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  • Nanomaterials, Thin Films and Coatings
    XUBao-qiang(徐宝强),DENGHua(邓 桦),DAIYong-nian(戴永年),YANGBin(杨 斌),
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 667-670.
    A novel aerosol method for the production of alighed carbon nanotubes was presented. Multi-walled carbon nanotubes (MWNTs) with fairly uniform diameters and aligned MWNT bundles were obtained by using solutions of organometallics such as ferrocene in hydrocarbon solvents. A hollow and multi-walled structure was observed with diameter ranging from 15 to 50 nm, leading aspect ratio to be over 200. The quality of the product is dependent on the pyrolysis temperature, carrier gas flow rate and the catalyst precursor concentration. For the sample synthesized at 900 ℃, G/D is 1.81. G/D of samples obtained at 850 ℃ and 800 ℃ are 1.18 and 0.77, respectively. The inclusion of acetylene to an atomized spray of ferrocene in hexane yield aligned MWNT bundles with a narrow diameter distribution.
  • Nanomaterials, Thin Films and Coatings
    LIANGShu-quan(梁叔全),JIAChun-yan(贾春燕),TANGYan(唐 艳),ZHANGYong(张 勇),ZHONGJie(钟 杰),PANAn-qiang(潘安强)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 675-679.
    Carbon nanotubes (CNTs)/epoxide resin composites were prepared, the mechanical and electrical properties of the composites were investigated. The effects of concentration and dispersion state of CNTs on the tensile strength, tensile modulus and electrical resistance of the composites were studied. The results indicate that the CNTs can be dispersed well in the epoxide resin matrix by ultrasonic method, and the mechanical and electrical properties of epoxide resin matrix can be improved significantly. The tensile tests show that the tensile strength and tensile modulus are higher than those of epoxide resin if the content of CNTs is less than 1.75% (mass fraction). When the content of CNTs is 0.75%, the conditional best results are obtained, the tensile strength of the composite is the highest, increased by 18.3% and the tensile modulus is increased by 20.5% compared with the matrix. With the increase of CNTs, the electrical resistance of the composites decreases greatly, while the conductivity of the composite increases. The percolation threshold values of electrical characteristic transformation for this composite material were determined for the first time.
  • Nanomaterials, Thin Films and Coatings
    XIAOLi(肖 利),FANGZheng(方 正),QIUGuan-zhou(邱冠周),LIUJian-she(柳建设)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 680-684.
    The sol-gel method was used to prepare three kinds of nanometer magnetic particles, such as the nano-cobalt ferrite oxide powders and those doped by LaCl3∙nH2O. In the thermo-decomposition process of the precursors to get these magnetic particles, TG/DTG was applied to investigate their character. The prepared magnetic particles with average diameter less than 100 nm were characterized by XRD and TEM. The results show the difference between the activation energies of these particles in different thermo-decomposition stages, even not in the same stage for different samples. The cobalt ferrite doped with La3+ affects its saturation magnetization(ms) and coercive force(Hc). As CoCl2∙6H2O is partly substituted by La3+, the value of Hc decrease with the increase of ms. When FeCl2∙4H2O is partly substituted by La3+, Hc increases obviously. The three kinds of nanometer magnetic particles were doped into polyethylene glycol-20000 (peg-20000) with different ratios respectively to obtain compound substance with optimal conductivity of 0.686 S/m.
  • Nanomaterials, Thin Films and Coatings
    HEXin-kuai(何新快),QIUGuan-zhou(邱冠周),CHENBai-zhen(陈白珍),ZHOUNing-bo(周宁波),WULu-ye(吴璐烨),XULi-jian(许利剑)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 685-691.
    Nanocrystalline chromium coating was prepared by pulse electrodeposition from trivalent chromium bath containing carboxylate-urea as complexing agent. The effects of electrodeposition parameters such as current density, bath temperature and solution concentration on the thickness and electrodeposition velocity of Cr deposited films were investigated. The crystallographic structures, morphology and chemical composition of Cr deposited films were analyzed by means of XRD, SEM and EDS. The results indicate that the deposited films with thickness up to 11.2 µm possess a smooth and clean appearance, and the grain size is less than 100 nm. The coating is pure chromium and the Cr deposit has face-centered cubic (fcc) structure and exhibits a (210) growth preference. Both the electrodeposition velocity and thickness exist maximum under different concentration complex agents, ureas, acetates, different temperatures and current densities. Compared with direct current electrodeposition, the thicker coating and finer grains can be obtained at lower temperature and current density by pulse electrodeposition. The electrodepostion velocity is about 0.24 µm/min, which is faster than that by direct current electrodeposition. In 1 mol/L H2SO4, 3.5% NaCl and 10% NaOH solution, corrosion potential of Cr pulse-deposited film is about 100 mV higher than that of direct current. Corrosion and passivation current densities are lower and the nanocrystalline exhibits better corrosion resistance.
  • Nanomaterials, Thin Films and Coatings
    ZhANGWen-yan(张文彦),LIGuang-zhong(李广忠),LIYa-ning(李亚宁),YUZheng-tao(于振涛),XIZheng-ping(奚正平)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 692-695.
    The vertically aligned highly ordered TiO2 nanotube arrays were fabricated by potentiostatic anodization of biologic Ti alloys(TLM) and pure Ti substrates, followed by annealing at 480 and 550 ℃ for 6 h. High-resolution scanning electron microscopy (SEM) was applied to characterize the original films. The phase of the film was characterized by XRD. The interfacial adhesion and bond strength between thin films coating and substrate were tested by scratch method. The results show that the films on the TLM alloy have high adhesion strength compared with them on pure Ti.
