In-situ TEM Study on Mierostruetural Evolution of Nanostruetured TiO2

The effect of electron beam on the microstructures and phase transformation of nanostructured TiO2 heat treated at various temperatures for different time was studied by in-situ TEM and SAED. Anatase ex-situ heated at 250℃ and 360℃ transformed to rutile while irradiated by the electron beam. With the increasing sizes and distribution of the powders on the amorphous carbon, the process of phase transformation by the electron beam was encumbered. These evolutions may be due to the changes of vacuum atmosphere and the properties of powders.     

Transition of Y<Subscript>2</Subscript>BaCuO<Subscript>5</Subscript> phase in powder melting processed YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−x</Subscript> superconductors

The morphology and the formation of Y2BaCuO5 phase in powder melting processed YBa2Cu3O7-x superconductors were investigated. The experimental results show the heat treatment can not change the shape of Y2BaCuO5 particles in powder melting processed samples. The formation of round Y2BaCuO5 phase is due to relative content of each constitution of precursor powders in powder melting process. For powder melting process, the excessive liquid phase is eliminated, which restrains the preferred growth of Y2BaCuO5 ...     

The Preparation of CoWO4／WO3 Nanocomposite Powder

Ammoniwn metatungstate and cobalt nitrate were mixed at the molecular level in distilled water and then spruy-decomposed to CoWO4/WO3 nanoconposite powder. The particle morphology, crystalline size,forming course, chemical composition ant phase structure of the powder were studied by SEM , TEM , DTA- TG , IR and XRD , respectively. Reshlts show that the powder is homogeneous, spherical and nano-aggregated.     

Effects of NaNbO3-Co2O3 Co-additive on the Properties of PZN-PZT Ceramics

NaNbO3-Co2O3 co-added PZN-PZT （PZCNNT） ceramics were prepared using conventional solid state reaction. The piezoelectric and dielectric properties were measured. The experimental results show that the addition of 0.3mo1% Co2O3 leads to low dielectric loss （tgδ） in PZCNNT ceramics and the proper addition of NaNbO3 not only improves piezoelectric properties but also decreases intensively dielectric loss and mechanical loss. The optimal ceramic having d33=310 pC/N, kp=0.59, εr=985, tgδ=0.0034, Qm=1380 was obtained.     

Effects of N<Subscript>2</Subscript> pressure on the structural and electrical properties of tin films deposited by laser molecular beam epitaxy

Titanium nitride (TiN) films were deposited on Si(100) substrates by laser molecular beam epitaxy(LMBE), and their properties of structure and resistivity with varying N₂ pressure were investigated. The results showed that atomically flat TiN films with layer-by-layer growth mode were successfully grown on Si(100) substrates, and (200) was the preferred orientation. With the increasing of N₂ pressure, the N/Ti ratio gradually increased and the diffraction peak progressively shifted towards lower diffraction angle. At pressure of 0.1 Pa, stoichiometric TiN film was formed which exhibited the characteristic diffraction angle of (200) plane. All films showed high reflectance to infrared spectrum and the films with overstoichiometry and understoichiometry had a higher resistivity owing to the surface particles and lattice distortion, while the stoichiometric TiN film depicted the minimum resistivity, around 19 μΩ·cm.     

Optical waveguide and nonlinear properties of Bi<Subscript>3</Subscript>NdTi<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films

Neodymium-substituted bismuth titanate (Bi₃NdTi₃O₁₂, BNT) thin films were prepared on quartz substrates by a metal-organic solution deposition process. The crystalline structure was evaluated by X-ray diffraction. Waveguide property was investigated by using prism coupling technique and optical transmittance measurement. The optical nonlinearities of the film were measured by the top-hat Z-scan techniques and a large positive nonlinear refractive index, nonlinear refractive coefficient and two-photon absorption coefficient were determined to be 3.84 × 10⁻⁷ esu, 0.7523 cm²/GW and 4.81 × 10⁴ cm/GW, respectively. These results reveal that the BNT film may be a kind of new multifunctional materials.     

Optical and magnetic properties of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript> nano-composite films

Fe₂O₃/SiO₂ nano-composite films were prepared by sol-gel technique combining heat treatment in the range of 100–900 °C. The particle size was observed by FE-SEM. Optical properties of the films were investigated by UV-visible spectra. Structural and magnetic characteristics were investigated through FT-IR and VSM. The transparency of the Fe₂O₃/SiO₂ nano-composite films decreased with the content of the Fe₂O₃. Water and organic solvent in the films were evaporated with heat treatment, so the transparency of the films was enhanced under high temperature. It is also found that the saturation magnetization (M _s) of the films increases with the temperature. As the content of the Fe₂O₃ increases, when the content of the Fe₂O₃ is around 30wt%, the M _s of the films has a maximum value.     

