载银氧化锌复合纳米粒子的制备与表征

采用沉淀法制备了纳米氧化锌,并以它为前驱物,采用高温分解法对纳米氧化锌进行了裁银改性处理,制备了栽银氧化锌复合纳米粒子,考察了载银前后纳米粒子的粒径与结构。研究发现,采用沉淀法制备的纳米氧化锌尺寸较为均匀,粒径约为170nm,分散性也较好;载银后的复合纳米粒子粒径略有增加,这来源于银在纳米氧化锌粒子外的成功包覆。     

高分散、均混合Al2O3-SiC-ZrO2(3Y)水悬浮液

用微波法制备纳米水合二氧化锆, 通过包覆工艺, 将Y(OH)3均匀地包覆在水合二氧化锆粒子表面, 制备出ZO2(3Y)的先驱体. 然后用聚甲基丙烯酸铵(PMAA-NH4)对α-Al2O3、纳米SiC及包覆水合二氧化锆表面改性. 使三种单相水悬浮液在pH=9.0时, 粒子表面电性相同, 且有良好分散状态. 从而制备出高分散、均混合Al2O3-SiC-ZrO2(3Y)先驱体水悬浮液.     

荧光介孔二氧化硅纳米粒子的制备及其性能探究

利用单层十六烷基三甲基溴化铵(CTAB)表面活性剂包覆染料并将其转相到水中,通过溶胶-凝胶法制备以荧光染料为核、介孔二氧化硅纳米粒子(MSNs)为壳的荧光介孔二氧化硅纳米粒子。利用DLS探讨了正硅酸乙酯、表面活性剂、氨水、染料浓度对粒子粒径的影响,利用SEM、TEM、TG、UV、PL光谱分析手段对复合纳米粒子结构、形貌、热稳定性、光谱进行了表征和探讨。结果表明,随着正硅酸乙酯和氨水用量增多,粒子粒径增加;表面活性剂用量较少时粒径会较大;染料浓度较低时对粒径影响较小;制备出的粉体可以在100nm左右可控;荧光强度提高、染料与二氧化硅最佳掺杂质量比为1.5×10-3;由于是物理包覆所以热稳定性提高有限,但抗紫外耐老化性有显著的提高。     

银/聚苯胺纳米复合材料的制备及电化学性能

采用苯胺为分散剂合成纳米银胶溶液,并在此基础上引发苯胺的原位复合,制备出银/聚苯胺(Ag/PANI)纳米复合材料。通过傅里叶变换红外光谱仪、X射线衍射分析仪、扫描电镜、透射电镜和电化学分析仪对产物进行了分析与检测。研究结果表明,Ag/PANI纳米复合材料中形成了聚苯胺在外、银纳米粒子在内的包覆结构,纳米复合粒子为类球形状形貌。引入纳米银粒子后,制备的Ag/PANI纳米复合材料的电化学活性和比容量较PANI有了很大提高。Ag/PANI纳米复合材料的腐蚀电流密度为72.1μA/cm2,比PANI的腐蚀电流密度106μA/cm2降低了33.9μA/cm2,纳米复合材料防腐性能得到显著提高。     

纳米碳酸钙表面原位聚合包覆

通过超重力场制备了纳米碳酸钙,对纳米碳酸钙进行超声波分散,然后进行原位乳液聚合,采用分步聚合的方式,在纳米碳酸钙表面包覆了丙烯酸酯类共聚物,制得了纳米碳酸钙表面原位聚合包覆产物.采用TEM、DSC、TGA和表面电子能谱(ESCA)对纳米碳酸钙表面原位聚合包覆产物进行了表征.结果表明:制备的纳米碳酸钙粒子粒径在20nm左右,通过原位乳液聚合包覆后,粒径在40～80nm,包覆后的纳米碳酸钙复合粒子表面几乎不含Ca元素,表明纳米碳酸钙被良好包覆,并形成了以纳米碳酸钙为核、PBA为中间层、MMA和EA,St共聚物为壳的三层结构有机-无机纳米复合粒子.     

功能化CdS纳米晶的制备

以氯化镉和硫化钠为原料,2-巯基乙醇(ME)为有机配体,成功制备了粒径可控的、表面富有羟基的CdS纳米晶.采用不同的ME/Cd2 及H2O/DMF比例以观察有机配体及溶剂对生成粒子尺寸的影响.透射电子显微图证实了球形CdS纳米粒子很好地分散在H2O/DMF溶液中,没有任何团聚现象发生.傅立叶变换红外谱图(FT-IR)显示了羟基基团成功地包覆在纳米晶的表面.X线衍射(XRD)测试揭示了功能化CdS纳米晶的晶形主要为立方晶.     