  • Nanomaterials, Thin Films and Coatings
    LIWei-xue(李维学),CUIYong-fu(崔永福),HAOYuan(郝 远),CHENTi-jun(陈体军),DAIJian-feng(戴剑锋),W
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 696-699.
    The experimental apparatus by self-designed was used, Fe/Co particles encapsulated in multi-walled carbon nanotubes (MWCNTs) were prepared by the method of anodic arc discharging plasma. The products were characterized by transmission election microscopy, Raman spectroscopy and X-ray diffractometry. The magnetic properties of the products were characterized with vibration sample magnetometer. The TEM results show that MWCNTs have little impurity and good particles size, and Fe/Co with high continuity encapsulaties in carbon nanotubes. The saturated magnetization (σs), remanence (σm) and coercivity (Hc) of the sample are 17.30 A/(m·kg), 3.96 A/(m·kg) and 31 521.60 A/m, showing better ferromagnetism compared with the bulk Fe/Co. The optimal conditions in this case are as follows: a helium gas atmosphere of 6.0×104 Pa, an arc current of 70 A, a voltage drop of 24 V, a constant distance of about 2 mm between the anodes and cathode, metallic powder contents of Fe and Co of 15.0% (mass fraction) and 15.0%, respectively, and well cooled electrodes and collector. This process is a convenient and effective that Fe/Co particles can be encapsulated in MWCNTs.
  • Nanomaterials, Thin Films and Coatings
    DengHua(邓 桦),K.Cheuk,ZHENGWei-ning(郑卫宁),WENChen(文 晨),XIAOChang-fa(肖长发)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 700-703.
    A low temperature preparation of nano TiO2 using sol-gel method was proposed. The antibacterial properties of the treatment solution and the treated cotton fabrics obtained via a dip-padding process were evaluated. XRD pattern shows that the nano TiO2 produced is an anatase phase. Aqueous nano-dispersion of the nano TiO2 exhibites positive results as an antibacterial finishing agent for cotton fabrics. The treatment solution possesses antibacterial rates of over 92% and 88.9% against Escherichia coli and Bacillus subtilis, respectively. The treated fabrics are slightly downgraded but still maintained over 89% and 83% of reduction towards the same bacteria. After washing for 50 times, the antibacterial performances of the treated fabric still remains at a relatively high level, indicating the durable characteristic of nano TiO2 treatment.
  • Nanomaterials, Thin Films and Coatings
    CHENChuan-sheng(陈传盛),CHENXiao-hua(陈小华),YIBin(易 斌),ZHANGGuo-bin(张国斌),LIFu-jin(李富进),LUOHui-shan(罗慧
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 704-707.
    In order to improve optical property of the multi-walled carbon nanotubes (MWNTs), MWNTs were decorated with europium oxide (Eu2O3) nanoparticles by using co-deposition method. The MWNTs/Eu2O3 composites were examined by XRD, scanning electron microscopy, transmission electron microscopy, and VUV-Vis Luminescence spectroscopy and citric acid (CA) molecules were introduced onto the surface of MWNTs. The results show that there are many oxygenated functional groups on the surface of the MWNTs after the treatment of mixture acid, such as carboxy, hydroxl, carbony and amidocyanogen. The results of electron microscopy illuminate that the MWNTs are coated by nano-europium oxide after annealed at 750℃. The MWNTs/Eu2O3 composite emits much strong red light at about 610 nm under UV excitation.
  • Nanomaterials, Thin Films and Coatings
    YANGLi(杨 丽),HEHuan(何 欢),LIUHong-bo(刘洪波),ZOUYan-hong(邹艳红),CHENHui(陈 惠),ZHOURu-quan(周如全)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 708-712.
    FeNi/graphite nanocomposites were prepared by reducing FeCl3-NiCl2-GICs in H2. The elemental composition, structure, magnetic and microwave absorption of FeNi/graphite nanocomposites were investigated using X-ray diffraction, energy dispersive spectra, hysteresis loop and electromagnetic parameter analysis. The results show that with the increase of the reduced temperature, the number and size of particles of FeNi increases, and the FeNi /graphite nanocomposites changes to soft magnetism. FeNi /graphite nanocomposites bear microwave absorption properties. With the increase of the thickness of the sample, the matching frequency tends to shift to the low frequency region, and theoretical reflection loss becomes less at the matching frequency. Microwave absorption property in the low frequency region of FeNi/graphite nanocomposites prepared at 600 ℃ (FeNi/C600) is the best. When the thickness is 2 mm, the maximum theoretical reflection loss of FeNi/C600 is −4.3 dB and the matching frequency is 3.5 GHz.
  • Nanomaterials, Thin Films and Coatings
    LIFa-tang(李发堂),LIURui-hong(刘瑞红),ZHAODi-shun(赵地顺),SUNZhi-min(孙智敏),QUZhi-ming(曲志明)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 713-715.
    Nano-F/Fe3+/TiO2 particles were prepared by hydrolysis of tetrabutyl titanate in a mixed CF3COOH-Fe(NO3)3-H2O solution. The photocatalytic decomposition of methylene blue in aqueous solution was used as a probe to evaluate their photocatalytic activities. The powders were characterized by X-ray diffraction (XRD), energy dispersion X-ray spectrum (EDS) and Brunauer-Emmett-Teller (BET) surface area analysis. The results show that F and Fe 3+ are doped into TiO2. The F and Fe3+ doping can help to enhance the nano-TiO2 photocatalytic activity greatly. The appropriate codoping conditions for F-Fe are n(F)/n(TiO2)=2%, n(Fe)/n(TiO2)=0.05%, and the degradation rate of methylene blue at 1 h is improved from 73.2% to 87.5%. The codoped nano-F/Fe3+/TiO2 particles have higher BET specific surface area, smaller crystallite size and higher photocatalytic activity than those of undoped TiO2 particles.
