The film-forming behavior on the interface between air and hydrosol of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles

The film forming behavior on the interface between air and hydrosol of Fe₂O₃ nanoparticles was investigated by the surface pressure-time isotherms, the surface pressure-trough area isotherms, Brewster angle microscopy and transmission electron microscopy. It is found that the freshly prepared hydrosol of Fe₂O₃ nanoparticles is not stable. The surface pressure increases with the aging time and finally approaches a constant, and the smaller the concentration is, the smaller the surface pressure is stabilized at and the shorter the time the hydrosol reaching stable needs. The surface pressure also increases with compression until collapsed, and the longer the hydrosol is aged, the higher the collapsing pressure is. A uniform and compact film composed of nanoparticles with an average diameter of about 2–3 nm on the air-hydrosol interface is observed by Brewster angle microscope and transmission electron microscope. Funded by the National Natural Science Foundation of China (50672089), the Encouraging Foundation for the Scientific Research of the Excellent Young and Middleaged Scientists in Shandong Province(2006BS04034)     

Micro-inhomogeneous structure of liquid Al-Fe alloys

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Study on BaTiO<Subscript>3</Subscript> films prepared by AC power microarc oxidation

BaTiO₃ films were prepared by microarc oxidation (MAO) with an in-house built alternating current (AC) power supply in Ba(OH)₂ solution in this study. The surface morphology, combinability with the substrate and phase composition of the films were investigated by XRD, SEM and TEM. The BaTiO₃ films were annealed at a temperature range of 900 to 1200°C and phase compositions were tested thereafter. The results showed that the BaTiO₃ films were mainly composed of the primitive hexagonal phase with relatively small amount of tetragonal and amorphous phases. Moreover, the amount of amorphous phase decreased with the time of annealing. The transformation of BaTiO₃ from hexagonal structure to tetragonal stucture became obvious until the annealing temperature reached 1200°C. The film consisted mainly of BaTiO₃ tetragonal structure with ferroelectric property. The influence of annealing on surface morphology and mechanism of phase transformation of the films were also discussed. Supported by Guangdong Natural Science Foundation (Grant No. 0500649)     

Electronic structure and FIM imaging mechanism of Fe-Al intermetallic compounds

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Synthesis of γ-Al2O3 nanoparticles by chemical precipitation method

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

The Influence of Annealing Temperature on the Structure and Properties of TiO2 Films Prepared by Sputtering

The TiO₂ films were prepared on slides by dc reactive magnetron sputtering, then the samples were annealed at 300°C, 350°C, 400°C, 450°C, 500°C and 550°C, respectively. X-ray diffraction (XRD) was used to obtain the TiO₂ film crystalline structure; X-ray photoelectron spectroscopy (XPS) was used to study the film surface stoichiometries; surface morphologies were studied by scanning electron microscopy (SEM); the contact angle was tested to indicate the TiO₂ film wettability; and the photocatalytic activity testing was conducted to evaluate the photocatalysis properties. The photocatalytic activity and contact angle testing results were correlated with the crystallinity, surface morphologies and surface ·OH concentration of TiO₂ films. The samples with a higher polycrystalline anatase structure, rough surface and high ·OH concentration displayed a better photoinduced hydrophilicity and a stronger photocatalysis. Funded by the National “863” Project Foundation (No. 2003LG0034)     

Study on the thermal stability and electrical properties of the high-k dielectrics (ZrO2)x(SiO2)1?x

(ZrO₂) _x (SiO₂)_1−x (Zr-Si-O) films with different compositions were deposited on p-Si(100) substrates by using pulsed laser deposition technique. X-ray photoelectron spectra (XPS) showed that these films remained amorphous after annealing at 800°C with RTA process in N₂ for 60 s. The XPS spectra indicated that Zr-Si-O films with x=0.5 suffered no obvious phase separation after annealing at 800°C, and no interface layer was formed between Zr-Si-O film and Si substrate. While Zr-Si-O films with x >0.5 suffered phase separation to precipitate ZrO₂ after annealing under the same condition, and SiO₂ was formed at the interface. To get a good interface between Zr-Si-O films and Si substrate, Zr-Si-O films with bi-layer structure (ZrO₂)_0.7(SiO₂)_0.3/(ZrO₂)_0.5(SiO₂)_0.5/Si was deposited. The electrical properties showed that the bi-layer Zr-Si-O film is of the lowest equivalent oxide thickness and good interface with Si substrate. Supported by the National Nature Science Foundation of China (Grant No. 60636010) and the National Basic Research Program of China (“973” Program) (Grant No. 2004CB619004)     

