纳米银胶的光化学制备及其特性研究

采用紫外光化学法制备了黄色银胶,并研究了硝酸银和柠檬酸三钠的浓度对制备的银胶吸收光谱的影响,发现随着硝酸银浓度的增加银胶的吸收峰先兰移然后红移;当柠檬酸三钠的浓度增加时,硝酸银吸收峰的位置几乎不变,而吸收峰强度增大.最后通过透射电镜成像研究其尺寸,发现其尺寸分布在5~20 nm之间.     

基于荧光光谱技术的大肠杆菌活性及灭菌效应研究

在食品和环境监测中,大肠杆菌是一个重要指标细菌,因此,对大肠杆菌的监测和灭菌效果也引起了人们广泛的关注。基于荧光光谱检测技术具有的灵敏度高、速度快、稳定性强等优点,利用荧光光谱技术研究了大肠杆菌的发射峰强度与大肠杆菌浓度的内在变化规律,得到了一种更加方便、快捷、监测浓度更低的大肠杆菌计数方法。采用289 nm的激发光照射大肠杆菌水溶液,得到大肠杆菌的荧光发射光谱;改变大肠杆菌溶液的浓度,得到不同浓度大肠杆菌溶液的荧光光谱,并分析大肠杆菌特征峰强度与大肠杆菌浓度的关系。在此基础上,利用荧光光谱技术研究了银纳米颗粒对大肠杆菌荧光发射的影响,分析了银纳米颗粒对大肠杆菌的灭菌效果,结果表明：(1)当289 nm的激发光照射大肠杆菌水溶液时,大肠杆菌分别在332和425 nm两处有明显的荧光特征峰;荧光特征峰强度随着大肠杆菌浓度降低而降低;当大肠杆菌浓度小于20%时,332和425 nm处特征峰强度与大肠杆菌溶液的浓度均呈线性关系。(2)当大肠杆菌水溶液中加入银纳米颗粒时,在4个小时内,银纳米颗粒的作用时间越长,大肠杆菌的荧光特征峰越弱,即灭菌率越高;增加银纳米颗粒的浓度或者提高环境温度,均可提高银纳米颗粒对大肠杆菌的灭菌率。本文的研究结果对食品、环境等中大肠杆菌的计数和灭菌研究有参考意义。     

银纳米膜的电化学制备方法及性能表征

采用电沉积方法在表面活性剂与电解液的界面上制备了银纳米膜。通过对甲磺酸银体系和硝酸银体系中纳米银膜的电沉积速率及纳米银膜颗粒进行比较发现，相同条件下硝酸银体系得到的纳米膜晶粒粒径比较小，膜的生长速率较快。选定硝酸银体系为电沉积体系。考察了槽压、电解液的浓度和温度及溶液的pH值对制备银纳米膜的影响，确立了制备银纳米膜的最佳工艺条件为硝酸银浓度5mmol/L，槽压4V，pH3.0,硬脂酸的质量浓度0.2g/L。实验表明，最佳工艺条件下制备的银纳米膜晶粒粒径均匀，平均粒径在20nm左右，近似球形。本方法制备的银纳米膜将在非线性光学材料方面得到应用。     

聚合物表面银纳米颗粒的大面积均匀沉积及其应用

通过化学浸润和光还原法在聚合物薄膜基片（三醋酸纤维树酯）上直接沉积制备出大面积范围内颗粒大小、表面密度等分布均匀的纳米金属银颗粒.紫外吸收光谱和高分辨透射电镜分析表明，在室温实验条件下调整化学溶液浓度，可获得颗粒直径在2—5nm范围内的球形金属纳米银颗粒.通过接触拷贝方式，获得了基于银纳米颗粒形成的全息光栅. 关键词： 银纳米颗粒 聚合物薄膜 浸润 光还原     

Co:BaTiO3/Si(100)纳米复合薄膜制备、微结构及其紫外光电子能谱研究

采用脉冲激光气相沉积(PLD)方法,在Si(100)晶面上制备了Co:BaTiO3纳米复合薄膜.采用X射线衍射(XRD)结合透射电镜(TEM)方法研究了两种厚度Co:BaTiO3纳米复合薄膜的晶体结构,当薄膜厚度约为30 nm时,薄膜为单一择优取向;当薄膜厚度约为100 nm时,薄膜呈多晶结构.原子力显微镜(AFM)分析表明,当膜厚为30 nm时,薄膜呈现明显的方形晶粒.采用紫外光电子能谱(UPS)研究了Co的价态和Co:BaTiO3纳米复合薄膜的价带谱.研究表明:当Co浓度很高时其态密度(DOS)与晶体BaTiO3明显不同.此外,嵌埋纳米Co颗粒的BaTiO3薄膜的能带结构可用纳米颗粒的浓度来调制,从而也可对其光学和电学性质进行改性.     