  • Nanomaterials, Thin Films and Coatings
    FANCai-mei(樊彩梅),TANGQi(唐 琦),WANGYun-fang(王韵芳),HAOXiao-gang(郝晓刚),LIANGZhen-hai(梁镇海),SUNYan-ping(孙彦平)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 716-720.
    The nano-TiO2 doped with Er3+ were prepared from Ti(OC4H9)4 by sol-gel method, and the effect of Er3+ dopant on microstructure and photocatalytic activity of nano-TiO2 was studied. The phase composition and crystallite sizes of Er3+-doped TiO2 samples were analyzed by X-ray diffractometry (XRD) and transmission electron microscopy (TEM). The photocatalytic activity of Er3+-doped TiO2 was investigated at different doping concentrations and different heat treatment temperatures in the photocatalytic degradation of phenol with 365 nm wavelength ultraviolet light irradiation. The results show that both the anatase phase and rutile phase are formed in doped TiO2. Er3+ doping hinders the crystal transformation and makes the TiO2 crystallite size change smaller as well as increases the photocatalytic activity of TiO2 greatly. When Er3+ doping concentration is 1.2%(mass fraction) and the heat treatment temperature is 700 ℃, the photocatalytic activity of Er3+-doped TiO2 is favorite in the experimental range. The photocatalytic activity is enhanced by about 18% compared with that of the pure TiO2 and almost approaches the photocatalytic activity of P25-TiO2.
  • Nanomaterials, Thin Films and Coatings
    DONGLin(董 林),JIAXiao-lin(贾晓林),TONGYan-hong(童艳红),MAYing(马 莹),LIUJing-wei(刘京伟)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 721-724.
    ZnO nanorod arrays with quite homogeneous size and shape were fabricated by introducing ZnO seed-layer as nucleation centers on the soft ITO substrates prior to the hydrothermal reaction. The samples were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction and photoluminescence method. After the ZnO seed-layer is introduced, the resulting deposits on the substrates develop into nanorods, and the diameter decreases obviously to about 100 nm. Influences of the coated nanocrystal seed nuclei on the morphology of ZnO nanorod arrays were discussed. The results show that each nanorod is monocrystalline with wurtzite-type structure and oriented in c-axis direction. The increase of the intensity ratio of ultraviolet to visible emissions in room-temperature photoluminescence spectra and the decrease of the ultraviolet PL linewidths show the improvement of the quality of ZnO nanorods. A simple and effective method to synthesize ZnO nanorod arrays with fairly uniform size and shape on soft substrates is dip-coating ZnO nanocrystals prior to hydrothermal reaction, and it may be also feasible for the fabrication of other small-size metal oxide nanostructures on soft substrates.
  • Nanomaterials, Thin Films and Coatings
    JIANGJian-jun(江建军),MAQiang(马 强),BIEShao-wei(别少伟),DUGang(杜 刚),TIANBin(田 斌),FENGZe-kun(冯则坤),HEHua-hui(何华辉)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 725-729.
    A series of multilayers of Co36Fe46B18/SiO2 were fabricated by DC/RF magnetron sputtering, and further post-annealed in vacuum magnetic field at 200℃ for 2 h. The results show that the microstructures and electromagnetic properties of Co36Fe46B18/SiO2 multilayer films can be altered by varying the thickness of CoFeB and the process of annealing. High permeability along with high magnetic loss in the GHz frequency range is achieved in the optimized discontinuous multilayer films. Both real and imaginary parts of the complex permeability are larger than 260 at 1.6 GHz for this film, and the resistivity is as high as 1.4 mΩ∙cm. The discontinuous Co36Fe46B18/SiO2 multilayers are supposed to serve as the microwave absorbers and EMI shielding materials in GHz range.
  • Nanomaterials, Thin Films and Coatings
    WANG Xin-jian(王新建), DONG Xian-ping (董显平), LIU Jia-cong(刘嘉聪), JIANG Chuan-hai(姜传海)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 730-735.
    The thin films of pure Cu and Cu-2.18%Cr (mole fraction, %) were deposited on Si(100) substrates. Then the samples were vacuum-annealed at 573−773 K to investigate the effect of Cr on the microstructural and electrical characteristics of Cu/Si systems. The XRD results reveal that the annealed Cu(Cr) film has a strong (111) texture. The results of AFM and FESEM indicate that the Cu(Cr) films with insoluble Cr have compact surface morphology and fine columnar microstructure. Upon annealing, most Cr segregates at the surface and interface. The residual insoluble Cr is enriched in amorphous structure between Cu grains and retards the crystallization of annealed Cu(Cr) films. As a result, the minimal annealing resistivity of the Cu-2.18%Cr film is 2.76 μΩ·cm at 773 K, which approaches to 2.55 μΩ·cm of the Cu film at 673 K. Significant changes in the microstructure and properties are obtained by adding Cr to Cu films after annealing.
  • Nanomaterials, Thin Films and Coatings
    .KeyLaboratoryofAutomobileMaterials,MinistryofEducation,CollegeofMaterialsScienceandEngineering, JilinUniversity,Changchun00,China;
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 736-740.
    Nanocrystalline copper films were prepared on the glass by electroless plating technique. The surface characterization of copper films with different deposition time was studied by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). The results indicate that the copper films have a (111) texture. A continuous and smooth film forms on the glass substrate at deposition times of 5 min. The surface roughness of as-deposited copper films becomes rougher with large nodules as the deposition time increases. According to Fuchs–Sondheimer (F–S), Mayadas–Shatzkes (M–S) theory and a combined model, the grain boundary reflection coefficient (R) is calculated in the range of 0.40−0.75. The theoretical analysis based on the experimental results show that the grain boundaries contribute mainly to the increase of electrical resistivity of nanocrystalline copper film compared with the film surfaces.
