茶多酚铝盐热分解法制备氧化铝纳米微粉

以茶多酚为沉淀剂,在溶液中与AlCl3充分反应,生成茶多酚铝盐前驱体,沉淀的最佳pH值为5．6,后者在空气中1030℃左右热处理90—150min制得质量分数为99．51％的AlCl3。样品的TEM、XRD和DTA分析结果表明,所得氧化铝样品为α-AlCl3,粒径约50nm。     

阴极等离子体电解法制备氧化铝纳米颗粒

以金属铝为阴极材料,以3mol·L-1浓度的NH4NO3水溶液为电解液,采用非对称电极阴极等离子体电解方法制备出氧化铝纳米颗粒.采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线能量色散谱(EDX)、X射线衍射(XRD)和X射线光电子能谱(XPS)对颗粒的形貌和结构进行了表征.结果表明颗粒以立方相Al2O3为主.还对放电过程的电流变化和发光现象进行了研究.结合实验结果提出了这种颗粒的生长机制.     

超临界抗溶剂微粒化的过程调控及应用

超临界抗溶剂技术已广泛应用于超导材料、颜料、聚合物、炸药及药物制备等领域,是一种与传统方法相比有很多优点的新型微粒化技术,最主要的优点之一是其过程的可调控性。本文主要介绍了超临界抗溶剂过程及该过程中对粒径及分布、形貌、结晶度等的调控,聚合物机构对颗粒的影响,以及在以聚合物和无机物制备复合粒子方面的应用,并对超临界抗溶剂过程中微粒的成形机理进行了简要的概括,指出了超临界抗溶剂技术在这方面的研究现状及存在的问题,并对其应用前景作了进一步的展望。     

发泡法合成纳米氧化铝

采用发泡法合在了粒径约为15nm的氧化铝。考察了发泡剂种类,发泡剂（柠檬酸）Al^3 ,蒸发温度,发泡温度等制度条件对粒子形成过程及粒径的影响,结果表明,发泡剂的稳定性和适度的络合能力是合成纳米氧化铝的重要因素,在有机配体（柠檬酸,乙二胺四乙酸）和水溶性高分子（聚乙烯醇,聚乙二醇）中,得到的柠檬酸粒径最小,在制备条件中蒸发温度和发泡温度对得到的氧化铝颗粒的影响较大,蒸发温度在70－90℃,发泡温度在120－150℃时为最佳,用XRD,IR,DTG－DSC,TEM和NMR等方法进行表征,探讨了发泡剂在合成纳米氧化铝过程中的作用。     

超临界co2中模板法制备氧化铝多孔材料

超临界co2;活性炭;模板;氧化铝;多孔     

微乳液法制备CaF2纳米颗粒

目前 ,通过微乳液合成方法已成功地制备出许多种类的化合物纳米微粒[1,2 ] .Bender等[3] 曾用微乳液法制备出掺杂钕的 Ba F2 纳米颗粒 ,并研究了其荧光特性 ,样品的最大发射波长为 1 0 52 nm,荧光寿命为 3 50～ 90 0 ns,在适当的钕掺杂浓度下 ,获得了较高的荧光强度 .Qiu等[4 ] 也于微乳液体系中制备出 Ce F3纳米颗粒 .纳米复合体系 (Mg2 Si O4 ∶Cr)可以用作光放大材料[5] ,其光学增益可以与路径长度相当的单晶体相比拟 .基于掺杂稀土离子的氟化物纳米复合体系存在着巨大的应用前景 ,本文用微乳液技术首次制备出 Ca F2 纳米微粒 ,为研…     

超临界二氧化碳光聚合制备可交联含氟聚合物颗粒及应用

通过自由基无规共聚和酰化反应两步法制备了两类侧链含丙烯酸酯双键的含氟低聚物,并通过调节反应物种类、配比和链转移剂用量,制备出一系列不同双键含量、氟含量的多官能度低聚物。以制备的含氟低聚物为原料,进行超临界二氧化碳光聚合制粒。聚合得到的含氟颗粒作为增强相,加入TPGDA光固化配方中,可实现颗粒与树脂的化学交联,显著提高基材的交联密度,改善疏水性,降低吸水率,并增强热稳定性。     