石墨烯/银纳米复合材料的制备及其影响因素研究

以硝酸银、鳞片石墨为原料, 在强碱环境下, 制备得到石墨烯/银纳米复合材料, 采用X射线衍射、红外吸收光谱、透射电子显微镜、紫外可见分光光度计对所制备的石墨 烯/银纳米复合材料进行了表征.结果表明: 氧化石墨烯和银离子在强碱NaOH的作用下, 氧化石墨烯失去部分含氧官能团, 被部分还原为石墨烯(rGO), 银离子被还原为纳米银颗粒, 均匀分布在氧化石墨烯片层表面, 颗粒大小和分布受硝酸银用量、反应温度、NaOH的加入顺序及前驱物混合方式等因素影响, 在GO与Ag粒子质量比为 1:1.08时, 负载在石墨烯片层上的银纳米颗粒集中在12 nm左右. 关键词： 石墨烯/银纳米复合材料 强碱溶液     

基于多形貌银纳米颗粒的多波长相干随机激光研究

采用溶剂热法分别制备了球形银纳米颗粒和多形貌银纳米颗粒,其中球形银纳米颗粒具有400 nm的窄带等离激元共振峰,而多形貌银纳米颗粒的共振区间在400～700 nm之间,将它们分别掺入R6G与PVP的混合溶液中,利用旋涂法在玻璃基板上制备银纳米颗粒嵌入染料掺杂聚合物薄膜随机激光器。采用纳秒脉冲激光进行随机激光泵浦实验,实验结果表明球形银纳米颗粒染料掺杂聚合物薄膜只有自发辐射峰,而多形貌银纳米颗粒染料掺杂聚合物薄膜具有线宽<0.8 nm的相干随机激光发射光谱,其阈值为1.9 mJ·cm-2, 这可能是由于银纳米颗粒的等离激元共振区间与R6G的发射光谱重叠,支持局域等离激元效应的形成,明显的局域场增强有效地改善了与附近分子的相互作用,从而激发了更多的辐射光子,促进了高增益的形成。进一步,利用多形貌银纳米颗粒在银纳米颗粒染料掺杂聚合物薄膜中随机分布的特性,通过改变泵浦位置,实现了20 nm范围内的随机激光输出波长的调控,具体输出范围为590.1～610.4 nm。认为这是由于多形貌银纳米颗粒在不同位置的组成和分布不同,改变了表面等离激元的相互作用和光子的散射能力,从而形成不同的增益效应和不同的封闭光振荡路径。此外,考虑到多形貌银纳米颗粒的共振波长较宽,探究了其用于输出其他颜色光的可能性。以与上述银纳米颗粒R6G染料掺杂聚合物薄膜相似的制备方法,制备了多形貌银纳米颗粒掺杂DCJTB染料聚合物薄膜,并且进行随机激光泵浦实验。结果表明,可以有效的产生波长为675 nm,半高宽<0.8 nm的相干红光随机激光,并且阈值仅为0.98 mJ·cm-2。研究结果在宽带可调谐随机激光器研究以及多色随机激光器研究领域具有重要的参考价值。     

单分散银纳米颗粒的超声辅助制备及表面拉曼与荧光增强效应

以硝酸银和甲硼烷叔丁胺络合物分别为反应前驱物和还原剂,在油胺油酸体系中,利用超声辅助方法在室温下制备出粒径为3.4 nm的单分散银纳米颗粒．通过XRD、TEM和EDX对产物进行表征,结果显示产物具有典型的面心立方结构,单分散特征明显、尺寸分布均匀,且最可几尺寸为3.4 nm．超声反应时间、油胺和油酸的用量及其比例对银纳米晶的形貌和尺寸有重要影响,其中油胺溶剂的使用是控制单分散银纳米晶尺寸的关键．同时,研究显示单分散银纳米颗粒对罗丹明6G模型分子具有很强的拉曼增强效应;双光子荧光照片显示其具有很好的荧光增强效应．     

