W/O微乳液制备纳米羟基磷灰石的影响因素研究

W/O微乳液制备的纳米羟基磷灰石粉体具有颗粒细小、团聚度低、分散性好、表面活性高等优点。综述了W/O微乳液制备纳米羟基磷灰石的原理;重点论述了影响粉体粒径和形貌的水油比、表面活性剂与助表面活性剂类型、前驱物浓度、反应温度等因素;并初步展望了该领域的研究发展趋势。     

Sol-gel法在烧结型NdFeB永磁材料表面制备耐蚀纳米MgO膜层的研究

以无机镁盐为前驱物,无水乙醇为溶剂,添加适量的表面活性剂,采用溶胶-凝胶法在烧结型NdFeB永磁材料表面首次成功制备了纳米MgO膜层.讨论了不同工艺条件对溶胶-凝胶稳定性的影响,采用DSC-TGA、XRD、腐蚀浸泡试验等手段对其进行表征,结果表明,前驱物镁离子浓度在0.03～0.15mol/L范围内,v(无水乙醇):v(表面活性剂(火棉胶))=(6:4)～(8:2)时,均能制备出透明、稳定的溶胶;通过最佳热处理工艺在烧结型NdFeB永磁材料表面形成了致密、耐蚀的纳米MgO膜层,且MgO的晶粒取向在{200}和{220}晶面上,在450℃热处理后的MgO平均晶粒尺寸为23.43nm.     

还原氧化石墨烯-贵金属纳米复合物的制备及表征

以氧化石墨和氯铂酸为前驱体,在油胺中简便地合成了还原氧化石墨烯-铂(Reduced graphene oxide-platinum,rGOPt)纳米复合物,并对其进行了表征。透射电子显微镜和光谱测试结果表明,铂纳米颗粒均匀分布在石墨烯表面,尺寸约为30nm,铂纳米粒子为多孔隙结构,结晶性能良好,氧化石墨在高温下转变为还原氧化石墨烯。用此方法也可以制备还原氧化石墨烯-金(rGO-Au)或还原氧化石墨烯-银(rGO-Ag)的纳米复合物,金、银纳米颗粒呈球状,对可见光具有明显的表面等离子吸收。同时,油胺作为溶剂、贵金属盐的还原剂和表面活性剂,使制备过程简单、快捷。     

表面活性剂浓度对纳米介孔SiO2薄膜结构的影响

利用溶胶-凝胶技术,在酸性条件下,采用十六烷基三甲基溴化氨(CTAB)为表面活性剂,正硅酸乙酯为硅源,以及二次去离子水,盐酸为催化剂等原料制备前驱体溶胶.利用表面活性剂与硅源水解后形成的聚集体相互作用,在溶液中形成分子自组装体,通过简单提拉迅速蒸发溶剂等方法制备二氧化硅-表面活性剂纳米介孔薄膜.分析了表面活性剂浓度对薄膜相结构的影响,发现表面活性剂浓度的变化,对薄膜的微结构和性能都有影响,通过调节表面活性剂的浓度可以对该纳米薄膜的微观结构和性能等进行控制,对样品进行了红外光谱,X射线衍射结构分析,原子力显微镜观察表面形貌.     

CTAB辅助水热法合成TiO_2微球

以TiCl3为前驱物,NaCl为矿化剂,十六烷基三甲基溴化铵(CTAB)为表面活性剂,用水热法制备出了纳米TiO2微球。用XRD和SEM对制备的样品进行表征。结果表明:微球为金红石型,直径约为1~5μm,微球由纳米棒放射状组装而成,纳米棒长度约为500nm,直径约为40nm。并研究了表面活性剂浓度、矿化剂浓度、反应时间等实验条件对微球的影响。     

银纳米晶掺杂玻璃基片对Er3+/Yb3+共掺碲酸盐薄膜的荧光增强及其数值模拟

采用电场辅助热扩散工艺制备了银纳米晶掺杂玻璃基片,用非水解溶胶—凝胶法在基片上制备了Er3+/Yb3+共掺碲酸盐薄膜,研究结果表明,玻璃基片中的银纳米颗粒对Er3+/Yb3+共掺碲酸盐薄膜具有明显的荧光增强效果.利用菲克第一、第二定律、欧姆定律、泊松方程对电场辅助热扩散过程进行了数值模拟,计算了玻璃内银的浓度分布.结果表明:玻璃内银纳米颗粒的总量越大、近玻璃表面银纳米颗粒的浓度和粒度越大、银耗尽层的厚度越小,荧光增强效果越好.此外,不仅近玻璃表面的银纳米颗粒可以产生荧光增强效应,而且远离表面的银纳米颗粒也有荧光增强效应.     

