介孔空心球状WC微球结构与晶相形成机理

采用喷雾干燥微球化处理-气固反应法制备了介孔空心球状WC微球，应用扫描电子显微镜(SEM)对微球的形貌变化进行了表征。结果表明，介孔空心球状结构是逐步形成的。其中，空心球状结构形成于前驱体微球化处理过程中，介孔结构形成于空心微球还原碳化过程中。在与样品制备工艺条件相同的情况下，采用原位X射线衍射技术(in situ XRD)对样品的晶相演变规律进行了监测。结果表明，样品在CO/CO₂气氛中进行还原碳化时，当温度缓慢而连续上升到750 ℃时，其晶相变化遵循AMT → WO₃ → WO₂ → W₂C → WC规律;当采用“阶跃式”升温，即温度缓慢而连续上升到400 ℃，然后再快速上升到750 ℃，并在750 ℃下进行还原碳化时，其晶相变化规律为AMT → WO₃ → WO₂ → WC。这说明，样品的晶相演变不仅与还原碳化温度和时间有关，而且与升温方式和升温速率有关。     

Hollow Cancrinite Zeolite Spheres in situ Transformed from Fly Ash Cenosphere

A novel hollow microsphere structure with cancrinite zeolite grown from the shell of fly ash cenosphere has been successfully prepared through in situ transformation in vapor phase; the orientation and morphology of cancrinite can be greatly improved by adding tetrapropylammonium hydrate into the synthetic system.     

Morphological investigations of crosslinked polystyrene microspheres by seeded polymerization

 Crosslinked polystyrene microspheres with novel surface and inner morphologies were synthesized by seeded polymerization following a seed-swelling method, using uncrosslinked polystyrene microspheres as seeds and a mixture of toluene, styrene (St), and divinylbenzene (DVB) as the swelling agent. With the increasing toluene/ (St+DVB) ratio, the crosslinked particles changed from smooth-surfaced spheres to deformed spheres with dimples or heavy dents at the surface. A single hole inside the spherical particles was produced at low St/DVB ratio, while higher St/DVB ratios gave irregular dented or dimpled particles. Ultrathin cross-section observation by TEM revealed a non-uniformly crosslinked inner structure. Received: 20 January 1998 Accepted: 14 April 1998     

溶剂热微乳法合成CdS微米球

CdS microspheres were prepared by a hydrothermal microemulsion method in cyclohexane/Triton X-100/pentanol/water at 180℃. The as-prepared samples were characterized by X-ray diffraction analysis, transmission electron microscopy, electron diffraction, energy diffraction X-ray analysis and photoluminescence spectra. It was found that CdS microspheres with diameter of 1.5-2.5μm were aggregated by nanocrystals. The formation mechanism was proposed.     

Adsorption of trypsin onto styrene-2-hydroxyethyl methacrylate copolymer microspheres and its enzymatic activity

Effects of the surface hydrophilicity of styrene-2-hydroxyethyl methacrylate (S-HEMA) copolymer microspheres on the adsorption immobilization of trypsin and on its enzymatic activity were discussed. In the case of a polystyrene (PS) microsphere, the amount of adsorption was large, whereas the enzymatic activity of the adsorbed trypsin was low. On the other hand, in the case of an S-HEMA copolymer microsphere whose HEMA content was 10 mole %, the maximum specific activity of trypsin adsorbed was nearly equal to that of free trypsin, although the amount of adsorption decreased to about 65 % of that in PS. Accordingly, total activity, which is the product of the amount of adsorption and the specific activity, could be enhanced by controlling the surface hydrophilicity of the microsphere.Part LXXXVII of the series Studies on Suspension and Emulsion.     