基于超分子结构的光电子材料的制备与表征(英文)

为实现短波长光存储材料,提出一种基于金属纳米粒子与染料共掺杂的复合材料制备新方法.采用透射电子显微镜(TEM)、紫外-可见吸收光谱(UV-Vis)以及傅立叶变换红外光谱(FT-IR)对所制备的复合薄膜进行表征.实验发现,与未掺杂银的薄膜相比,掺杂银的复合薄膜中甲基橙的吸收蓝移了6nm.提出并利用超分子结构模型分析了该吸收蓝移的机理.研究结果显示,本研究所提出的这种新的材料制备方法具有制备吸收波长在400～500nm,且可望与GaN激光器在光存储技术中匹配的能力.     

有机表面修饰温度对纳米二氧化钛微结构的影响

首先制备出纳米二氧化钛水分散液, 然后通过蒸馏的方法, 把纳米二氧化钛粒子由水分散液转移到溶有硬脂酸的甲苯溶液中, 以确保纳米二氧化钛在有机相中进行表面修饰. 然后升温到不同的温度, 利用硬脂酸对纳米二氧化钛进行有机表面修饰, 研究了有机表面修饰温度对纳米二氧化钛微结构的影响. 采用红外光谱(FT IR)、X 射线光电子能谱（XPS）、热分析(TG DTG)、X 射线粉末衍射（XRD）和透射电镜(TEM)等对有机表面修饰前后的纳米二氧化钛进行分析表征. 结果表明, 硬脂酸与纳米二氧化钛表面之间存在双齿配位方式的化学键作用, 硬脂酸在纳米二氧化钛表面形成了均匀的单分子化学修饰层. 随着表面修饰温度的升高, 纳米二氧化钛的晶粒逐渐长大, 硬脂酸在纳米二氧化钛表面的化学包覆量逐渐下降, 硬脂酸分子间排列更加紧密, 硬脂酸包覆层由1nm变为2～3nm. 表面修饰温度对硬脂酸与纳米二氧化钛表面的结合方式影响不大.     

轻质高导电镀银复合粒子的制备研究

采用分散聚合工艺,以聚乙烯吡咯烷酮为分散剂,偶氟二异丁腈为引发剂,无水乙醇为分散介质,制备出粒径2.0μm、表面光滑、分散均匀的聚苯乙烯微球.将其进行表面磺化处理后运用化学镀工艺制备出了具有轻质高导电特性的聚苯乙烯/银复合粒子.对所制备的复合粒子进行了扫描电镜、红外光谱以及体积电阻率的测试.结果表明:所制备的复合粒子包覆均匀、导电性能良好;表面修饰提高了PS微球表面的电负性和亲水性并引入了磺酸基团,对PS微球表面镀银起到了重要作用;另外,随着PdCl2浓度和AgNO3/PS质量比的增加,复合粒子包覆完整性和导电性能都随之增加,最佳体积电阻率为1.61×10 -4Ω·cm.     

纳米纤维素/银纳米粒子的制备和表征

以纳米纤维素(NCC)为分散剂,硼氢化钠为还原剂还原硝酸银,化学还原法制备纳米纤维素/银纳米粒子。m(Ag)/m(NCC)=5%制备的纳米纤维素/银纳米粒子,X射线衍射分析结果表明,纳米纤维素/银纳米粒子中NCC和银纳米粒子相互混合并未改变各自的晶型,纳米纤维素/银纳米粒子中银纳米粒子的晶粒尺寸为11.87nm,与透射电子显微镜(TEM)所测银纳米粒子直径(10nm)相近;热重分析结果表明,纳米纤维素/银纳米粒子的热稳定性较纳米纤维素稍有下降。透射电子显微镜(TEM)分析、紫外光谱分析、固含量分析、机理分析和抑菌活性分析结果表明,m(Ag)/m(NCC)=3%时制备的纳米纤维素/银纳米粒子对大肠杆菌和金黄色葡萄球菌均有抑制作用,且银纳米粒子在纳米纤维素/银纳米粒子中分散较均匀。     

Gold/palladium and silver/palladium colloids as novel metallic substrates for surface-enhanced Raman scattering

New surface-enhanced Raman scattering (SERS) substrates, composed of gold or silver colloidal nanoparticles doped with palladium, were prepared. These novel colloids are stable and maintain a satisfactory SERS efficiency, even after long aging. The interest in doping the coinage metal nanoparticles with palladium is due to the well-known catalytic activity of this metal. Transmission electron microscopy (TEM) and ultraviolet-visible absorption spectroscopy were used to characterize the shape and size of the metal particles. It was found that these bimetallic colloidal nanoparticles have a core-shell structure, with gold or silver coated with palladium clusters.     

