/Si3N4 radome material was prepared by chemical vapor infiltration (CVI) with SiCl4-NH3-H2 systems. XRF analysis shows the specimen mainly contains Si, N, O three kinds of elements. XRD patterns indicate the sample consists of α-Si3N4, amorphous deposit, noncrystalline SiO2, small amount of β-Si3N4 and Si. Amorphous deposit can be converted into α-Si3N4 and β-Si3N4 by high temperature heat treatment. SEM photographs show weak bonding and large pores exist among granulae. Maximum flexural strength of the samples is 94MPa, and dielectric constants are between 4.1 and 4.8.
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Structure Evolution of Woodceramics by X-ray Diffraction and Raman Spectroscopy
TU Jian-Hua,ZHANG Li-Bo,PENG Jin-Hui,PU Jing-Zhong,ZHANG Shi-Min
2006 Vol. 21 (4): 986992
Abstract(
3330 )
PDF(478KB)(
1683
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The laser Raman spectroscopy and X-ray diffraction (XRD) techniques were applied to investigate the structure of woodceramics (WCS) from carbonizing tobacco stems and phenolic resin at different carbonization temperatures up to 1773K. Experimental results show WCS are non-graphitic carbon consisting of tobacco stems-originated amorphous carbon reinforced by glass-like carbon generated from phenolic resin. With the increase of carbonization temperature, the number of diffraction peaks is increasing, but the interlayer spacing of graphene sheets, d002, is decreasing. As carbonization temperature increased above 973K, the turbostratic crystallites grew very little, but the graphene sheets grew substantially from 2.7 to 5.6nm by Scherrer equation. The Raman spectra of WCS show the known D band which is related to disorder carbon and G band which corresponds to graphite with varying characteristics that are similar to other graphitoidal materials. The integrated intensity ratio R=I D/I G(R-value) which is the degree of disorder of WCS is decreasing with the increase of carbonization temperature above 973K. And the trend of L a calculated by using the Tuinstra-Koening empirical relation is opposite but is consistent by Scherrer equation of XRD technique. The obtained results also indicate that 973K is the turning point temperature for preparation of WCS and the Raman spectroscopy will become a quick method for the structure analysis of WCS.
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Effects of Post-annealing Treatment on the Structural and Optical Properties of Cubic MgxZn1-xO Thin Films Grown on Sapphire
CHEN Nai-Bo,WU Hui-Zhen,XU Tian-Ning,YU Ping
2006 Vol. 21 (4): 993998
Abstract(
3269 )
PDF(427KB)(
1682
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Single cubic-phase MgxZn1-xO(x>0.5) alloy films were synthesized on c-plane sapphire substrates by low temperature physical deposition. The effects of the post-annealing treatment on the structural properties of the films were investigated by the measurements of XRD and transmission spectra. Hexagonal-phase (wurtzite) MgZnO was observed segregating from the cubic-phase Mg0.53Zn0.47O film after annealing at 900℃, while no secondary phase was seen in the samples with Mg fraction exceeding 0.55. Electrical measurement indicates that cubic-phase Mg0.55Zn0.45O films can be used in metal-insulator-silicon (MIS) structures as insulators with low leakage current densities. It could be concluded that the cubic-phase MgxZn1-xO films with x exceeding 0.55 are stable enough to be applied in fabricating high quality optoelectronic devices.
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Preparation of ZnO Films with Rod Crystal Arrays by Aqueous Solution Method
LIU Xiao-Xin1,JIN Zheng-Guo1,WANG Hui2,ZHAO Juan1 LIU Zhi-Feng1
2006 Vol. 21 (4): 9991004
Abstract(
2890 )
PDF(676KB)(
1728
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Highly c-oriented ZnO films were prepared on ZnO buffer-coated ITO substrate by a solution method at 80℃. The effects of precursor concentration and growth time on the morphology of the films were investigated. The structure, morphology were characterized by using X-ray diffraction, transmission electron microscope, scanning electron microscope, field emission scanning electron microscope. The results show that the morphology of ZnO films is strongly dependent on the precursor concentration and growth time, all the ZnO rods belong to the hexagonal wurtzite structure . The growth manner of ZnO is layer by layer. Special lath-like crystals formed by secondary growth when growth time was 48h.
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Influence of Substrate Temperature on the Structure and Optical Properties of ZnO Thin Films Grown by Pulsed Laser Deposition
SUN Bai,ZOU Chong-Wen,LIU Zhong-Liang,XU Peng-Shou,ZHANG Guo-Bin
2006 Vol. 21 (4): 10051010
Abstract(
3604 )
PDF(796KB)(
1944
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Highly c-axis oriented ZnO thin films were fabricated on Si(111) substrates at different substrate temperatures by pulsed laser deposition .X-ray diffraction and atom force microscope were employed to characterize the structure and surface morphology of the deposited ZnO films. The optical properties of the ZnO thin films were investigated by photoluminescence with He-Cd laser and synchrotron radiation as light source. The ZnO thin films grown at 500℃ show good crystallinity and intense UV emission. We also observed the violet emission centering about 430nm of ZnO films excited by synchrotron radiation at 18K. The violet luminescence is ascribed to the defects related to the interface traps existing at the grain boundaries, which probably originate from interstitial zinc(Zn i).
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Li-doped ZnO Ceramic Target Preparation and RF Magnetron Sputtering ZnO Films
CHEN Zhu,ZHANG Shu-Ren,DU Shan-Yi,YANG Cheng-Tao,ZENG Ze-Yu,LI Bo,SUN Ming-Xia
2006 Vol. 21 (4): 10111017
Abstract(
3439 )
PDF(706KB)(
1713
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We successfully prepared high quality Li-doped ZnO ceramic targets with 70mm in diameter and 10~15mm in depth by solid-state reactions. The paper studied the influence of different concentration of Li2CO3 on the electrical properties of ZnO ceramic target. By comparing and analyzing the IR( insulative resistivity ) and tgδ(dielectric loss), the optimum concentration of Li2CO3 doped in ZnO ceramic target was obtained(2.2%mol ratio). And the optimum process for preparing ZnO-Li2.2% ceramic target was also realized through the investigation of physics and electrics of ZnO ceramic under the different sintering temperatures and molding pressure treatments. By using Li2.2%-doped ZnO ceramic as the target, the ZnO films with highly c-axis (002) preferred orientation were grown by RF magnetron sputtering on Si(100), glass and Pt(111)/Ti/SiO2/Si(100) substrates respectively.
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Effects of Process Conditions on Electric Properties of Hot-filament CVD Diamond Films
LIU Jian-Min,XIA Yi-Ben,WANG Lin-Jun,ZHANG Ming-Long,SU Qing-Feng
2006 Vol. 21 (4): 10181024
Abstract(
2720 )
PDF(580KB)(
1607
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By using different deposition conditions, four CVD diamond films with different qualities and orientation were grown by the hot-filament CVD technique. The dielectric properties of these films before and after annealing were investigated in detail. A study of the relationship between the different deposition conditions and annealing process with respect to the dielectric properties was carried out. These CVD diamond films were also characterized with SEM, Raman spectroscope, XRD, I-V characteristics and impedance analyzer. The annealing process reduces the hydrogen contamination of the films and therefore improves the film quality. CVD diamond films with high quality and good electric properties such as a resistivity of 1.2×108Ω·cm at a bias of 50V, a dielectric constant of 5.73 and a dielectric loss of 0.02 at a frequency of 2MHz were obtained.
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