  • Nanomaterials, Thin Films and Coatings
    TANGMing-hua(唐明华),ZHOUYi-chun(周益春),ZHENGXue-jun(郑学军),WEIQiu-ping(魏秋平),CHENGChuan-pin(成传品),YEZhi
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 741-746.
    A detailed investigation about the dependence of microstructure and electrical properties on annealing temperature was carried out for cerium oxide(CeO2) ultra-thin films (18 nm to 110 nm) on n-type Si(100) substrates by RF magnetron sputtering. Substrate temperature was kept constant at 400 ℃ for all samples. The as-deposited films were subsequently annealed in air ambient at 700, 800 and 900 ℃ for 1 h respectively. The crystallinity and surface morphology of the CeO2 films were analyzed with X-ray diffractometer(XRD), scanning electron microscope(SEM), atomic force microscope(AFM) and Raman scattering measurement. Electrical properties of the Au/CeO2/Si/Au structure were examined by high frequency capacitance—voltage (C—V) characteristics at 1 MHz and leakage current density—electric field (J—E) characteristics. A Raman peak of the CeO2 thin films was seen at 463 cm−1. From C—V data, these films exhibit dielectric constants ranging from 18 to 23, the hysteresis width (ΔVFB) ranging from 0.015 V to 0.12 V and the density of trapped charges ranging from 1.45×1011 to 3.01×1011 cm−2. A leakage current of 4.75×10−8 −9.0×10−7 A/cm2 at  2 MV/cm was observed. The experimental results show that the CeO2 buffer layers are suitable for non-volatile metal- ferroelectric-insulator-semiconductor(MFIS) structure field-effect-transistors(FETs) memory applications.
  • Nanomaterials, Thin Films and Coatings
    YE Qi(叶  奇), KANG Zhi-xin(康志新), LI Yuan-yuan(李元元)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 747-751.
    The 6-mercapto-1, 3, 5-triazine-2, 4-dithiol monosodium (TTN) compound was used to fabricate an organic film on pure copper. The polymer plating process of TTN on pure copper in Na2CO3 aqueous solution and the growth mechanism of poly(6-mercapto-1, 3, 5-triazine-2, 4-dithiol) (PTT) film were studied by means of cyclic voltammetry. The polymer plating under galvanostatic mode at 0.05 mA/cm2 was conducted to generate PTT film on pure copper in the same electrolyte with different polymer-plating time. The film mass was determined by electronic balance and the insoluble fraction in tetrahydrofuran (THF) Is tested. The performance of organic film formed on copper surface was investigated preliminarily by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). It is found that a slight peak measured at 0 V vs SCE attributes to the oxidation of copper and generated Cu+ or/and Cu2+ to produce Cu-TTN complex, then a strong oxide peak is observed at 0.311 V vs SCE due to the polymerization of TTN for the increase of the film thickness. Electrochemical measurement results reveal that 10 min is an optimum polymer-plated time to obtain high quality film. The results of potentiodynamic polarization show that current density decreases from 1.85 μA/cm2 for bare copper to 0.168 μA/cm2 for polymer-plated copper while polymer-plated time is 10 min. The charge transfer resistances of bare copper and polymer-plated copper are 937 Ω∙cm2 and 11.12 kΩ∙cm2, respectively. The film capacitor for polymer-plated copper is as low as 1.82 μF∙cm2. The EIS results confirm the results of potentiodynamic polarization and reveal that a homogenous and compact film is obtained by polymer plating technique.
  • Nanomaterials, Thin Films and Coatings
    ZHENGXue-jun(郑学军),ZHANGJun-jie(张俊杰),ZHOUYi-chun(周益春),TANGMing-hua(唐明华),YANGBo(杨 博),CHENYi-qiang(陈义强)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 752-755.
    Metal-ferroelectric-insulator-silicon (MFIS) capacitors with Bi3.15Nd0.85Ti3O12 (BNT) ferroelectric thin film were simulated using a commercial software Silvaco/Atlas, and the effects of applied voltage and insulator layer on capacitance−voltage (C−V) hysteresis loops and memory windows were investigated. For the MFIS capacitors with CeO2 insulator, with the increase of applied voltage from 2 V to 15 V, the C−V loops become wider and memory windows increase from 0.15 V to 1.27 V. When the thickness of CeO2 layer increases from 1 nm to 5 nm at the applied voltage of 5 V, the C−V loops become narrower and the memory windows decrease from 1.09 V to 0.36 V. For MFIS capacitors with different insulator layers (CeO2, HfO2, Y2O3, Si3N4 and SiO2), the high dielectric constants can make the C−V loops wider and improve the capacitor’s memory window. The simulation results prove that Silvaco/Atlas is a powerful simulator for MFIS capacitor, and they are helpful to the fabrication of MFIS nonvolatile memory devices.
  • Nanomaterials, Thin Films and Coatings
    DENG Lian-wen(邓联文), HUANG Xiao-zhong(黄小忠), ZHOU Ke-sheng(周克省), YANG Bing-chu(杨兵初)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 756-759.
    From the point of view of application in the microwave band, the theoretic and experimental researches of nanostructural magnetic films were carried out. Micromagnetic structure of the nano-magnetic film was simulated by the finite element method. The typical micromagnetic was obtained. Corresponding experiments were also done aiming at the Co40Fe40B20-SiO2 nano-granular films. The results show that the characteristics of nano-magnetic film correspond with the micromagnetic ripple theory. The microwave permeability of nano-magnetic films deduces and well fits the Landau-Lifshitz-Gilbert (LLG) equation. The films present large microwave permeability and high resonant frequency (μ′ and μ″ at 2 GHz are about 100 and 40 respectively and the resonant frequency is about 2.8 GHz). The additional peak of μ″ originated from perpendicular anisotropy and micromagnetic ripple structure can be suppressed by the annealing process. Thus, the microwave complex permeability spectra of these nano-magnetic films can be tailored for different applications.