表面活性剂对超细BaTiO3纳米颗粒制备的影响

以钛酸四丁酯为钛源,醋酸钡为钡源,采用改进的水热法(即溶剂热法)在低温条件下合成钙钛矿结构的超细钛酸钡纳米颗粒,重点研究表面活性剂对产物的影响,探讨了不同表面活性剂影响产物形貌和种类的作用机理.通过扫描电子显微镜(SEM)、X射线衍射(XRD)及能谱(EDS)对产物进行表征,结果表明加入不同的表面活性剂时,制备的产物不同,其产物的形貌分别为超细纳米线、纳米棒(直径约几十纳米)和纳米颗粒(尺寸约50～100nm).通过调节反应过程中的表面活性剂,可以实现从线状钡的硫酸盐到纯相的超细钛酸钡纳米颗粒的转变.此方法为尺寸小于20nm的钛酸钡颗粒的制备及铁电材料尺寸限制效应的研究提供了重要参考.     

纳米TiO2薄膜的制备及其表面形貌AFM观测

采用溶胶-凝胶法在玻璃载波片及ITO导电玻璃片上制备出负载型纳米TiO2薄膜,并用原子力显微镜(AFM)对不同条件下制备的TiO2的表面形貌进行了表征.结果表明,TiO2薄膜能较好地负载在玻片表面,并且TiO2薄膜的表面形貌与前驱物的配比浓度、基片、热处理温度等都有密切的关系.随浓度和镀膜层数的增大,薄膜中TiO2纳米微晶的颗粒尺寸逐渐增大,从细小均匀粒子膜变为较大不规则的板块结构.在ITO薄膜面形成的TiO2薄膜具有较小的颗粒和均匀的分布.     

聚乙烯吡咯烷酮为稳定剂制备银纳米粒子及表征

以聚乙烯吡咯烷酮(PVP)为稳定剂,AgNO3为前驱物,乙醇为还原剂及溶剂,制备得到了银纳米粒子。采用紫外-可见吸收光谱及透射电子显微镜等方法对银纳米粒子的光学性质及形貌进行了表征。结果表明,以乙醇为溶剂,PVP可以对银纳米粒子的生长起到很好的表面修饰作用,银纳米粒子在400nm～410nm处产生明显的纳米银所具有的表面等离子态特征吸收峰,银纳米粒子的吸收强度随反应时间延长及前驱物浓度增加而提高。透射电子显微镜结果表明银纳米粒子具有球状形貌特征,尺寸分布窄。改变PVP与AgNO的投料比,可以得到不同尺寸的银纳米粒子。     

纳米Cu-Ni复合氧化物的制备及表征

通过溶胶-凝胶法制备了纳米Cu-Ni复合氧化物,利用DTA、XRD、TEM等方法对样品结构和性质进行了表征,研究了前驱体焙烧温度、原料浓度、搅拌速度和表面活性剂对粉体晶形和粒度的影响.结果表明,焙烧温度为350℃时能制得CuO-NiO复合物,其尺度为纳米结构;原料液浓度越低,搅拌速度越小,纳米粉体越易团聚;聚乙二醇表面活性剂对纳米粉体有良好的分散作用,颗粒较均匀.     

Superior bactericidal activity of SDS capped silver nanoparticles: Synthesis and characterization

Silver nanoparticles were synthesized through UV photo-reduction of silver nitrate aqueous solution, containing ethanol and sodium dodecyl sulfate (SDS) using an UV digester equipped with high pressure mercury lamp of 500 W. The synthesized nanoparticles were characterized by UV–vis spectroscopy (UV–vis), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The formation of silver nanoparticles was confirmed from the appearance of surface plasmon absorption maxima at 418 nm. TEM showed the spherical nanoparticles with size in 23–67 nm (average 45 ± 10 nm). The silver nanoparticles were stable for more than 8 months. The antibacterial activity of these SDS capped silver nanoparticles was tested using Pseudomonas aeruginosa as a model strain for gram-negative bacteria. SDS capped silver nanoparticles exhibit a much higher bactericidal activity compared to silver nanoparticles capped with other capping agents. Even at a low silver nanoparticle concentration of 5 μg/ml, complete inhibition of 10⁷ colony forming units (CFU) was achieved with SDS capped silver nanoparticles. This concentration is much lower than the values reported by other authors. This enhanced bactericidal activity is attributed to much efficient transport of silver nanoparticles by SDS to the outer membrane of cell wall compared to the other capping agents and have a better interaction of nanoparticles with the cell.     

