Ag(TCNQ)准一维微米结构的制备及表征

利用溶液化学反应法制备了准一维结构的金属有机配合物Ag(TCNQ). X射线衍射(XRD)表明，所制备的Ag(TCNQ)为晶态结构;扫描电子显微镜(SEM)的观察证明，Ag(TCNQ)为准一维的微米管或线；Raman 测试结果表明，单根的Ag(TCNQ)形成时,Ag原子与TCNQ分子之间发生了电荷转移.对样品的制备工艺,即 Ag膜厚度和浸入溶液的反应时间对生成Ag(TCNQ)晶体形貌的影响进行了研究.结果表明，Ag膜越薄，生长出的晶体越稀疏;Ag膜与TCNQ乙腈溶液的反应时间影响其形貌的变化.反应历经三个阶段,晶体形成和长大阶段、反应完全阶段及溶解阶段.     

The microstructure and optical transmittance thermal analysis of sodium borosilicate bio-glasses

The conditions to fabricate the bulk porous specimens have been studied on account of sodium borosilicate (NBS) glasses. Glass composition, heat treatment at phase separation and TiO₂ addition have been considered in this study. Original glass samples of composition in mol%: sample A: 9.19 Na₂O - 23.58 B₂O₃ - 67.23 SiO₂, sample B: 9.29 Na₂O - 3.17 TiO₂ - 23.82 B₂O₃ - 63.72 SiO₂ were prepared by melting reagent grade chemicals (Na₂CO₃, HBO₃, SiO₂ and AgNO₃) in platinum crucibles at 1480°C for 1 h in air. The melts were poured onto stainless steel plates and were annealed at 500°C for 0.5 h after cooling. Thus, obtained samples were phase separated at 700°C for 2, 15, 25 and 50 h to study their microstructure by scanning electron microscope (SEM). Besides the direct study of the microstructure by SEM, information on glass structural changes of samples are provided by measuring in situ changes by the optical transmittance thermal analysis. The isothermal measurements were carried out at 700, 720 and 740°C. The temperature of phase separation, the leaching and nucleator addition (TiO₂), significantly influence the microstructure of the resulting leached product. TiO₂ additive seems to suppress crystallization of cristobalite: especially at the extended above heat treatment phase separation runs. The phase-separated domains of glasses containing above 80 moles of SiO₂ are so small that it is very hard to observe them by SEM. The glass composition in our case was selected in a way to have relatively large phase separated areas easily observed by SEM at magnification 20 000·. The influence of TiO₂ is not too pronounced. It seems to suppress the cristobalite crystallization, especially of longer heating runs. The image analysis of leached glasses shows the prevailing content of the skeletal phase in a comparison to pores. The TiO₂ content diminishes the content of the skeletal phase. This revised version was published online in July 2006 with corrections to the Cover Date.     

Microporous SiO2 and SiO2/MOx (M=Ti,Zr, Al) for ceramic membrane applications: A microstructural study of the sol-stage and the consolidated state

Microporous SiO₂ and SiO₂/MO₂ (M=Ti, Zr, Al; 10 mol% MO_x) materials for gas separation membrane applications have been prepared from polymeric sols. Characterization of these sols with SAXS showed that the mean fractal dimension of the SiO₂ sols is 1.3–1.4 with a radius of gyration of approximately 2.5 nm. The dried and calcined films are microporous and the pore size distribution was bimodal with maxima at diameters of 0.5 nm and 0.75 nm. For the SiO₂/TiO₂, SiO₂/ZrO₂ and SiO₂/Al₂O₃ systems, much milder reaction conditions proved to be necessary to obtain sols with comparable fractal dimensions due to the high reactivity of the Ti/Zr/Al-alkoxides. Microporous supported membranes with molecular sieve-like gas transport properties can be prepared from a relatively wide range of sol structures: from polymers too small to characterize with SAXS to structures with fractal dimensions: 1<d _f<2.04.     

