Derivatization of 1-phenyl substituted 4-amino-2-benzazepin-3-ones: evaluation of Pd-catalyzed coupling reactions

Several Pd-catalyzed reactions were explored to further functionalize the bromo-substituted 4-amino-1,2,4,5-tetrahydro-2-benzazepin-3-one scaffold (Aba). We report in this paper suitable reaction conditions for Suzuki, Buchwald-Hartwig, and Heck reactions. The substitution pattern of the starting aminobenzazepinone turned out to be crucial for the success of these transition metal-catalyzed reactions, which often required modifications of standard literature procedures. The Pd-catalyzed methods provide access to novel substitution patterns of the Aba scaffold.     

敏化光波长对(Fe,Ni):LiNbO3晶体全息记录性能的影响

分别采用514 nm绿光、488 nm蓝光和390 nm紫外光作为敏化光,633 nm红光作为记录光,详细研究了敏化光波长对氧化(Fe,Ni):LiNbO3晶体全息记录性能的影响.结果表明:随着敏化光波长的逐渐减小,氧化(Fe,Ni):LiNbO3晶体的非挥发全息记录性能逐渐优化,390 nm紫外光是这三种敏化光中最优的敏化光.考虑敏化光的吸收,为了在双中心全息记录中获得最优的性能,应当选择合适波长的敏化光:一方面短波长敏化光能有效地敏化深中心;另一方面短波长敏化光的吸收太强(如对光折变效应无用的基质吸收),不能沿厚度方向有效地敏化晶体,所以实际上需折衷考虑,并从理论上给予了解释.     

Qualitative properties of stationary measures for three-dimensional Navier-Stokes equations

The paper is devoted to studying the distribution of stationary solutions for 3D Navier-Stokes equations perturbed by a random force. Under a non-degeneracy assumption, we show that the support of such a distribution coincides with the entire phase space, and its finite-dimensional projections are minorised by a measure possessing an almost surely positive smooth density with respect to the Lebesgue measure. Similar assertions are true for weak solutions of the Cauchy problem with a regular initial function. The results of this paper were announced in the short note [A. Shirikyan, Controllability of three-dimensional Navier-Stokes equations and applications, in: Sémin. Équ. Dériv. Partielles, 2005-2006, École Polytech., Palaiseau, 2006].     

基于频域方法的三维物体分层重现

基于频域方法实现了数字记录和再现三维物体离轴全息图.通过频谱对应关系求得各个面的频谱分布,使用数字滤波方法,成功地消除了零级衍射和共轭像;通过改变再现距离,分别获取了三维物体各个截面的再现像.     

Influence of SiO2 in SiCp on the microstructure and impact strength of Al/SiCp composites fabricated by pressureless infiltration

The effect of SiO₂ in SiC_p and the following processing parameters on the microstructure and impact strength of Al/SiC_p composites fabricated by pressureless infiltration was investigated: Mg content in the aluminum alloy, SiC particle size, and holding time. Preforms of SiC_p in the form of rectangular bars (10 × 1 × 1 cm) were infiltrated at 1150°C in an argon→nitrogen atmosphere for 45 and 60 min by utilizing two aluminum alloys (Al-6 Mg-11 Si and Al-9 Mg-11 Si, wt.%). The results obtained show that the presence of SiO₂ in SiC affects the microstructure and impact strength of the composites significantly. When Al₄C₃ is formed, the impact strength decreases. However, a high proportion of SiC to SiO₂ limits the formation of the unwanted Al₄C₃ phase in the composites. Also, a higher content of Mg in the Al alloy lowers the residual porosity and, consequently, increases the composite strength. The impact strength grows with decrease in SiC particle size and increases considerably when the residual porosity is less than 1%. Russian translation published in Mekhanika Kompozitnykh Materialov, Vol. 42, No. 3, pp. 401–418, May–June, 2006.     

1.5μm波段基于级联二阶非线性的铌酸锂光波导全光波长变换的理论分析

研究了基于级联二阶非线性的铌酸锂波导全光波长变换器的特性.首先从耦合模方程出发,比较了数值分析结果与小信号近似分析的结果.其次在数值分析基础上,分析了铌酸锂晶体的温度变化导致相应基频光波波长与极化反转光栅周期的变化关系.最后分析了在不同相互作用长度下,转换的光波功率与有效基频光波波长带宽、温度调谐带宽、极化反转光栅周期带宽等关系,以对全光波长变换器件进行优化设计 关键词： 级联二阶非线性 波长变换 准位相匹配 铌酸锂光波导     

Synthesis, structure and optical properties of Eu/TiO2 nanocrystals at room temperature