Properties of Al-doped Copper Nitride Films Prepared by Reactive Magnetron Sputtering

Cu3N and Al Cu3N films were prepared with reactive magnetron sputtering method. The two films were deposited on glass substrates at 0.8 Pa N2 partial pressure and 100 ℃ substrate temperature by using a pure Cu and AI target, respectively. X-ray diffraction （XRD） measurements show that the un-doped film was composed of Cu3N crystallites with anti-ReO3 structure and adopted [111] preferred orientation. XRD shows that the growth of Al-doped copper nitride films （AlxCu3N） was affected strongly by doping AI, the intensity of [111] peak decreases with increasing the concentration of Al and the high concentration of Al could prevent the Cu3N from crystallization. AFM shows that the surface of AlCu3N film is smoother than that of Cu3N film. Compared with the Cu3N films, the resistivities of the Al-doped copper nitride films （AlxCu3N） have been reduced, and the microhardness has been enhanced.     

Preparation of TiO<Subscript>2</Subscript> thin film by the LPD method on functionalized organic self-assembled monolayers

In this paper, uniform titania (TiO₂) films have been formed at 50° on silanol SAMs by the liquid-phase deposition (LPD) method at a temperature below 100°C. OTS (Octadecyltrichloro-Silane) self-assembled monolayers (SAMs) on glass wafers were used as substrates for the deposition of titanium dioxide thin films. This functionalized organic surface has shown to be effective for promoting the growth of films from titanic aqueous solutions by the LPD method at a low temperature below 100°C. The crystal phase composition, microstructure and topography of the as-prepared films were characterized by various techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The results indicate that the as-prepared thin films are purely crystallized anatase TiO₂ constituted by nanorods after being annealed at 500°. The pH values, concentration of reactants, and deposition temperatures play important roles in the growth of TiO₂ thin films. Support by the National Natural Science Foundation of China (Grant No. 50672055) and National Key Technology R&D Program (Grant No. 2006BAF02A28)     

Erosion-Corrosion Behaviors of High Velocity Arc Sprayed Fe-Al/Cr3 C2 Coating

1 IntroductionArc Spraying (AS) is a technique that utilizes anelectric arc as the heat source to melt wires into droplets ,which are subsequentlysprayed ontosubstrates bytheflowof compressed air . High Velocity Arc Spraying (HVAS)technology was developed on the basis of AS. Aspecialtube designed according to the principle of aerodynamicswas mounted at the exit of compressed air .Thenthe hightemperature fuel air or compressed air was accelerated bythe tube .Hence ,a higher velocityand be…     

Preparation and properties of SrBi2.2 Ta2O9 thin film

SrBi_2.2 Ta₂O₉ (SBT) thin film with thickness of 2 μm was successfully prepared by sol-gel method, using strontium acetate semihydrate [Sr(CH₃ COO)₂ · 1/2H₂O] and bismth subnitrate [BiO(NO₃)], and tantalum ethoxide [Ta(OCH₂CH₃)₅] as source materials, glacial acetic and ethylene glycol as solvents. The X-ray diffraction (XRD) and transmission electron microscope(TEM) results indicate that SBT layer-perovskite phase obtained has to be single phase, SBT thin film is formed after being annealed at 800 °C for for 1 min. The typical hysteresis loop of SBT thin film on Pt/Ti/SiO₂/Si is obtained, and the measured polarization value of the SBT thin film is 4. 2 μ/C/cm². Foundation item: Project (HIT. 2001. 67) supported by the Scientific Research Foundation of Harbin Institute of Technology; project (50172012) supported by the National Natural Science Foundation of China     

Fabrication and magnetic properties of Sm3(Fe,Ti)29Nx/α-Fe dual-phase nanocomposite permanent magnetic material

Sm3(Fe,Ti)29Nx/α-Fe dual-phase nanometer magnetic material was fabricated through rapid solidification, crystallization and nitridation of Sm-Fe (Ti) alloy. The effect of combination of rapid solidification and Ti alloy addition on the phase formation and microstructure of the Sm-Fe alloy is investigated in this paper. The microstructure of amorphous phase and dual-phase nano-grain crystals before and after crystallization annealing were observed using a high-resolution transmission electron microscope (HREM). The dual-phase nano-grains after annealing were compacted together with a clear interface with the direct exchange-coupling mechanism. Different annealing processes were used to examine the melt-spun alloy. Comparison of the images of SEM showed that annealing at 750℃ for 10 min was most suitable to get homogeneous and nano-grains. No obvious kink was detected in the second quadrant of the hysteresis loop like a single hard magnet, and strong exchange coupling was found between hard magnets and soft magnets.     