TiO2表面电子结构及其光催化活性

利用ＨＣｌ和ＨＣｌＯ４对不同方法制备的ＴｉＯ２进行了表面修饰,发现经强酸修饰后ＴｉＯ２的光催化活性有明显提高,其中ＨＣｌ的修饰效果好于ＨＣｌＯ４。     

Lattice orientation within stirring-induced crystals of polyethylene

Micro-shish-kebab stirring-induced polyethylene crystals, as defined and described in the preceding paper, are flat, ribbon-shaped fibers. Selected area electron-diffraction techniques were used to determine the orientation of the crystal axes with respect to the external fiber shape. It has been shown that in addition to the crystal-lographic c-axis laying along the fiber direction, the normal to the ribbon plane is parallel to the crystallographic a-axis.     

Stroboscopic microscopy—direct imaging of structure development and phase separation during spin‐coating

Spin‐coated polymer blends possess a rich variety of accessible non‐equilibrium morphologies, formed through a process of phase separation and self‐assembly, the complexities of which remain incompletely understood. The technique of stroboscopic microscopy has now been developed to allow direct observations of microscopic and mesoscopic morphological development during spin‐coating and has afforded unequivocal information regarding morphological development. The technique so far has three modes of operation providing information on topographical, compositional, and crystal development. In this review, we look at the technique's development, its applications and comment on the future potential for this technique. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 17–25     

Limit theorems for the pre-averaged Hayashi–Yoshida estimator with random sampling

We will focus on estimating the integrated covariance of two diffusion processes observed in a nonsynchronous manner. The observation data is contaminated by some noise, which possibly depends on the time and the latent diffusion processes, while the sampling times also possibly depend on the observed processes. In a high-frequency setting, we consider a modified version of the pre-averaged Hayashi–Yoshida estimator, and we show that such a kind of estimator has the consistency and the asymptotic mixed normality, and attains the optimal rate of convergence.     

简单方法制备与表征新颖复合凝胶及表面微结构——由科研成果转化的化学综合实验

材料表面的微结构会赋予材料独特的性能，水凝胶在生物医学领域有广泛的应用前景。采用紫外光刻蚀法创新性地实现了复合凝胶的制备和凝胶表面图案化微结构的构筑一步完成；通过原子力显微镜和光学显微镜的表征，复合凝胶聚N-异丙基丙烯酰胺/聚乙二醇二丙烯酸酯兼具了温敏性能与图案化微结构的新颖性能结构特征。本实验有助于培养学生的创新意识，激发学生的学习兴趣以及未来从事科研的兴趣。     

Analysis of polished polycrystalline diamond using dual beam focused ion beam microscopy

This paper presents a study on polycrystalline diamond (PCD) polished by dynamic friction polishing (DFP) with the aid of advanced dual beam FIB (focused ion beam) microscopy. After disclosing a variety of wear tracks by DFP using electron imaging in combination with the ion channelling effect, a dual beam FIB was successfully employed at wear track sites to specifically create both the large cross-sectional specimen for microanalysis and thin foil for nanoanalysis. The study concluded that the polished PCD subsurface was free from microscale cracking. However, the attached debris layer on the top surface contained metal oxides and non-diamond carbon phase with inhomogeneous distributions of C, Fe, Cr, Ni, Si and O across the layer. An attached layer directly above a diamond grain was composed of essentially amorphous carbon, suggesting that a direct phase transformation from diamond crystalline to amorphous occurred during DFP.     

Living anionic polymerization of (E)‐1,3‐pentadiene and (Z)‐1,3‐pentadiene isomers

The anionic polymerization of (E)‐1,3‐pentadiene (EP) and (Z)‐1,3‐pentadiene (ZP) together with mixture of the E/Z isomers are investigated, respectively. The kinetic analysis shows that the activation energy for EP (86.17 kJ/mol) is much higher than that for ZP (59.03 kJ/mol). GPC shows that it is the EP rather than the ZP isomer that undergoes anionic living polymerization affording quantitative products of the polymers with well‐controlled molecular weights and narrow molecular weight distributions (1.05 ≤? ≤ 1.09). In addition, THF as polar additive has proved its validity to reduce the molecular weight distribution of poly(ZP) from 1.38 to as low as 1.19. The microstructure and sequence distributions of polypentadiene are characterized by ¹H NMR and quantitative ¹³C NMR. Finally, the distinctive reaction activity of two isomers can be elucidated by two different mechanisms which involve the presence of four forms of zwitterions for EP and the typical [1,5]‐sigmatropic hydrogen‐shift phenomenon for ZP. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 54, 2291–2301