Preparation and characterization of nanocomposite MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript>

Nanocomposites MgFe₂O₄/SiO₂ were successfully synthesized by the sol-gel method in the presence of N, N-dimethylformamide (DMF). The formation of pure MgFe₂O₄ was confirmed by powder X-ray diffraction (XRD) and electron diffraction. The structural evolution of MgFe₂O₄ nanocrystals was followed by powder X-ray diffraction and IR absorption spectroscopy. The formation of spinel structure of MgFe₂O₄ started at 800 °C, and completed at 900 °C. The transmission electron microscopy (TEM) measurements suggest that the particle sizes increase with the increasing annealing temperature, and the mean particle sizes of the spherical samples annealed at 800 °C, 900 °C and 1 050 °C are ca. 3 nm, 8 nm and 11 nm, respectively. Magnetization measurements at room temperature and 78 K indicate superparamagnetic nature of these MgFe₂O₄ nanocrystals. Funded by the National Natural Science Foundation of China(No. 30771676), the Natural Science Foundation of Jiangsu Province (No. BK20081842), and the Foundation of Nanjing Bureau of Personal for the Returned Overseas Chinese Excellent Scholars     

Preparation and ferroelectric properties of Bi<Subscript>3.4</Subscript>Ce<Subscript>0.6</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films grown by sol-gel method

We have investigated the preparation and properties of Bi_3.4Ce_0.6Ti₃O₁₂ thin films. The Bi_3.4Ce_0.6Ti₃O₁₂ thin films were fabricated on the Pt/Ti/SiO₂/Si substrates using sol-gel method. The structure and morphology of the films were characterized using X-ray diffraction and atomic force microscopy. The thin films showed a perovskite phase and dense microstructure. The dielectric constant and the dissipation factor of the Bi_3.4Ce_0.6Ti₃O₁₂ thin films were about 172 and 0.031 at 1 kHz, respectively. The 2P _r and 2E _c of the Bi_3.4Ce_0.6Ti₃O₁₂ thin films were 67.1 μC/cm² and 299.7 kV/cm, respectively, under an applied field of 600 kV/cm. The Bi_3.4Ce_0.6Ti₃O₁₂ film did not show fatigue up to 4.46×10⁹ switching cycles at a frequency of 1 MHz, and showed good insulating behavior according to the test of leakage current. Supported by the Natural Science Foundation of Hubei Province (Grants No. 2004ABA082)     

Synthesis and characterization of (PEO)<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>−(V<Subscript>0.85</Subscript>Mo<Subscript>0.15</Subscript>)<Subscript>2</Subscript>O<Subscript>5</Subscript> nanocomposite films

(PEO) _x −(V_0.85Mo_0.15)₂O₅(x=0,0.5,1.0) nanocomposite films were prepared by a modified sol-gel method. The structure of the films was analyzed by XRD, and the DC electrical conductivity. Cyclic voltammogram and optical spectral transmittance were investigated. The results show that the (V_0.85Mo_0.15)₂O₅ xerogel has a layered structure and its interlayer space increased from 1.3181 nm at x=0 to 1.7897 nm at x=1.0. The introduction of MoO₃ improved the DC electrical conductivities of the films due to the generation of V₄₊ to maintain the electrical neutrality of the oxides. PEO intercalated in the interlayer of (V_0.85Mo_0.15)₂O₅ oxides has interaction with the oxides, enhancing the amount of Li⁺ ions inserted into the interlayer of the oxides. Moreover, the intercalation of PEO into the interlayer of (V_0.85Mo_0.15)₂O₅ oxides improved the cathodic electrochromic property in near ultraviolet region and anodic electrochromic property in visible range. JIANG Cong-sheng: Born in 1963 Supported by the Science Foundation of Hubei Province (Grant No. 2001ABB083)     

UV-vis and photoluminescent spectra of TiO<Subscript>2</Subscript> films

TiO₂ fims have been deposited on glass substrates using DC reactive magnetron sputtering at different oxygen partial pressures from 0. 10 Pa.to 0.65 Pa. The transmittance (UV-vis) and photoluminescence (PL) spectra of the films were recorded. The results of the UV-vis spectra show that the deposition rate of the films decreased at oxygen partial pressure P(O₂)≥0.15 Pa, the band gap increased from 3.48 eV to 3.68eV for direct transition and from 3.27 eV to 3.34 eV for indirect transition with increasing the oxygen partial pressure. The PL spectra show convincingly that the transition for films was indirect, and there were some oxygen defect energy levels at the band gap of the films. With increasing the O₂ partial pressure, the defect energy levels decreased. For the films sputtered at 0.35 and 0.65 Pa there were two defect energy levels at 2.63 eV and 2.41 eV, corresponding to 0.72 eV and 0.94 eV below the conduction band for a band gap of 3.35 eV, respectively. For the films sputtered at 0.10 Pa and 0.15 Pa, there was an energy band formed between 3.12 eV and 2.06 eV, corresponding to 0.23 eV and 1.29 eV below the conduction band. ZHAO Qing-nan : Born in 1963 Funded by Natural Science Foundation of Hubei Province, China.     