  • Nanomaterials, Thin Films and Coatings
    XIAOLai-rong(肖来荣),XULiang-liang(许谅亮),YIDan-qing(易丹青),LIUHui-qun(刘会群),CAIZhi-gang(蔡志刚),
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 760-765.
    A silicide coating was prepared on the surface of the Nb521 alloy by the complex pack cemented method. The oxidation resistance properties of the present coating were examined by the static oxidation tests at 1 700 ℃ in air. The compositions and the microstructures of the coating before and after test were characterised and analysed through scanning electron microscopy (SEM), X-ray diffraction analysis (XRD), energy dispersive X-ray spectrometry (EDS) and electron probe microanalysis (EPMA), respectively. The present silicide coating can provide an effective protection for the Nb alloy for 25 h at 1 700 ℃ in air. The results show that the oxidation kinetics of the present silicide coating is parabolic. The diffusion of Si leads to the phase transformation and evolution during the oxidation.
  • Nanomaterials, Thin Films and Coatings
    ZHUDong-mei(朱冬梅),LOUXia(娄 霞),LUOFa(罗 发),XIONGLiang-ming(熊良明),ZHOUWan-cheng(周万城)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 766-769.
    A series of BaO-La2O3-B2O3 (BLB) glass coats on the Ti-based alloy substrates were developed at different temperatures for different times. The BLB glasses were analyzed by differential thermal analysis (DTA) and thermal mechanical analysis (TMA) to determine the crystallization temperature and coefficients of thermal expansion (CETs) of the glass. The tensile strength and microstructure of the glass coats were analyzed and the effects of the coating condition on the tensile strength and microstructure were discussed. The results show that the CETs of the borate glass at different temperatures match with those of Ti-based alloy, and the difference between the borate glass and Ti-based alloy at each temperature is below 5%. The spreading area in N2 atmosphere is much larger than that in air atmosphere, indicating that N2 atmosphere is helpful for the wetting of borate glass to Ti-based alloy. The tensile strength of the glass coats can reach as high as 28.42 MPa, meeting the requirements for the coat binder. With the increase of coating time, the tensile strength of coats increases firstly while then decreases. The coat prepared at 730 ℃ for 30 min is fairly smooth and complete, while the other coats contain lots of defects such as large or small uncoated region. It is believed that the coating temperature of 730 ℃ and coating time of 30 min are the proper coating conditions to prepare BLB glass coats.
  • Nanomaterials, Thin Films and Coatings
    PANYong(潘勇),JIANGShan(江山),DAICui-ying(戴翠英),TANGTian(唐甜),ZHOUZhao-fen
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 770-775.
    Nanocrystalline nickel coatings were prepared by both direct current(DC) and pulse current(PC) jet-electrodeposition. The influences of current density and jet velocity on the surface morphology, microstructure and preferred orientation of the coatings obtained were investigated by SEM, TEM and XRD. It is found that the current density strongly affects the microstructure of the nickel coating. An increase of the DC current density results in a slight increase of the grain size and preferred orientation progressive evolution (i.e. from (111) to (200)), whereas an increase of the PC current density leads to a certain decrease of the grain size and preferred orientation change (i.e. from (111) to a strong (220)). Moreover, jet velocity shows no significant effect on the grain size and preferred orientation for the nanocrystalline coatings obtained in both DC and PC within the range of jet velocity studied.
  • Nanomaterials, Thin Films and Coatings
    ZHAO Zi-yu(赵紫玉), ZHANG Su-zhi(张素芝), FANG Jian-cheng(方建成)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 776-779.
    Two different technologies, electro-brush plating and arc spraying, were employed to deposit copper film and brass coating on the surface of nonmetal artworks, respectively. The principles of the oxidizing corrosion and coloring were researched. The nonmetal artworks attain vivid and ancient bronze effect by the surface deposition and surface coloring processing. By using this technology, the problems of difficulty-to-plating copper and difficulty-to-archaizing for the large outdoor sculptures and other artworks can be solved, and it has prospective application due to low investment.
  • Nanomaterials, Thin Films and Coatings
    ZHANGShu-juan(张淑娟),LIMing-sheng(李明升),FENGChang-jie(冯长杰),LIUTing-zhi(刘庭芝),DUOShu-wang(多树旺)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 780-784.
    Cr-Al-N ternary coatings were deposited by arc ion plating method using isolated Cr target and Al target. The influence of AlN content on the phase change was studied by synthesizing Cr1−xAlxN coatings with different x values. The effects of substrate negative bias on the surface morphology, deposition rate and phase structure were investigated. As the aluminum content increases, the structure of (Cr1−xAlx)N changes from B1(NaCl) phase to B4(wurtzite) phase. The critical content of AlN solubilized in B1(NaCl) lattice is close to 0.7. With the increasing pulse negative bias, the deposition rate decreases constantly, the droplet contamination is more serious, the ion-etching effect on coating surface is more obvious, and the change of preferred orientation and the shift of XRD peak take place.
  • Nanomaterials, Thin Films and Coatings
    ZHANGShu-fang(张淑芳),WANGFang-yuan(王方圆),ZHANGRong-fa(张荣发),LIMing-sheng(李明升),ZHAOFang(赵芳),ZHOUChong(周冲)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 785-788.