纳米银粒子在微乳液中的制备及其抗菌性能

在以二丁酸二异辛酯磺酸钠为表面活性剂、异辛烷为油相形成的W／O型微乳体系中,以AgNO3为银源、抗坏血酸为还原剂,讨论了AgNO3浓度、抗坏血酸浓度以及水核半径（W）对制备纳米银粒子的影响。利用紫外一可见光谱分析（UV-Vis）、透射电镜（TEM）和纳米粒度仪对制得的纳米银进行表征。结果表明,在AgNO3浓度为0．2mol／L,抗坏血酸浓度为0．2mol／L,W值为10的条件下,得到大小为10nm左右,单分散性好的均匀球状纳米银溶胶。抗菌性能测试表明,当纳米银粒子质量浓度为10μg／mL时,对大肠杆菌的杀菌率达98％以上。     

树枝状与球状PbS纳米结构的组装合成及其形成机理研究

以醋酸铅为铅源,硫代乙酰胺为硫源,在表面活性剂SDS单独作用和表面活性剂SDS和CTAB共同作用下可选择性地组装合成出颗粒以相同晶面粘连组装成的单晶树枝状PbS纳米结构和颗粒以不相同晶面粘连组装成的多晶球状PbS纳米结构,而且提高反应物浓度能起到调节树枝状和球状PbS纳米结构尺寸的作用.对树枝状和球状PbS纳米结构的形成机理进行了初探,发现SDS单独作用时其烷基链起到的软模板作用有利于PbS小颗粒组装成树枝状的PbS纳米结构.当反应溶液中再加入适量的CTAB时,它在溶液中形成微胶束起到了软模板作用,迫使颗粒粘连组装成球状PbS纳米结构,有效地限制树枝状结构的生长.     

Fumed silica/polymer hybrid nanoparticles prepared by redox-initiated graft polymerization in emulsions

Hybrid particles comprising aggregated fumed silica nanoparticles as the core and hydrophobic polymers existing around the nanoparticles were prepared by ‘grafting from’ polymerization in emulsions. The emulsion polymerization employed cetyltrimethylammonium bromide (CTAB) as a cationic surfactant and sodium dodecyl sulfate (SDS) as an anionic surfactant, respectively, to stabilize the emulsion polymerization. The polymerization was initiated by the redox reaction between ceric ion Ce(IV) and the amine groups on the surfaces of aminated fumed silica nanoparticles that were modified by 3-aminopropyltriethoxysilane. Infrared spectroscopy and thermogravimetric analysis demonstrated that both poly(methyl methacrylate) (PMMA) and polystyrene (PS) were successfully grafted onto the fumed silica surface. The type of surfactant greatly affected the grafting ratio, monomer-to-polymer conversion, and morphology of the product. When CTAB was used as the surfactant, both the grafting ratio and monomer-to-polymer conversion were lower than when SDS was used, but transmission electron microscopy and light scattering analysis indicated that most of the resultant particles were sub-100 nm hybrid nanoparticles with a non-spherical shape and particles sizes of 75–90 and 57–85 nm for PMMA and PS-grafted fumed silica, respectively. Whereas, when SDS was used as the surfactant, the particles agglomerated to form large irregular clusters or even networks, possibly due to the electrostatic attractions between SDS and Ce(IV) and/or the aminated fumed silica nanoparticles in aqueous solution.     

稳定苯乙烯／丙烯酸丁酯细乳液的制备

以十二烷基硫酸钠（SDS）作乳化剂,不同链长的脂肪烃或肪醇作共乳化剂,分别用搅拌和超声乳化方法制备一系列苯乙烯（St)／丙烯酸丁酯（BA）细乳液,测定细乳液稳定性的结果表明,SDS／十六烷（HDE）的乳化效果最,HDE先与单体混合结合超声波制备的细乳液最稳定,乳化剂,共乳化剂的种类和浓度,乳化温度,超声时间等对细乳液的稳定性均有影响。     

Parameters controlling silver nanoparticle growth in sol-gel silica coatings

Silica based sol-gel coatings doped with different silver amounts have been prepared. Apart from silver concentration, other experimental parameters such as thermal densification conditions, presence of other co-dopants and the nature of the substrate have been varied in order to determine their influence on the final microstructure and properties. Characterisation of the materials prepared was carried out by optical spectroscopy (photoluminescence and absorption), secondary ion mass spectroscopy (SIMS) and transmission electron microscopy (TEM). The study was oriented to determine the parameters governing the nucleation and growth of silver nanoparticles. The results showed that formation of silver nanoparticles was promoted when one or more of the following conditions were achieved: silver concentration in the initial sol over 5%, thermal densification under reducing atmosphere and use of pure silica substrate (in general, glass substrates without modifier ions and, therefore, with few non-bridging oxygen positions).     