Sensing characterization of Sn/In/Ti nanocomplex oxides for CO,CH<Subscript>4</Subscript> and NO<Subscript>2</Subscript>

The nanocomplex oxides of Sn-In and Sn-In-Ti were prepared by controlled co-precipitation method as sensing materials of semiconductor gas sensors for detection of CO, CH4 and NO2. Through manipulating the Sn/In cation ratio, metal salt total concentration, precipitation pH value and aging time, the nanocrystalline powders were successfully derived with chemical homogeneity and superior thermal stability, compared with the single component oxides. The particle size and morphology, surface area, and thermal and phase stabilities were characterized using TEM, TG-DTA, BET and XRD. The sensing tests showed that the Sn-In composites exhibit high sensitivity and selectivity for CO and NO2. The introduction of TiO2 enhanced CH4 sensitivity and selectivity, particularly, additives of Pd and Al2O3 as a dopant and surface modification greatly enhanced the sensing properties. The sensitivity depended on the composition of composites, calcination temperature and operating temperature. The optimal values were (25%In2O3- 75%SnO2)-20%TiO2 for ternary composite, 600 and 300℃, respectively. Temperature-programmed desorption (TPD) studies were employed to explain the gas adsorption behavior displayed by the surface of nanocomposites and X-ray photoelectron spectroscopic (XPS) analysis was used to confirm the electronic interactions existing between oxide components. The sensing mechanism of the nanocomposites was attributed to chemical and electronic synergistic effects.     

Corrosion behavior of amorphous/nanocrystalline Al-Cr-Fe film deposited by double glow plasmas technique

In order to improve the corrosion resistance of AZ31 magnesium alloy, the amorphous/nanocrystal Al-Cr-Fe film has been successfully prepared on AZ31 magnesium alloy by double glow plasma technology. The amorphous/nanocrystalline consists of two different regions, i.e., an amorphous layer on outmost surface and an underlying lamellar nanocrystalline layer with a grain size of less than 10 nm. The corrosion behavior of amorphous/nanocrystalline Al-Cr-Fe film in 3.5% NaCl solution is investigated using an electrochemical polarization measurement. Compared with the AZ31 magnesium alloy, the amorphous/nanocrystalline Al-Cr-Fe film exhibits more positive corrosion potentials and lower corrosion current densities than that of AZ31 magnesium alloy. XPS measurement reveals that the passive film formed on the Al-Cr-Fe film after the anodic polarization tests is strongly enriched in Cr₂O₃, Fe₂O₃ and Al₂O₃ at outer surface of the film and in the inner layer consists of Cr₂O₃, FeO and Al₂O₃. Supported by the National Natural Science Foundation of China (Grant Nos. 50571045 and 50704022) and the Natural Science Foundation of Jiangsu Province, China (Grant No. BK2007591)     

AFM research on the mechanism of Fe-based alloy stress annealed inducing magnetic anisotropy

The cross-section of the Fe-based alloy (Fe_73.5Cu₁Nb₃Si_13.5B₉) ribbon annealed at 540°C under various tensile stress was investigated with atomic force microscope (AFM). The stress effect mechanism in Fe-based alloy ribbon tensile stress annealed inducing transverse magnetic anisotropy field was studied using the X-ray diffraction spectra and longitudinal drive giant magneto-impedance effect curves, and the model of direction dominant in encapsulated grain agglomeration was established. The relationship between the direction dominant in encapsulated grain agglomeration and magnetic anisotropy field was disclosed. Supported by the Natural Science Foundation of Zhejiang Province (Grant No. Y405021), Key Project of Science and Technology of Zhejiang Province (Grant No. 2006C21109) and Key Project of Science and Technology Research of China Ministry of Education (Grant No. 204059)     

Controlled synthesis and magnetic properties of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> walnut spherical particles and octahedral microcrystals

Magnetite Fe₃O₄ walnut spherical particles and octahedral microcrystals were successfully synthesized from K₄ [Fe (CN)₆], K₃ [Fe (CN)₆] and NaOH reagents via a simple hydrothermal process. And the uniform morphology of octahedral microcrystals was obtained in the presence of ethylene glycol. The morphology and structure of products were characterized by powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that the Fe₃O₄ walnut spherical particles and octahedral microcrystals were single crystals with the face-center cubic structure and with size distributions from 2.2 to 8.6 μm and 1.6 to 12.5 μm, respectively. Their magnetic properties were detected by a vibrating sample magnetometer at room temperature. The walnut spherical particles exhibited a ferromagnetic behavior with the coercive force (Hc), saturation magnetization (Ms) and remanent magnetization (Mr) being 150.57 Oe, 97.634 and 12.05 emu/g, respectively. For the octahedral microcrystals they were 75.28 Oe, 101.90 and 6.69 emu/g, respectively. Different sizes of walnut spherical particles were controlled synthesized through adjusting the NaOH concentration. It was found that ethylene glycol molecules have a significant effect on the formation of Fe₃O₄ octahedra. A possible mechanism was also proposed to account for the growth of these Fe₃O₄ products. Supported by Fund of weinan Teachers University (Grant No. 08YKZ008), the National Natural Science Foundation of China (Grant No. 20573072) and Doctoral Fund of Ministry of Education of China (Grant No. 20060718010)     