溶胶-凝胶法制备纳米二氧化钛颗粒的研究

本文采用钛酸丁脂等原料,利用sol-gel方法制备了TiO2纳米颗粒.研究了不同实验顺序(滴入方式)和工艺参数对制备效果的影响.通过实验和对TiO2纳米粉末的TEM分析,获得了粒度(30-40nm)比较均匀的球型TiO2纳米颗粒.     

纳米氧化铝制备中若干反应过程的研究

本文报道纳米氧化铝材料研制中若干关键步骤的反应过程的考察结果.(1)铝酸钠溶液与碳酸氢钠溶液混合后,产生无定形氢氧化铝沉淀.在碳酸氢钠未大量过剩条件下,氢氧化铝沉淀前有一个反应诱导期.在此期间溶液的紫外吸收光谱已有显著变化.在260nm附近紫外吸收增强;和Ba2[Al2(OH)10]等含六配位铝原子的晶体的紫外光谱对比,讨论了铝酸钠溶液分解的机理;(2)实验表明:和丝钠铝石相比,在上述反应条件下无定形氢氧化铝不是平衡固相而是亚稳相;(3)实验表明:无定形氢氧化铝在拍散和凝胶形成过程中晶化,形成拟薄水铝石.     

水溶液法制备CeF3纳米颗粒

氟化铈(CeF3)具有很高的离子电导率［1］和独特的光学特性［2］, 可用于制作化学传感器和光学元器件. CeF3还是良好的固体润滑剂［3］. 近年来的研究结果表明, 与氟化物粗晶材料相比, 纳米尺度的氟化物的性能有显著的提高， 因此, 其制备方法也很受关注. 目前, 制备氟化物纳米颗粒的方法有蒸发法［4］、 微乳液法［2, 5~8］、 水醇混合溶液法［3,9］和微波固相氧化还原合成法［10］等. 但是, 水溶液直接沉淀法作为一种操作简单, 成本低, 适合批量生产的制备方法尚未见用于制备纳米CeF3颗粒.     

Preparation of Alumina Aerogel Films by Low Temperature CO2 Supercritical Drying Process

Alumina aerogel thin films were formed by a new synthesis route. Sols were prepared by the Yoldas process. Gels were formed by sol evaporation in a few hours. Films were prepared by dip coating glass or alumina substrates into both the sols and the gels. Aerogel films with special morphology were produced for the first time by exchanging the film solvent with acetone after the dip coating, followed by supercritical drying. The morphology of the films, studied by SEM and TEM, consists of fiber-like network of round chains (≈0.1 μm thick), and pores (0.1–0.5 μm in diameter). It is shown that the fibers contain a homogeneous arrangement of sol particles, 2–4 nm in size. Formation of this microstructure can be attributed to phase separation in the alumina-water-acetone system in a 2D film geometry. A conceptual model for the film development is proposed.     

Loading of Bacterial Cellulose Aerogels with Bioactive Compounds by Antisolvent Precipitation with Supercritical Carbon Dioxide

Bacterial cellulose aerogels overcome the drawback of shrinking during preparation by drying with supercritical CO₂. Thus, the pore network of these gels is fully accessible. These materials can be fully rewetted to 100% of its initial water content, without collapsing of the structure due to surface tension of the rewetting solvent. This rehydration property and the high pore volume of these material rendered bacterial cellulose aerogels very interesting as controlled release matrices. Supercritical CO₂ drying, the method of choice for aerogel preparation, can simultaneously be used to precipitate solutes within the cellulose matrix and thus to load bacterial cellulose aerogels with active substances. This process, frequently termed supercritical antisolvent precipitation, is able to perform production of the actual aerogel and its loading in one single preparation step. In this work, the loading of a bacterial cellulose aerogel matrix with two model substances, namely dexpanthenol and L-ascorbic acid, and the release behavior from the matrix were studied. A mathematical release model was applied to model the interactions between the solutes and the cellulose matrix. The bacterial cellulose aerogels were easily equipped with the reagents by supercritical antisolvent precipitation. Loading isotherms as well as release kinetics indicated no specific interaction between matrix and loaded substances. Hence, loading and release can be controlled and predicted just by varying the thickness of the gel and the solute concentration in the loading bath.     