单分散亚微米级磁性微球的合成

以磁性氧化铁胶体粒子为种子粒子，采用吸附－溶胀法，进行苯乙烯－丙烯酸－二乙烯基苯的乳液聚合，制备亚微米级磁性高分了微球。研究了分散介质、丙烯酸、种子粒子、苯乙烯和ＰＨ调节剂等因素对聚合行为和磁性微球的影响，成功地合成了平均粒径为０．１３和０．２７μｍ、单分散性很好的磁性微球。     

A new rapid ultra‐performance liquid chromatography method for the pharmacokinetic and bioavailability study of diclofenac sodium aqueous injection and lipid microsphere injection in rats

A novel, rapid and selective ultra performance liquid chromatography mass spectrometric method had been developed for the pharmacokinetic study of diclofenac sodium (DS) after single intravenous injection of DS aqueous injection and DS lipid microsphere (LM) injection in rats. Ketoprofen (KP) was used as internal standard. Samples were treated by a one‐step liquid liquid extraction. Separation was performed on an Acquity UPLC? BEH C₁₈ column (50 × 2.1 mm i.d., 1.7 μm). The mobile phase consisted of acetonitrile–0.1% ammonium hydroxide aqueous solution (20 : 80, v/v) initially in the gradient mode. The detection was carried out by means of electrospray ionization mass spectrometry in negative ion mode with multiple‐reaction monitoring mode. Standard curves showed good linearity (r > 0.99) from the plasma concentration of 0.1–50 μg/mL. The lower limit of quantification was 0.1 μg/mL. The intra‐ and inter‐day precisions and the accuracy all satisfied the acceptance criteria. The developed method was validated and successfully applied to the pharmacokinetics study of DS aqueous injection and LM injection. The results showed that the two preparations were bioequivalent in rats. Copyright © 2009 John Wiley & Sons, Ltd.     

Interfacial deformation of confined photocurable fluid for fabrication of shape-imprinted microspheres

This study presents a simple route to fabricate shape imprinted microspheres and their application toward multiplex immunoassay. Specifically, a photocurable fluid (polyethylene glycol diacrylate, [PEGDA]) confined in a micromold results in drop formation due to mold swelling and capillarity upon addition of immiscible wetting fluid; during this formation, part of the photocurable fluid is entrapped at the swollen open end, thereby producing polymeric microspheres with controlled imprinted shapes on their surface upon photopolymerization. This approach is able to produce highly uniform microspheres with different imprinted shapes depending on mold geometry in a consistent manner; their size can also be tuned by varying mold dimensions. Furthermore, we impart amine-reactive functional groups to the microsphere, which allows them to be functionalized efficiently. Lastly, we conjugate different capture antibodies on microspheres with different imprinted shapes, and these microspheres were demonstrated to be shape-encoded suspension arrays for multiplex immunoassays. This technique provides high selectivity and a simple decoding method for biosensing applications.     

Synthesis of polymer microsphere-supported chiral pyrrolidine catalysts by precipitation polymerization and their application to asymmetric Michael addition reactions

Polymer microsphere-supported chiral pyrrolidine catalysts were successfully synthesized by a precipitation polymerization incorporating a methacrylate monomer bearing chiral N-Boc-pyrrolidine moiety, followed by removal of the N-Boc groups. The resulting polymeric catalysts were applied to the asymmetric Michael addition reactions of aldehydes with alkyl vinyl ketones. The effects of the comonomer, the molar ratios within the catalyst, the catalyst loading, the temperature, and the solvent on the catalytic performance were investigated in detail. The reactions were found to proceed smoothly in the absence of a solvent. A hydrophobic polystyrene-based chiral pyrrolidine catalyst exhibited high reactivity (up to 97% yield) and enantioselectivity (up to 95% ee) during these reactions. The catalyst could also be recovered and reused up to five times without significant loss of activity.     

Photonic nanojet‐mediated SERS technique for enhancing the Raman scattering of a few molecules

We report a two‐step enhancement of Raman scattering signal (η) of a few dye molecules. In the first step, high‐quality surface‐enhanced Raman scattering (SERS) substrates have been used. The SERS substrates were fabricated by direct current sputtering of Au followed by thermal annealing. The role of thermal annealing of the SERS substrates and numerical aperture of Raman microscopic objective lens on the enhancement has been studied for optimizing the enhancement in the SERS technique. In the second step, the value of η obtained with conventional SERS technique has been improved significantly with the help of photonic nanojet (PNJ) of an optical microsphere (PNJ‐mediated SERS technique). The signal to noise ratio and reproducibility of the experimental results have been found to be very high. Based on our theoretical simulations on PNJ, a few suitable parameters have been proposed for obtaining better enhancement using this technique. To the best of our belief, this report will enable the SERS community to improve η value with ease. Copyright © 2016 John Wiley & Sons, Ltd.