    In a basic solution containing 10 g/L NaOH, the thickness, morphology and corrosion resistance of anodic coatings formed in solutions without and with additions of Na2SiO3, Na2CO3, Na2B4O7 and Na2SnO3 were separately determined and evaluated. The results show that the electrolytes used above take part in the coating formation and the obtained anodic coatings contain elements from the electrolytes. These electrolytes, especially Na2SiO3 and Na2B4O7, contribute to the film thickness. The coating uniformity obtained by addition of Na2SiO3 is the best, while Na2CO3, Na2B4O7 and Na2SnO3 decrease the number of pores per area on the coatings surface though they worsen the uniformity of the anodic coatings. In addition, the anodic coatings formed in solutions with addition of Na2CO3 or Na2SnO3 exhibit loose and net-like structure. Na2SiO3 and Na2B4O7 can significantly improve the corrosion resistance of the anodic coatings while Na2CO3 and Na2SnO3 have minor effects on improving the coating corrosion resistance.
  • Nanomaterials, Thin Films and Coatings
    ZHANGRong-fa(张荣发),XIANGJun-huai(向军淮),CHAOQiang-hua(巢强花),DUOShu-wang(多树旺),LIMing-sheng(李明升),LIWen-kui(李文
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 789-793.
    In a basic solution containing 18 g/L Na2SiO3, the anodizing of AZ91HP magnesium alloy was investigated with and without addition of phytic acid (C6H18O24P6). The thickness, composition and morphologies of anodic coatings formed at different concentrations of C6H18O24P6 were determined. The corrosion resistance of anodized samples was evaluated by salt spray test in 5% (mass fraction) NaCl solution. The results show that C6H18O24P6, which is harmless and environmentally friendly, greatly affects the properties of anodic coatings. Under the same electric parameters, the final voltage increases with the concentrations of C6H18O24P6. The coating thickness slightly increases from 8 mm formed in the base electrolyte without C6H18O24P6 to 9−10 mm in C6H18O24P6 solution. The P content and color of anodic coatings separately increases and darkens with the addition of C6H18O24P6. After the anodizing solutions were changed from 0 to 16 g/L addition of C6H18O24P6, the largest size of micropores decreases from 4 mm to   3 mm, while the number of micropores per area on coating surface decreases from 0.076 to 0.047 mm−2. The salt spray test shows that C6H18O24P6 can improve the corrosion resistance of the anodic coatings and the coating formed in the electrolyte containing 12 g/L C6H18O24P6 exhibits the highest corrosion resistance.
  • Nanomaterials, Thin Films and Coatings
    JIANGSheng-lin(姜胜林),ZHANGHai-bo(张海波),XIETian-tian(谢甜甜),FANMao-yan(范茂彦),ZENGYi-ke(曾亦可),LÜWen-zhong(吕文中)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 794-797.
    In order to get high-performance low voltage varistors, Cr2O3 doped ZnO ceramic thick films were fabricated by modified sol-gel process. The precursors were fabricated by dispersing doped-ZnO ceramic nano-powders in the sols, which were prepared by dissolving zinc acetate dihydrate into 2-methoxyethanol and stabilized by diethanolamine and glacial acetic acid and doped with a concentrated solution of bismuth nitrate, phenylstibonic acid, cobalt nitrate, manganese acetate and chromium nitrate. The results show that ZnCr2O4 phase can form in ZnO based ceramic films doped 1.0% (mole fraction) Cr2O3. Three secondary phases, such as Bi2O3, Zn7Sb2O12, and ZnCr2O4 phases, are detected in the thick films. The Raman spectra show that the intensity and the position of Raman bands of Zn7Sb2O12 and ZnCr2O4 phases change obviously with increasing Cr2O3 doping. The nonlinearity coefficient α of ZnO thick films is 7.0, the nonlinear voltage is 6 V, and the leakage current density is 0.7 µA/mm2.
  • Nanomaterials, Thin Films and Coatings
    ZENG Hao-ping(曾好平)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 798-802.
    A two-dimensional axisymmetric model, with 8700 and 7500 quadrilateral elements for the fluid and substrate zone separately, was developed to simulate the impacting and flattening process. The volume of fluid technique was employed to track the interface between the air and droplet. The relationships between the droplet pre-impact parameters and the flattening time as well as the flattening ratio were investigated by altering one of the parameters while remaining the others unchanged. The results show that the droplet height reaches its minimum value at approximately half of the spreading time, which also indicates the finish of vertical fluid flow at that time. The flattening ratio increases with the increase of the three pre-impact parameters-droplet diameter, temperature and velocity, even though the flattening time decreases when the droplet velocity increase.
  • Nanomaterials, Thin Films and Coatings
    WANG Guang-jun(王光君), WANG De-zhi(王德志)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 803-807.
    Mo powders with average particle size of 3 μm were attempted to coat with copper by electroless plating technique. The effect of the solution composition and plating conditions on the electroless copper plating was studied. The uncoated and coated powders were subjected to the microstructural studies by SEM and the phases were analyzed by XRD. The results indicate that the Mo powders are coated with copper, at the same time, Mo-Cu composite powders with Cu content ranging from 15% to 85% (mass fraction) can be obtained. The optimal values of pH, HCHO concentration and temperature are in the ranges of 12−13, 22−26 ml/L and 60−65 ℃, respectively. The diffusion-shrinkage autocatalytic model is suggested for the growth mechanism of electroless coating over the surface.
  • Nanomaterials, Thin Films and Coatings
    SHI Guo-dong (史国栋), LIANG Jun (梁  军), CHEN Gui-qing (陈贵清), DU Shan-yi (杜善义)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 808-813.