玻璃基TiO_2-Fe_2O_3-CeO_2复合纳米薄膜的光催化性能研究

在溶胶-凝胶法制备的TiO2胶膜表面涂覆金属离子,通过焙烧制备TiO2-Fe2O3-CeO2复合纳米薄膜。以甲基橙为目标降解物,讨论过渡金属离子Fe3+和稀土金属离子Ce3+的掺杂对TiO2薄膜光催化活性的影响。采用SEM、XRD、EDS等表征手段对复合氧化物薄膜进行表征。结果表明:所制备的薄膜具有纳米结构;Fe3+、Ce3+单掺和Fe3+/Ce3+共掺均可提高TiO2薄膜的光催化性能,但相同条件下共掺离子的光催化活性更高。     

Tuned optical properties of in-situ synthesized m-nitroaniline doped Ag/PVA nano-composites

Meta-nitroaniline (m-NA) doped silver/poly(vinylalcohol) (Ag/PVA) nanocomposites are prepared via in-situ reduction of silver salt by employing hydrazine hydrate (HH) in order to study the effect of the NLO active m-NA on the optical properties of nanoparticles of silver in the colloidal as well as self supported film form. Reduction of silver salt in aqueous alcoholic PVA with HH is done first followed by doping of the reaction mixture with m-NA. The UV-Visible absorption spectra show peak at about 400 nm for Ag nanoparticles due to surface plasmon resonance phenomenon, which gets blue shifted with the change in m-NA concentration. The Second Harmonic Generation (SHG) studies show improvement in intensity with increasing m-NA concentration up to a saturation point (approximately 2.52 wt% with respect to PVA). Further increase in m-NA concentration leads to decrease in SHG intensity. The solutions and the films are characterized by photoluminescence (PL), FTIR spectroscopy, XRD, SEM, TEM, and thermal analysis. m-NA doped composites showed better PL efficiency. SEM of the nanocomposite film shows uniform distribution of particles within the film. The particle size as shown by TEM is found to be less than 10 nm.     

Photocatalytic degradation of methyl red dye by silica nanoparticles

Silica nanoparticles (SiO2 NPs) were found to be photocatalytically active for degradation of methyl red dye (MR). The SiO2 NPs and SiO2 NPs doped with silver (and or) gold nanoparticles were prepared. From the transmission electron microscopy (TEM) images the particle size and particle morphology of catalysts were monitored. Moreover, SiO2 NPs doped with silver and gold ions were used as a photocatalyst for degradation of MR. The rate of photocatalytic degradation of MR was found to be increased in the order of SiO2 NPs, SiO2 NPs coated with gold nanoparticles (Au NPs) and silver nanoparticles (Ag NPs), SiO2 NPs coated with Ag NPs, SiO2 NPs coated with Au NPs, Ag+-doped SiO2 NPs, and Au3+-doped SiO2 NPs. The kinetic and mechanism of photocatalytic reaction were studied and accorded well with experimental results.     

Characterization of SiO2/Ag composite particles synthesized by in situ reduction and its application in electrically conductive adhesives

In the study, SiO₂/Ag composite particles with silver coating onto the surface of silica have been successfully prepared via a novel and facile approach (Oxidation–Reduction Method). In this approach, the SiO₂ particles were first modified with 3-ammoniatriethoxysilane (APTES) and glyoxalic acid (GA) through two-step reaction, the aldehyde group (CHO) were anchored onto the surfaces of silica spheres via electrostatic attraction, these [Ag(TEA)₂]⁺ ions in the solution were then reduced by the CHO and coated onto the surface of silica to obtain SiO₂/Ag composite particles. The effects of the reaction conditions on silver content and synthetic mechanism had also been discussed. The structure, morphology and optical properties of the SiO₂/Ag composite particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV–vis spectroscopy. The results showed the surface of SiO₂ was surrounded by pure silver nanoparticles, and the silver nanoparticles had face-centered-cubic structure, the SiO₂/Ag composite particles with core–shell morphology and special optical properties. And the small content SiO₂/Ag composite particles applied in electrically conductive adhesives (ECAs) improved the electrical bulk resistivity and tensile shear strength.     