The nanocrystal samples of titanium dioxide doped with europium ion (Eu³⁺/TiO₂ nanocrystal) are synthesized by the sol-gel method with hydrothermal treatment. The Eu³⁺ contents (molar ratio) in the samples are 0, 0.5%, 1%, 2%, 3% and 4%. The X-ray diffraction, UV-Vis spectroscopy data and scanning electron microscope image show that crystallite size is reduced by the doping of Eu³⁺ into TiO₂. Comparing the Raman spectra of TiO₂ with Eu³⁺/TiO₂ (molar ratio Eu³⁺/TiO₂=1%, 2% and 4%) nanocrystals at different annealing temperatures indicates that the anatase-to-rutile phase transformation temperatures of Eu³⁺/TiO₂ nanocrystals are higher than that of TiO₂. This is due to the formation of Eu-O-Ti bonds on the surface of the TiO₂ crystallite, as characterized by the X-ray photoelectron spectroscopy. The photoluminescence spectra of TiO₂ in Eu³⁺/TiO₂ nanocrystals are interpreted by the surface self-trapped and defect-trapped exciton relaxation. The photoluminescence of Eu³⁺ in Eu³⁺/TiO₂ nanocrystals has the strongest emission intensity at 2% of Eu³⁺ concentration.     

Isothermal crystallization kinetics of poly(3‐hydroxybutyrate)/layered double hydroxide nanocomposites

Poly(3‐hydroxybutyrate) (PHB)/layered double hydroxides (LDHs) nanocomposites were prepared by mixing PHB and poly(ethylene glycol) phosphonates (PEOPAs)‐modified LDH (PMLDH) in chloroform solution. Both X‐ray diffraction data and TEM micrographs of PHB/PMLDH nanocomposites indicate that the PMLDHs are randomly dispersed and exfoliated into the PHB matrix. In this study, the effect of PMLDH on the isothermal crystallization behavior of PHB was investigated using a differential scanning calorimeter (DSC) and polarized optical microscopy. Isothermal crystallization results of PHB/PMLDH nanocomposites show that the addition of 2 wt % PMLDH into PHB induced more heterogeneous nucleation in the crystallization significantly increasing the crystallization rate and reducing their activation energy. By adding more PMLDH into the PHB probably causes more steric hindrance of the diffusion of PHB, reducing the transportation ability of polymer chains during crystallization, thus increasing the activation energy. The correlation among crystallization kinetics, melting behavior and crystalline structure of PHB/PMLDH nanocomposites can also be discussed. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 3337–3347, 2006     

Development of a “Built-in” Scanning Near Field Microscope Head for an Atomic Force Microscope System and Stress Mapping of an Al2O3/ZrO2 Eutectic Composite

We constructed a scanning near-field optical microscope (SNOM) on a commercially available atomic force microscopy (AFM) apparatus (SPM-9500J2; Shimadzu Corp.) to measure the stress distribution in ceramic composite materials. Features of our SNOM system are: (1) a compact SNOM head substituted for the original AFM head; (2) a wide scanning range (125 × 125 μm²) inherited from the original scanner; (3) use of conventional shear-force regulation; (4) an optical system for the illumination-collection (I-C) mode; (5) excitation by a 488 nm line of an Ar-ion laser, and (6) light detection by photon counting or a polychromator equipped with an electronically cooled charge coupled device (CCD). This SNOM system was used to measure the surface structure and stress distribution of an Al₂O₃/ZrO₂ eutectic composite. We simultaneously measured topographic images and fluorescence spectra of an Al₂O₃/ZrO₂ eutectic composite. We estimated its peak intensity, peak position, and peak width from the fluorescence spectrum during scanning, which respectively correspond to the abundance of Al₂O₃, stress in the grain, and the anisotropy of that stress. Mapping images showed that the stress and its anisotropy were weaker in the center of the Al₂O₃ grain than its boundary between Al₂O₃ and ZrO₂. That observation suggests that Al₂O₃ underwent intense anisotropic stress induced by volume expansion in the phase transition of ZrO₂ from the cubic phase to the monoclinic phase during preparation.     

Phase transformation of Ni-B, Ni-P diffusion barrier deposited electrolessly on Cu interconnect

In this paper, we report that the phase transformation of Ni-B, Ni-P diffusion barriers deposited electrolessly on Cu, for the reason that the Ni-P layer is a more effective diffusion barrier than the Ni-B layer. The Ni₃B crystallized was decomposed to Ni and B₂O₃ above 400 °C and the Ni₃P crystallized was decomposed to Ni and P₂O₅ above 600 °C respectively in Ar atmosphere. Also, the Ni₃B was decomposed to Ni and free B above 400 °C and the Ni₃P was decomposed to Ni and free P above 600 °C respectively in H₂ atmosphere. The decomposed Ni formed a solid solution with Cu. The Cu diffusion occurred above 400 °C for Ni-B layer and above 600 °C for Ni-P layer, respectively. Because the decomposition temperature of Ni-P layer is about 200 °C higher than that of Ni-B layer, the Ni-P layer is a more effective barrier for Cu than the Ni-B layer.