绿色合成银纳米粒子及其在SERS中的应用

采用无毒、绿色的酪氨酸作为还原剂和稳定剂,在碱性条件下还原硝酸银,经60 ℃恒温水浴处理20 min,成功地合成了银纳米粒子。混合溶液颜色由淡黄色变为棕黄色直观地呈现了银纳米粒子的生成。利用紫外可见吸收光谱(UV-Vis)和透射电子显微镜(TEM)对制备样品进行分析和表征。粒子的UV-Vis吸收在412 nm附近。TEM图像显示,银纳米粒子的形状近似球形,粒子直径在15～25 nm。分别以结晶紫(CV)和叶酸(FA)为探测分子,进一步研究了该银纳米粒子的表面增强拉曼散射(SERS)效应。实验结果表明,该合成方法不仅方便、快速、绿色环保,而且合成的银纳米粒子对CV和FA分子有很好的SERS效应。     

金纳米颗粒阵列基底的化学置换制备及其表面增强拉曼散射特性研究

表面增强拉曼(SERS)作为一种分析手段,具有高灵敏度、高选择性、高重复性、非破坏性等优点,在过去的几十年中,被广泛应用在成分检测、环境科学、生物医药及传感器等领域。其中以金、银等贵金属纳米颗粒薄膜在表面增强拉曼(SERS)活性基底方面得到了更为广泛的应用。SERS技术一个关键的因素是如何制设计并备具有大面积、高增强能力及高重复性、可循环使用的SERS基底。通常,贵金属纳米颗粒规则阵列结构的单元颗粒电磁增强特性及其颗粒间的电磁耦合增强特性的综合作用可大力提升SERS基底的探测性能。然而,利用传统微纳米加工方法如光刻、电子束光刻等方法制备得到的贵金属纳米阵列结构的表面粗糙度不够理想。结合光刻与化学置换方法制备金纳米颗粒四方点阵列孔洞结构,并研究其作为SERS基底的电磁增强特性。具体研究利用光刻法在硅衬底上制备了规则排列的四方点阵列孔洞结构,用磁控溅射在其表面镀上金属铁膜;接着在衬底上旋涂浓度为1.893 8 mol·L-1的氯金酸液膜,在孔洞内铁和氯金酸发生置换反应,进而孔洞生成金纳米颗粒,最终得到金纳米颗粒四方点阵SERS活性基底。采用罗丹明6G(R6G)分子作为探测分子测试不同金纳米颗粒阵列结构基底的SERS谱。实验结果表明,随着化学置换反应时间的延长,金纳米颗粒排列更加紧凑有序,SERS谱增强性能更好。     

Synthesis and characterization of radiation crosslinked nano silver- polyvinyl alcohol/polyethylene oxide composites

Poly (vinyl alcohol)/poly (ethylene oxide) (PEO/PVA) blends were modified by gamma irradiation in the presence of acrylic acid (AAc) monomer. The modified PVA/PEO blends were then complexed with silver nitrate salt and lithium trifluoromethanesulfonate. Transmission electron microscopy was used to determine the distribution as well as the particle size of the silver nanoparticles (NP) formed in the matrix. The UV–vis absorbance spectra of the prepared grafted nanocomposite membranes confirmed the formation of Ag NP based on their surface plasmon band at 438?nm. The electrical properties of the blended electrolyte polymer films were characterized and discussed.     

Laser sintering of silver nanoparticle thin films: microstructure and optical properties

We present a method for the sintering of silver (Ag) nanoparticle thin films by millisecond pulsed laser irradiation. The microstructure of sintered thin films and sintering behaviors of nanoparticles were systematically investigated in this paper. Absorption spectra of sintered thin films showed blue-shifted surface plasmon resonances (SPR) from 500 nm to 480 nm and red-shifted from 480 nm to 550 nm when laser power was varied from 100 W to 140 W and from 140 W to 200 W, respectively. This indicates a new technique to control light absorption through joining nanoparticles with laser sintering. According to theoretical calculations based on a heat diffusion model, the melting temperature of these Ag nanoparticles was estimated to be 440 °C during laser irradiation.     

Efficient fabrication of transparent antimicrobial poly(vinyl alcohol) thin films

We have explored in situ synthesis of Ag nanoparticles in transparent PVA films in view of increasing areas of application of those films. The two-step procedure consists of ion incorporation in the matrix and subsequent thermal reduction. Smooth and transparent PVA films containing Ag nanoparticles of 5–20 nm were fabricated by this approach. The optical property of the films and the size of metal nanoparticles could be controlled by changing the reaction conditions. By increasing heating temperature, the absorbance and wavelength of surface plasmon resonance (SPR) of the composite film increased, and nanoparticles with larger particle sizes and broader size distributions were obtained. In the temperature range of 130–170 °C, the wavelength of SPR increased with increasing the AgNO₃ concentration. At 190 °C, however, the wavelenght of SPR blue-shifted initially when the AgNO₃ concentration increased from 10 to 80 mmol/L, and red-shifted thereafter. The composite films showed excellent antimicrobial performance toward bacteria such as Escherchia coli. Such hybrids afford very effective and environment-friendly antimicrobial surface coatings.     