天然石墨-纳米银/聚氨酯导电复合薄膜的制备及性能

采用热处理还原银盐原位引入银粒子的方法, 成功制备了天然石墨-纳米银/聚氨酯(C-Ag/PU)导电复合薄膜。并通过透射电镜(TEM)、 扫描电镜(SEM)观察了该复合薄膜的微观结构, 用X射线衍射仪(XRD)跟踪了银的还原和银粒子的生长过程, 探讨了加热温度和加热时间对银还原过程的影响, 研究了纳米银的生成和聚集对C/PU复合体系导电性能的影响。结果表明, 随着热处理的进行, 银粒子不断地生成和聚集, 最终以纳米尺寸(约10nm)均匀分散在聚合物基体中。纳米银粒子在天然石墨粒子之间起到了桥梁的作用, 改善了复合体系的导电通路, 显著提高了复合体系的导电性。      

Microstructures and Photocatalytic Properties of S Doped Nanocrystalline TiO2 Films

The nanocrystalline S doped titanium dioxide films were successfully prepared by the improved sol-gel process. Here TiO(C₄H₉O)₄ and CS(NH₂)₂ were used as precursors of titania and sulfur, respectively. The as-prepared specimens were characterized using x-ray diffraction (XRD), x-ray energy dispersive spectroscopy (EDS), high-resolution field emission scanning electron microscopy (FE-SEM), Brunauer-Emmett-Teller (BET) surface area, and ultraviolet-visible diffuse reflectance spectroscopy. The photocatalytic activities of the films were evaluated by degradation of organic dyes in aqueous solution. The results of XRD, FE-SEM, and BET analyses indicated that the TiO₂ films were composed of nanoparticles. S doping could obviously not only suppress the formation of brookite phase but also inhibit the transformation of anatase to rutile at high temperature. Compared with pure TiO₂ film, S doped TiO₂ film exhibited excellent photocatalytic activity. It is believed that the surface microstructure of the modified films is responsible for improving the photocatalytic activity.     

Layer-by-layer deposition of green synthesised silver nanoparticles on polyester air filters and its antimicrobial activity

Silver nanoparticles stabilised with anionic polymeric polyelectrolytes were successfully synthesised by high-energy UV reduction. Three types of polyelectrolytes were used including poly(methacrylic acid) (PMA), poly(acrylic acid) (PAA) and poly(4-styrenesulphonic acid-co-maleic acid) (CoPSS). The formation of the prepared solutions exhibited surface plasmon resonance at the wavelength of 475, 730 and 408 nm by using PMA, PAA and CoPSS as the stabilising agents. UV–visible spectrophotometer, transmission electron microscope (TEM) and zeta potential analyser were employed to characterise the formation of the prepared solutions. The silver nanoparticles stabilised with anionic polyelectrolytes were immobilised on polyester air filters using a layer-by-layer technique. This is the sequential dipping of polyester air filters in a dilute solution of cationic poly(diallyldimethylammonium chloride) and anionic polymeric polyelectrolytes capped silver. The surface topography of the polyester air filters were measured by field emission scanning electron microscope. Results showed that silver nanoparticles had the highest surface coverage on the polyester air filters probably because it is a good bonding candidate and insures strong film growth. The multilayers polyester air filters coated silver nanoparticles were tested against the gram positive pathogen Staphylococcus aureus. The deposition of silver nanoparticles onto the polyester air filters resulted in 92.18%, 84.32% and 71.19% of bacteria removal using PMA, PAA and CoPSS as the stabilising agent.     

Layer-by-layer assembly of polyelectrolyte/TiO2 thin films with reflection-enhancing function

Colloidal TiO₂ was prepared by hydrolyzing tetra-n-butyl titanate. Composite multilayer films of poly(sodium 4-styrenesulfonate) (PSS) and colloidal TiO₂ particles were layer-by-layer assembled onto optic fibers and microscope glass slides. As the PSS/TiO₂ film was deposited onto the end face of a glass fiber, the reflected optic intensity periodically oscillated as the bilayer number of the film increased. After a 24-bilayer film was coated onto the both sides of a glass slide, the transmittance at 850 nm decreased more than 20%, which means that the film could serve the function as a reflection-enhancing coating. X-ray diffraction analysis and data of TEM electron diffraction analysis show that the colloidal TiO₂ particles are mainly brookite nanocrystals and that the PSS/TiO₂ films are polycrystalline films. Scratching experiments indicate that the composite films are of relatively high hardness.     

Synthesis and layer-by-layer self-assembly of silver nanoparticles capped by mercaptosulfonic acid

Spherical silver nanoparticles capped by mercaptosulfonic acid with a diameter of about 8 nm were prepared by a simple chemical reaction. The resulting silver nanoparticles were characterized by UV–vis spectroscopy (UV–vis) and transmission electron microscopy (TEM). Using layer-by-layer (LBL) self-assembly technique, the multilayer films containing silver nanoparticles and polycation poly(dialyldimethylammonium chloride) (PDDA) were successfully fabricated. The fabrication process was monitored by UV–vis spectra and the morphology of the multilayer films was investigated by atomic force microscopy (AFM). The cyclic voltammogram (CV) measurements further confirmed that the silver nanoparticles had assembled into the multilayer films successfully. Surface-enhanced Raman spectroscopy (SERS) measurements showed that the multilayer films containing silver nanoparticles could serve as SERS-active substrate.