Ferroelectric properties of Bi<Subscript>4</Subscript>Zr<Subscript>0.5</Subscript>Ti<Subscript>2.5</Subscript>O<Subscript>12</Subscript> thin films prepared on LaNiO<Subscript>3</Subscript> bottom electrode by sol-gel method

The Bi4Zr0.5Ti2.5O12 (BZT) thin films were fabricated on the LaNiO3 bottom electrode using sol-gel method. The structure and morphology of the films were characterized using X-ray diffraction, AFM and SEM. The results show that the films have a perovskite phase and dense microstructure. The 2Pr and 2Vc of the Pt/BZT/LaNiO3 capacitor are 28.2 μC/cm2 and 14.7 V respectively at an applied voltage of 25 V. After the switching of 1×1010 cycles, the Pr value decreases to 87% of its pre-fatigue values. The dielectric constant (ε) and the dissipation factor (tanδ) of the BZT thin films are about 204 and 0.029 at 1 kHz, respectively. The films show good insulating behavior according to the test of leakage current. The clockwise C-V hysteresis curve observed shows that the Pt/BZT/LaNiO3 structure has a memory effect because of the BZT film's ferroelectric polarization.     

Orientation of Bi<Subscript>3.2</Subscript>La<Subscript>0.8</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ferroelectric thin films with different annealing schedules

Fatigue-free Bi_3.2La_0.8Ti₃O₁₂ ferroelectric thin films were successfully prepared on p-Si (100) substrates using metalorganic solution deposition process. The orientation and formation of 5-layers thin films were studied under different processing conditions using XRD. Experimental results indicate that increase in annealing time at 700 °C after preannealing for 10 min at 400 °C can remarkably increase (200)-orientation of the films derived from the precursor solutions with two contents of citric acid. Meanwhile, high content of citric acid increases the film thickness and is conducive to the a-orientation of the films with the preannealing, and low concentration of the solution is conducive to the c-orientation of the films without the preannealing.     

The Mechanical Properties of Skutterudite CoAs3 by Molecular Dynamics （MD） Simulation

Skutterudite CoAs3 is a potentially important thermoelectric material. Morse potential is employed here to carry out molecular dynamics simulations of nanobulk CoAs3 at the temperature of 0 K. The stress-strain relationships under uniaxial tensile and/or compressive strain are obtained. The elastic modulus, extreme strength and deformation mechanism are studied. The simulation results indicate that nanobulk CoAs3 abruptly ruptures at much higher strain level under tension than conventional bulk CoAs3. Both the extreme stresses under tension and compression are much higher than those of conventional bulk CoAs3.     

Microstructures and fatigue-free properties of the La<Superscript>3+</Superscript> and Nd<Superscript>3+</Superscript> doped Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films prepared by modified sol-gel technique

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) and Bi_3.15Nd_0.85Ti₃O₁₂ (BNT) thin films were fabricated on Pt/TiO₂/SiO₂/Si (100) substrates by a modified sol-gel technique. X-ray diffraction indicated that these films were of single phase with random polycrystalline orientations. The surface morphologies of the films were observed by scanning electron microscope, showing uniform, dense films with grain size of 50–100 nm. Well-saturated hysteresis loops of the films were obtained in metal-ferroelectric-metal type capacitors with Cu top electrodes at an applied voltage of 400 kV/cm, giving the remanent polarization (2P _r) and coercive field (2E _c) values of the films of 25.1 μC/cm² and 203 kV/cm for BLT, and 44.2 μC/cm² and 296 kV/cm for BNT, respectively. Moreover, these capacitors did not show fatigue behaviors after up to 1.75×10¹⁰ switching cycles at the test frequency of 1 MHz, suggesting a fatigue-free character. The influences of the La³⁺ and Nd³⁺ doping on the properties of the films were comparatively discussed. Supported by the National Key Basic Research and Development Program of China (Grant No. 2006CB932305) and the Natural Science Foundation of Hubei Province, China (Grant No. 2004ABA082)     

Effect of La doping on microstructure and ferroelectric properties of Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films prepared by sol-gel method

The Bi4Ti3Oi2 and Bi3.25La0.75Ti3O12 thin films were prepared on the Pt/Ti/SiO2/Si substrate using the sol-gel method. The effect of La doping on the microstructure and ferroelectric properties of Bi4Ti3O12 films were investigated. Both the Bi4Ti3O12 and Bi3.25La0.75Ti3O12 thin films exhibited typical bismuth layered perovskite structure. The 2Pr （remanent polarization） value of Bi3.25La0.75Ti3O12 thin films is 18.6 μC/cm^2, which is much larger than that of Bi4Ti3O12 thin films. And the Bi3.2eLa0.75Ti3O12 films show fatigue-free behavior, while the Bi4Ti3O12 thin films exhibit the fatigue problem. The mechanism of improvement of La doping was discussed.     