Structural,thermal and optical behavior of laser irradiation-induced PVA–PEG–Ag nanocomposites

Polyvinyl alcohol?polyethylene glycol?silver (PVA–PEG–Ag) nanocomposites were prepared by adding Ag nanoparticles with 5?wt.% to the (PVA–PEG) blend. The films of 0.05?mm thickness were prepared by the casting method. Samples from these films were irradiated with infrared (IR) laser fluences ranging from 1.7 to 15?J/cm². The effect of IR laser radiation on the structural properties of PVA–PEG–Ag has been investigated using X-ray diffraction and Fourier transform infrared spectroscopy. The results indicate that the crosslinking dominates due to laser exposure at the fluence range 1.7–15?J/cm², reducing the ordering character of the nanocomposite samples. Also, the variation of transition temperatures with the laser fluence has been determined using differential thermal analysis. The nanocomposite thermograms were characterized by the appearance of an endothermic peak due to melting, and were found to be dependent on the laser fluence. In addition, the color changes due to laser irradiation were computed using the transmission data. It is found that the color difference is largely dependent on the proportions of the red color component.     

The effect of the deposition parameters on size, distribution and antimicrobial properties of photoinduced silver nanoparticles on titania coatings

Controlled photodeposition of silver nanoparticles (AgNP) on titania coatings using two different sources of UV light is described. Titania (anatase) thin films were prepared by the sol-gel dip-coating method on silicon wafers. AgNPs were grown on the titania surface as a result of UV illumination of titania films immersed in aqueous solutions of silver nitrate. UV xenon lamp or excimer laser, both operating at the wavelength 351 ± 5 nm, was used as illumination sources. The AFM topography of AgNP/TiO₂ nanocomposites revealed that silver nanoparticles could be synthesized by both sources of illumination, however the photocatalysis carried out by UV light from xenon lamp illumination leads to larger AgNP than those synthesized using the laser beam. It was found that the increasing concentration of silver ions in the initial solution increases the number of Ag nanoparticles on the titania surface, while longer time of irradiation results the growth of larger size nanoparticles. Antibacterial tests performed on TiO₂ covered by Ag nanoparticles revealed that increasing density of nanoparticles enhances the inhibition of bacterial growth. It was also found that antibacterial activity drops by only 10-15% after 6 cycles compared to the initial use.     

Thin films of silver nanoparticles deposited in vacuum by pulsed laser ablation using a YAG:Nd laser

We report the deposition of thin films of silver (Ag) nanoparticles by pulsed laser ablation in vacuum using the third line (355 nm) of a YAG:Nd laser. The nanostructure and/or morphology of the films was investigated as a function of the number of ablation pulses, by means of transmission electron microscopy and atomic force microscopy. Our results show that films deposited with a small number of ablation pulses (500 or less), are not continuous, but formed of isolated nearly spherical Ag nanoparticles with diameters in the range from 1 nm to 8 nm. The effect of increasing the number of pulses by one order of magnitude (5000) is to increase the mean diameter of the globular nanoparticles and also the Ag areal density. Further increase of the number of pulses, up to 10,000, produces the formation of larger and anisotropic nanoparticles, and for 15,000 pulses, quasi-percolated Ag films are obtained. The presence of Ag nanoparticles in the films was also evidenced from the appearance of a strong optical absorption band associated with surface plasmon resonance. This band was widened and its peak shifted from 425 nm to 700 nm as the number of laser pulses was increased from 500 to 15,000.     