Formation of bulk ferromagnetic nanostructured Fe<Subscript>40</Subscript>Ni<Subscript>40</Subscript>P<Subscript>14</Subscript>B<Subscript>6</Subscript> alloys by metastable liquid spinodal decomposition

Nanostructured Fe₄₀Ni₄₀P₁₄B₆ alloy ingots of 3–5 mm in diameter could be synthesized by a metastable liquid state spinodal decomposition method. For undercooling ΔT > 260 K, the microstructure of the undercooled specimen had exhibited liquid state spinodal decomposition in the undercooled liquid state. The microstructure could be described as two intertwining networks with small grains dispersed in them. For undercooling ΔT > 290 K, the overall microstructure of the specimen changed into a granular morphology. The average grain sizes of the small and large grains are ≅ 30 nm and ≅ 80 nm, respectively. These prepared samples are soft magnets with saturation magnetization B _s ≅ 0.744 T. Supported by the Hong Kong Research Grants Council the National Natural Science Foundation of China (Grant No. 50861007) and Xinjiang University Doctoral Research Start-up Grant (Grant No. BS050102)     

Properties of plasma sprayed NiCrAlY+(ZrO2+Y2O3) coating on refractory steel surface

NiCrAlY+(ZrO₂+Y₂O₃) thermal barrier coating was prepared on the surface of refractory steel 1Cr18Ni9Ti with plasma spraying technique. The phases and microstructure of the thermal barrier coating were determined by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results show that the bonding between thermal barrier coating and substrate is sound. The surface hardness of 1Cr18Ni9Ti reaches up to 1 000 HV, but that of substrate is only 300 HV. The patterns sprayed with CoNiCrAlY+(ZrO₂+Y₂O₃) ceramic coating have a good heat insulation effect at 800 °C for heat insulation temperature difference reaches 54 °C, which increases the operating temperature and service life of refractory steel. Foundation item: Project (5040202140) supported by Scientific Research Common Program of Beijing Municipal Commission of Education     

AFM research on Fe-based nanocrystal crystallization mechanism

The cross-section pattern of Fe-based alloy ribbon (Fe_73.5Cu₁Nb₃Si_13.5B₉) annealed at different temperatures was investigated by AFM (atomic force microscope), and the effect mechanism of Nb and Cu in Fe-based alloy ribbon annealing was analyzed with XRD diffraction crystal analysis technique and other research results. New concepts of encapsulated grain, Nb vacancy cluster, Nb-B atom cluster and so on were proposed and used to describe the formation mechanism of α-Fe (Si) nanocrystal. Finally, a three-phase (separation phase, encapsulated phase and nanocrystalline phase) interconnected structure model in Fe-based nanocrystalline alloy was established. Supported by the Natural Science Foundation of Zhejiang Province (Grant No. Y405021), Zhejiang Provincial Science and Technology Key Project (Grant No. 2006C21109) and Key Project of Science and Technology Research of China Ministry of Education (Grant No. 204059)     

Ferroelectric properties of Bi3.4Ho0.6Ti3O12 thin films prepared by sol-gel method

We have prepared the Ho-substituted bismuth titanate (Bi_3.4Ho_0.6Ti₃O₁₂, BHT) thin films on Pt/Ti/SiO₂/Si substrates using sol-gel method. The crystal structure and morphology of the films were characterized using X-ray diffraction and atomic force microscopy. The BHT film shows a single phase of Bi-layered Aurivillius structure and dense microstructure. The 2Pr and 2Ec of the 600-nm-thick BHT film were 38.4 μC/cm² and 376.1 kV/cm, respectively at applied electric field 500 kV/cm. The dielectric constant and dielectric loss are about 310 and 0.015 at a frequency of 1 MHz, respectively. The Pr value decreased to 93% of its pre-fatigue values after 4.46×10⁹ switching cycles at 1 MHz frenquency, and the BHT film shows good insulating behavior according to the test of leakage current. Supported by the Hubei Province Natural Science Foundation (Grant No. 2007ABA309)