超临界二氧化碳中功能化聚乙二醇稳定的钯纳米粒子催化醇的选择氧化反应

 以超临界二氧化碳 (scCO2)/聚乙二醇 (PEG) 两相为反应介质, 双齿氮配体功能化聚乙二醇稳定的 Pd 纳米颗粒作为催化剂, 进行了醇的需氧氧化反应. 系统研究了催化剂制备条件和反应条件对苯甲醇需氧氧化反应的影响. 结果表明, 以氢气为还原剂制备的 Pd 纳米粒子的催化活性最高. 反应结束后, 可以利用 scCO2 直接进行原位萃取得到产物, 实现了催化剂与产物的有效分离和催化剂的循环使用. 反应中没有检测到钯的流失. 催化剂经过 5 次循环利用后转化率仍可达 98%.     

制备超细微粒的超临界流体沉淀技术新进展

超临界流体沉淀(SFP)技术以其特有的优点成为具有广阔应用前景的超细微粒制备方法.本文着重综述了气体饱和溶液沉析(PGSS)、超临界辅助雾化(SAA)和膨胀液体有机溶液减压(DELOS)等最新SFP技术的原理、特点及相关的应用,指出了目前SFP技术存在的问题及今后的研究方向.     

微等离子体氧化Al2O3陶瓷膜的组织结构与形成过程

The alumina ceramic coatings were prepared on aluminum alloy using micro-plasma oxidation. The structure and morphologies of ceramic coatings were studied by X-ray diffraction (XRD) and scanning electron microscope (SEM), and then its formation process was investigated. The results of XRD reveal that with increasing oxidation time the content of γ-Al₂O₃in the ceramic coatings decreases, and in which the content of α-Al₂O₃increases. The results of SEM show that many crater-mouth like traces formed by the plasma discharge are observed on the coatings surface, it indicates when the plasma is discharging, a plasma thermal chemical reaction occurs between the aluminum from the substrate and the oxygen and other ions from the electrolyte. The reaction products then are propelled away from the inner-wall of the discharging channels. Finally, these products agglomerate in the inner-wall of the discharging channels and on the surface near the discharging channels to produce the ceramic coatings. The change of ceramic coatings thickness with increasing oxidation time divides into two stages, and the final thickness is formed in first stage. With increasing current density the final thickness of ceramic coatings increases.     

超临界CO2中以活性碳为模板由TEOS制备多孔SiO2

在超临界CO2中以活性碳为模板由正硅酸乙酯(TEOS)前体涂层焙烧法制备多孔SiO2材料。结构分析表明,超临界涂层法制备的多孔SiO2材料的比表面积、比孔容和平均孔径分别达到1147m2/g、1.4cm3/g和2.20nm,优于常规液相浸渍涂层法。并研究了活性碳含水量、超临界涂层的温度和压力等因素对涂层效果的影响,确定了较好的涂层条件。     

超临界二氧化碳流体在酶催化反应中的应用

酶催化反应已发展到了利用超临界二氧化碳流体为介质来进行。文章评述了在超临界二氧化碳中影响酶活性和稳定性的重要因素，介绍了SCCO2介质中酶催化反应的最新进展。     

用超临界CO2制备疏水改性聚丙烯酸

用超临界CO2制备疏水改性聚丙烯酸;丙烯酸十八酯;超临界二氧化碳;疏水缔合