激光辐照对热退火金属/掺氟二氧化锡透明导电薄膜光电性能的影响

采用532 nm纳秒脉冲激光对热退火的铝(Al)/掺氟二氧化锡(FTO)、铜(Cu)/FTO和银(Ag)/FTO三种双层复合薄膜表面分别进行处理, 结果显示薄膜样品的光电性能都得到提高.其中, 热退火Ag/FTO薄膜的平均透光率(400–800 nm)增幅最大, 从72.6%提高到80.5%, 主要是由于其表面产生了具有减反增透作用的光栅结构.激光辐照后热退火Ag/FTO薄膜的导电性也略有提高, 其方块电阻从5.6 Ω/sq下降到5.3 Ω/sq, 原因主要是激光辐照的热效应造成的退火作用使薄膜的晶粒尺寸增大, 减少了晶界散射而使载流子迁移率提高.计算结果显示, 激光辐照后热退火Ag/FTO薄膜的品质因子从0.73×10^-2Ω^-1增大为2.16×10^-2Ω^-1, 表明其综合光电性能得到显著提高.激光辐照可同步实现薄膜表面光栅结构的制备和附加退火作用, 这为金属层复合透明导电薄膜光电性能的综合优化提供了新的思路.     

Highly Luminescent Material Based on Alq3:Ag Nanoparticles

Tris (8-hydroxyquinoline) aluminum (Alq₃) is an organic semiconductor molecule, widely used as an electron transport layer, light emitting layer in organic light-emitting diodes and a host for fluorescent and phosphorescent dyes. In this work thin films of pure and silver (Ag), cupper (Cu), terbium (Tb) doped Alq₃ nanoparticles were synthesized using the physical vapor condensation method. They were fabricated on glass substrates and characterized by X-ray diffraction, scanning electron microscope (SEM), energy dispersive spectroscopy, atomic force microscope (AFM), UV-visible absorption spectra and studied for their photoluminescence (PL) properties. SEM and AFM results show spherical nanoparticles with size around 70–80 nm. These nanoparticles have almost equal sizes and a homogeneous size distribution. The maximum absorption of Alq₃ nanoparticles is observed at 300 nm, while the surface plasmon resonant band of Ag doped sample appears at 450 nm. The PL emission spectra of Tb, Cu and Ag doped Alq₃ nanoparticles show a single broad band at around 515 nm, which is similar to that of the pure one, but with enhanced PL intensity. The sample doped with Ag at a concentration ratio of Alq₃:Ag?=?1:0.8 is found to have the highest PL intensity, which is around 2 times stronger than that of the pure one. This enhancement could be attributed to the surface plasmon resonance of Ag ions that might have increased the absorption and then the quantum yield. These remarkable result suggest that Alq₃ nanoparticles incorporated with Ag ions might be quite useful for future nano-optoelectronic devices.     

Photoinduced formation and aggregation of silver nanoparticles at the surface of carboxymethylcellulose films

Formation and aggregation of photolytic silver nanoparticles at the surface of silver salt of carboxymethylcellulose films (CMCAg films) have been investigated. Detailed X-ray photoelectron spectroscopy (XPS) study and field emission type scanning electron microscopy (FE-SEM) observation have been carried out to characterize silver nanoparticles at the film surface. When the CMCAg films were irradiated with UV light in wet air at room temperature for 30–60 min, silver nanoparticles of ca. 10 nm size were formed at the irradiated surface. According to the FE-SEM observation, the growth of the particle diameter and aggregation of nanoparticles took place after prolonged irradiation, and finally, the irradiated side of the film surface was densely covered with the silver nanoparticles of ca. 35 nm size. Chemical composition analysis by the XPS measurements has confirmed the increase in the atomic concentration of silver with irradiation time. It is suggested that silver atoms and clusters can move in the film and precipitate at the irradiated surface.     

Synthesis and photo physical properties of Au @ Ag (core @ shell) nanoparticles disperse in poly vinyl alcohol matrix

Synthesis of core @ shell (Au @ Ag) nanoparticle with varying silver composition has been carried out in aqueous poly vinyl alcohol (PVA) matrix. Core gold nanoparticle (~15 nm) has been synthesized through seed-mediated growth process. Synthesis of silver shell with increasing thickness (~1–5 nm) has been done by reducing Ag⁺ over the gold sol in the presence of mild reducing ascorbic acid. Characterization of Au @ Ag nanoparticles has been done by UV–Vis, High resolution transmission electron microscope (HRTEM) and energy dispersive X-ray (EDX) spectroscopic study. The blue shift of surface plasmon resonance (SPR) band with increasing mole fraction of silver has been interpreted due to dampening of core, i.e. Au SPR by Ag. The dependence of nonlinear optical response of spherical core @ shell nanoparticles has been investigated as a function of relative composition of each metal. Simulation of SPR extinction spectra based on quasi-static theory is done. A comparison of our experimental and the simulated extinction spectra using quasi-static theory of nanoshell suggests that our synthesized bimetallic particles have core @ shell structure rather than bimetallic alloy particles.