    Two substrates with surface roughness (Ra) of about 1.6 and 0.8, respectively, were employed to fabricate two NiCoCrAl/YSZ microlaminates by using EB-PVD method. The average ceramic-layer thicknesses of the two NiCoCrAl/YSZ microlaminates are different, about 0.9 μm and 1.2 μm, respectively, but their average metal-layer thicknesses are equal, about 5 μm. The microstructures and fractographs were examined by SEM. Uniaxial tensile testing was performed to determine the mechanical properties. The results show that the microlaminate deposited on the relatively coarse substrate (MDCS) contains wavy layer interfaces and larger flaws, while the microlaminate deposited on the relatively smooth substrate (MDSS) has relatively flat layer interfaces and no larger flaws. The tensile specimens of the two microlaminates display obvious difference in tensile strengths and fracture modes. The ratio of strength of MDCS to that of MDSS is 0.5 at room temperature, 0.67 at 700 ℃ and 1.33 at 1 000 ℃, increasing with increasing temperature. The factors which caused the variation of the strength ratio were discussed. It is found that the larger flaws in MDCS result in the relatively low strength ratio at room temperature and 700 ℃, and the wavy layer interface in MDCS is responsible for the relatively great strength ratio at 1 000 ℃.
  • Nanomaterials, Thin Films and Coatings
    LOUXiao-bo(楼晓波),SHENHong-lie(沈鸿烈),ZHANGHui(张 惠),LIBin-bin(李斌斌)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 814-817.
  • Nanomaterials, Thin Films and Coatings
    MAZeng-sheng(马增胜),LONGShi-guo(龙士国),ZHANGXiao-bing(张小兵),PANYong(潘 勇),ZHOUYi-chun(周益春)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 818-822.
    Nickel coating deposits with better ductility on a lower carbon steel sheet were produced by electrodeposition method and the electrodeposited nickel coating was deformed with the strain of 10%. Then the surface morphology, the deformation texture and the mechanical properties were analyzed by scanning electron microscopy (SEM), X-ray diffractometry (XRD) and nano-indentation measurement, respectively. The principle of nano-indentation to measure the hardness and elastic modulus of nickel coating was introduced. The relation curves of the load and displacement were obtained, including the original electrodeposited samples and the samples under tension. The results show that: 1) there are only two main texture components Ni (111) and Ni (200) in the nickel coating, and no new texture component is found due to the elongation; 2) after tensile deformation in the coating, the surface roughness increases and the microcrack is found; 3) The hardness and the elastic modulus decrease after tensile deformation; and 4) for the original electrodeposited sample, the indentation depths change with the load, the hardness and the elastic modulus decrease with the increase of the depth. In addition, the investigation of creep shows that the value of creep increases when the tensile strain ε>10%.
  • Nanomaterials, Thin Films and Coatings
    LONGShi-guo(龙士国),MAZeng-sheng(马增胜),ZHANGXiao-bing(张小兵),PANYong(潘 勇),ZHOUYi-chun(周益春)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 823-826.
    The deformation texture and surface microstructure of nickel coating induced by deep cup-drawing were studied by X-ray diffractometry and SEM. The steel sheet with nickel coating was firstly punched to designed degree of cup shapes. Then the texture of the coating was determined by XRD and the surface microstructure was observed by SEM. The results indicate that, the nickel coating material includes three kinds of textures, i.e. Ni (111), Ni (200) and Ni (220). After cup-drawing deformation, there doesn’t appear new texture component for nickel coatings but the change of the intensity of the deformation textures. In the cup-deformation process, the two kinds of main textures Ni (111) and Ni (200) increase in the first and second cup-drawing procedures and then reduce quickly in the third and fourth drawing procedure. However, for the Ni (220) texture, it always increases in whole cup-drawing procedures. With the increase in the drawing, there are some cracks to be found, but not delamination. This shows that nickel coating and the substrate have a good combinable performance.
  • Nanomaterials, Thin Films and Coatings
    LIMing-sheng(李明升),ZHANGShu-juan(张淑娟),LOUJin(娄 瑾),LIUTing-zhi(刘庭芝),ZHOUZe-hua(周泽华),YANGGan-lan(杨干兰),HUChang-yuan(胡长员),LIWen-kui(李文魁)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 827-830.
    TiO2 and N-doped TiO2 films were deposited on the glass substrates by arc ion plating method. The results show that the deposition rate does not change with the increasing deposition time. The increase of mass flow rate of N2 gives rise to the increase of deposition rate. All as-deposited TiO2 and N-doped TiO2 films are amorphous. The anatase TiO2 phase with preferred orientation (101) is acquired by post-annealing at 400 ℃ for 2 h. The incorporation of N into the TiO2 films and the heat treatment extensively shift the band edge to the visible light region.
  • Nanomaterials, Thin Films and Coatings
    LIMing-sheng(李明升),FENGChang-jie(冯长杰),YANGGan-lan(杨干兰),HEXiang-ming(何向明),LIWen-kui(李文魁),XIANGJun-huai(向军
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 831-834.
    The composite metastable (Ti0.5Al0.5)N, (Ti0.45Al0.45Cr0.1)N and (Ti0.35Al0.35Cr0.3)N coatings were respectively deposited on a wrought martensite steel 1Cr11Ni2W2MoV for aero-engine compressor blades by arc ion plating technique with pulse substrate bias. All the coatings have B1NaCl phase with a (200) preferred orientation and dense structures. The results show that the introduction of Cr into (Ti,Al)N gives rise to a minute shrinkage of crystal lattice. The incorporation of chromium into the coatings dramastically improves the oxidation-resistance of the coatings. For (Ti0.5Al0.5)N, a layered oxide scale forms after 100 h oxidation and the outer layer is the blend oxide of TiO2 and Al2O3, and the middle layer is rich in Al and the inner layer is rich in Ti. For (Ti0.45Al0.45Cr0.1)N, the oxide scale possesses a double-layered structure and the outer layer is rich in Ti. For (Ti0.35Al0.35Cr0.3)N, a Cr-rich compound oxide scale of Ti, Al and Cr forms, and a out-diffusion of Fe from steel to the nitride coating and oxide film during the oxidation takes place.