Enhancing foam drainage using foam fractionation column with spiral internal for separation of sodium dodecyl sulfate

A new type of foam fractionation column with spiral internal had been designed for enhancing the foam drainage and thus for the removal of minute hazardous materials. The column without spiral internal was served as the comparison column, and an anionic surfactant sodium dodecyl sulfate (SDS) was used as the foaming solution. Effects of liquid loading volume, initial SDS concentration and superficial gas velocity on enrichment ratio and recovery percentage of SDS were investigated. The experimental results showed that the spiral column successfully enhanced the enrichment ratio of SDS by reducing countercurrent resistance between the rising bubbles and the entrained liquid of reflux. Enrichment ratio of SDS obtained by using the spiral column was 15.7, which was 2.5 times of that obtained by using the comparison column under the suitable operating conditions of liquid loading volume 0.4 L, initial SDS concentration 0.2g/L and superficial gas velocity 1.7 mm/s.     

Synthesis of silver chromate nanoparticles: Parameter optimization using Taguchi design

The Taguchi method of experimental design is very well suited to improving the production process of synthetic nanoparticles. The current application of the Taguchi method was successful in optimizing the experimental parameters affect on synthesis procedure of silver chromate nanoparticles. Ultrafine silver chromate particles were synthesied by precipitation method using addition of silver ion solution to the chromate reagent. The effect of reaction conditions such as: silver and chromate concentrations, flow rate of reagent addition and temperature on the particle size of synthesized silver chromate particles were investigated. The effect of these factors on the diameter of silver chromate particles were quantitavely evaluated by the analysis of variance (ANOVA). The results showed that silver chromate particles can be synthesized by controlling silver concentration, flow rate and temperature. Finally, the optimum conditions for synthesis of silver chromate particles by this simple and fast method were proposed. The results of ANOVA showed that 0.001 mol/l silver ion concentration, 40 ml/min flow rate for addition of silver reagent to the chromate solution and 0°C temperature are optimum conditions for producing silver chromate particles with 100 ± 33 nm width. On the other hand, the Ag₂CrO₄ nano-superstructures were synthesized by electrosynthesis method. The results showed that Ag₂CrO₄ nanoparticles synthesized by this method have 75 nm average diameter.     

Morphological analysis of self-assembled SIS block copolymer matrices containing silver nanoparticles

The intrinsic ability of block copolymers to self-assemble at nanoordered level into different nanoscale structures has been used in this study to obtain nanocomposites. Ordered architectures of silver nanoparticles confined in a poly(styrene-b-isoprene-b-styrene) (SIS) block copolymer matrix have been generated. Both cetyl trimethylammonium chloride (TMAC) and dodecanethiol (DT) were used as surfactants to obtain dispersed nanocomposite films. Morphologies generated in Ag/SIS nanocomposites, detected through atomic force, resulted to be more dependent on the amount of silver nanoparticles than on the other variables chosen in the present study such as amount and type of surfactant and preparation parameters. The experimental observations are consistent with phase diagram predictions obtained for hybrid systems composed of block copolymers and nanoparticles.     

球形纳米银粒子制备新方法及其表征

采用水热法,不添加任何还原剂,在表面活性剂聚乙烯吡咯烷酮(polyvinyl pyrrolidone,PVP)的保护下,热分解碳酸银制得纳米银溶胶.将纳米银溶胶经过后续离心分离,干燥后得到纳米银粉.通过改变反应温度、反应时间、表面活性剂浓度、种类及反应物浓度等反应条件,分析了各反应条件对纳米银粒子形貌的影响.利用X射线衍射仪(X-ray diffraction,XRD)、扫描电子显微镜(scanning electron microscope,SEM)和电子能谱仪(energy dispersivespectroscopy,EDS)分析表明,在反应温度为180℃、反应时间为5 h、AgNO3浓度为0.1 mol/L、NaHCO3浓度为0.05mol/L、PVP为1.7 g的最佳制备工艺条件下,纳米银粒子为球形,粒径分布范围窄,单一分散,粒径40 nm左右.结果表明,表面分散剂PVP以及AgNO3与NaHCO3的浓度对球形纳米银的合成具有关键作用.