Nanocomposite films of V<Subscript>2</Subscript>O<Subscript>5</Subscript>−MoO<Subscript>3</Subscript> xerogel with poly ethylene oxide intercalation

Poly ethylene oxide (PEO)_x−V₂O₅−V₂O₅−MoO₃ (x=0, 0.5, 1) films were prepared by the sol-gel method. The synthesis and structure of the films were investigated by XRD, TG-DTA, FTIR, etc. The results show that V₂O₅−MoO₃ xerogel has a layered structure and its interlayer space increased from 1.3181 nm at x=0 to 1. 7898 nm at x=1 after the nanocomposite films were dried, and PEO in the interlayer changes the interface structure by forming hydrogen bonds with V=0 bands. CV measurement indicates that the intercalation of PEO improves insertion/extration properties of Li⁺ ions in the interlayer. ZHENG Jin-xia: Born in 1976 Funded by the National Natural Science Foundation of China (No. 50172036) and Natural Science Foundation of Hubei Province(No. 2001ABB083)     

Optical bandgap energy of CH<Subscript>3</Subscript>NH<Subscript>3</Subscript>PbI<Subscript>3</Subscript> perovskite studied by photoconductivity and reflectance spectroscopy

Organic-inorganic hybrid perovskite materials have been receiving considerable attention due to their promising applications in many optoelectronic fields. However, the optical bandgap of CH₃NH₃PbI₃ perovskite is still disputed. In order to comprehend the intrinsic characteristics of these materials, we study the near-band-edge optical responses of the solution-processed CH₃NH₃PbI₃ perovskite crystals by photoconductivity and reflectance spectroscopy at room temperature. All these spectra of the CH₃NH₃PbI₃ polycrystals show only one significant absorption edge at 1.58 eV. However, we observe an extra absorption edge at 1.47 eV in CH₃NH₃PbI₃ single crystal. We establish a simple kinetic model of charge annihilation processes to explain why the low-energy structure of the photoconductivity and diffuse reflectance spectra of CH₃NH₃PbI₃ polycrystals disappear, which provides another possibility for understanding the difference in absorption edge. It is noteworthy that this low-energy absorption edge of CH₃NH₃PbI₃ single crystal has, to the best of our knowledge, seldom been reported on organic-inorganic hybrid perovskites. Therefore, the CH₃NH₃PbI₃ single crystal exhibits a relatively wide absorption which makes it a promising candidate for photoelectric applications.     

Synthesis,characterization and catalytic application of H<Subscript>3</Subscript>PW<Subscript>12</Subscript>O<Subscript>40</Subscript>/MCM-48 in the esterification of methacrylic acid with n-butyl alcohol

A novel environmental friendly catalyst, H3PW12O40/MCM-48, was prepared by impregnation method. The catalysts were characterized by means of XRD and FT-IR. The synthesis of n-butyl methacrylate catalyzed by H3PW12O40/MCM-48 was studied with methacrylic acid and n-butyl alcohol as reactants. H3PW12O40/MCM-48 is an excellent catalyst for synthesizing n-butyl methacrylate and Keggin structure of H3PW12O40 kept unchanged after being impregnated on surface of the molecular sieve support. Effects of n（methacrylic acid）：n（n-butyl alcohol）, catalyst dosage, cyclohexane（water-stripped reagent） and reaction time on yields of the product were investigated. The optimum conditions have been found, that is, molar ratio of acid to alcohol is 1：1.6, mass ratio of catalyst used to the reactants is 0.5% and reaction time is 2.0 h. Under these conditions, the yield of n-butyl methacrylate can reach 93.7%.     

Microstructure and AMR Properties of Permalloy Films Sputtered on （Ni0.81Fe0. 19 ）0.66Cr0.34 Buffer

(Ni_0.81 Fe_0.19)_0.66 Cr_0.34 has a high resistivity and a crystal structure close to that of Ni_0.81 Fe_0.19. The electrical and X-ray diffraction measurements prove that a thin NiFeCr seed layer induces a well (111)-orented Ni_0.81 Fe_0.19 film. Post-annealing treatment improves the magnetic properties of (Ni_0.81Fe_0.19)_0.66 Cr_0.34(45Å)/Ni_0.81Fe_0.19 (150Å)/Ta(55Å) thin film prepared under a deposition field, whereas the inter-diffusion of NiFe/Ta deteriorates the magnetoresistance properties of the film.