  • Nanomaterials, Thin Films and Coatings
    LIXue-song(李雪松),ZHANGWen-xue(张文雪),JIANGZhong-hao(江中浩)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 835-840.
    Taking a bath with basic nickel carbonate as the source of nickel, sodium hypophosphite as the reducing agent and citric acid as the complexing agent, the Ni-P coatings on AZ91D magnesium alloy were prepared. The influence of pH value of the bath on the content of phosphorus, microhardness and corrosion resistance of the deposits was examined. The XRD analysis results show that the Ni-P coatings plated under all conditions have a mixed microstructure of amorphous and nanocrystalline and undergo a phase transformation to crystalline nickel and nickel phosphide upon heat-treatment. The microhardness of the Ni-P coatings increases with the increase of pH value of the bath and has a maximum at pH=6. The potentiodynamic polarization test in 3.5%(mass fraction) NaCl solution reveals that the Ni-P coatings exhibit a very good corrosion resistance to protecting AZ91D magnesium alloy.
  • Nanomaterials, Thin Films and Coatings
    DUOShu-wang(多树旺),ZHUMing(朱 明),LIUTing-zhi(刘庭芝), LIZhong-jun(李忠峻),WANGPeng(王 鹏),LIMei-s
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 841-846.
    CrN and Cr-Al-N coatings were deposited by reactive magnetron sputtering on the glass substrate, and their corrosion behavior was studied. The electrochemical tests using both DC (polarization curves) and AC techniques (EIS) were carried out on Potentiostat/Galvanstat (EG&G) in 3.5% (mass fraction) NaCl solution. After immersed into NaCl solution for 1 h, the mass of the CrN coating keeps constant with the time continuing. This can be explained by the passivation of the coating. The comparison between the corrosion potential (φcorr) of the Cr-Al-N coatings with different aluminum contents reveals that the corrosion potentials of the aluminum contain coatings are nobler than that of the CrN coatings. This means that the addition of aluminum shifts the corrosion potential to more positive potential value. Among these coatings, CrN in NaCl solution exhibits the worst corrosion resistance, while the corrosion resistance of Cr0.63Al0.37N in NaCl solution is the best. The polarization data and EIS data suggest that addition of aluminum can improve the corrosion resistance of CrN coating.
  • Nanomaterials, Thin Films and Coatings
    DUXin-kang(杜心康),WANGJian-jiang(王建江),WANGTian-min(王天民),LIUHong-wei(刘宏伟),LIWei-bo(李伟波)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 847-850.
    Utilizing self-propagating high-temperature synthesis (SHS) reactive spraying technology, the feeding self-combustion agglomerated particles composed of Ti, B4C and C powders, TiC-TiB2 multi-phase ceramic coatings were prepared on the steel substrates. Orthogonal experiment was carried out to optimize the spraying parameters. The phase component and microstructure of the coating fabricated at the optimized parameters were studied by XRD and SEM. The reactive mechanism in flying agglomerated particles was discussed. The optimized conditions, spraying distance of 220 mm, powders delivering gas pressure of 0.3 MPa and preheating temperature of 240 ˚C to sprayed particles, were obtained from orthogonal experiment. For the coating, porosity of 2.5% and HV 1 595 are achieved under the optimized parameters. The coatings are mainly composed of TiC0.3N0.7, TiB2 and a little TiO2. The SEM analysis shows the morphology of TiC0.3N0.7 matrix in which the fine granular TiB2 crystals evenly disperse. It is concluded that, as solo reactive units, the agglomerated particles would finally form into the coatings after going through four successive stages in the flame, which are, respectively, pregnant reaction, flight combustion, collision and structure transformation and solidification. The solid diffusion and dissolution-precipitation are the two mechanisms to control the synthesis reaction.
  • Nanomaterials, Thin Films and Coatings
    ZHOU Hai(周  海), CHEN Fei(陈  飞), LÜ Xiao-jing(吕晓静)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 851-853.
    The NiCrAlY+ZrO2 thermal barrier coating was prepared on the surface of TiAl alloy by plasma spraying technique. The microstructure and phase structure were analyzed using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). The high temperature oxidation resistance of the plasma sprayed samples at 850℃ was investigated. The results show that the bonding between thermal barrier coating and substrate is very good. Surface hardness of TiAl alloy is improved too. The microhardness of the coating surface is about HV 900 after the oxidation test at 850 ℃. The oxidation resistance of the samples is improved remarkably.
  • Nanomaterials, Thin Films and Coatings
    NIEXiao-liang(聂小亮),LANZhong-wen(兰中文),YUZhong(余 忠),SUNKe(孙 科),LILe-zhong(李乐中)
    Transactions of Nonferrous Metals Society of China. 2007, 17(Special 1): 854-857.
    Ti4+ substitution for Fe3+ in Ni0.5Zn0.5Fe2O4 (NZF) ferrite thin films were realized by sol-gel method and annealing at 600℃ for 30 min in the air. Crystal structure and lattice constant determination was performed by X-ray diffractometer (XRD). Surface microstructure was observed by scanning electron microscope (SEM) and atomic force microscope (AFM), and the magnetic properties were measured by vibrating sample magnetometer (VSM). XRD analyses of the samples show that Ni0.5+xZn0.5TixFe2−2xO4 (NZTF) films with x varying from 0 to 0.15 in steps of 0.05 are composed of single phase with spinel structure. And the lattice parameter, particle size and the diffraction intensity of the films increase with substitution of Ti as the result of the larger radius ions entering the lattice. SEM and AFM show homogeneous grain size of each sample, but there is a few differences in grain size with different Ti-substitution contents. As the nonmagnetic Ti4+ substitutes Fe3+, both the saturation magnetization and coercivity decrease.