摘要
由于纳米金属粒子具有独特的光学、电学性质,在合适的尺度可产生超强的表面增强拉曼光谱(SERS)效应,特别是产生的“热点”(hot spot)效应时,其增强因子可高达1014,故受到了广大科研工作者的广泛关注。DNA是天然的生物大分子。DNA分子具有良好的纳米尺度以及分子识别和自组装能力。以DNA为模板合成纳米材料是当前合成纳米材料的热点之一。具有Keggin结构的无机簇合物12-硅钨酸具有多种功能。利用上述两种物质为模板剂,结合光辐照法等方法合成出Au-Ag-DNA和Ag-SMNs等新奇结构的SERS敏感基底,并实现了对材料的大小和形貌的控制合成;同时研究了利用这些材料对TNT的痕量检测。详细内容归纳如下:
1在光照射条件下,以DNA为模板,太阳光提供反应动力,通过两步光化学反应,成功在DNA纳米网上构建出Au-Ag合金以及Au@Ag核壳材料。DNA在合成过程中担当着模板剂和还原剂的双重功能。金壳银核或金-银合金纳米DNA网络结构的合成是源于纳米颗粒的种子理论。实验发现,这种金壳银核或金-银合金纳米DNA网络结构是良好的表面增强拉曼散射(SERS)活性基底,对TNT检测效果突出。最低检测限可达10-12M,增强因子可达1011-1012数量级。
2利用硅钨酸合成钼酸银纳米线,如果在合成中加紫外光照射条件,在多聚钼酸银表面将原位生成银纳米颗粒。为了实现对目标分子TNT的主动抓捕富集,我们又将含有氨基的对巯基苯胺修饰到上述银-钼酸银复合基地上。同样在紫外光激发下,对巯基苯胺在银表面发生自催化的二聚反应,生成4,4-偶氮苯(DMAB), DMAB作为交联剂,将大量的纳米线连接到一起,生成许多“热点”。同时,我们采用类分子印迹的方法,在上述交联的DMAB分子中构建TNT分子识别位点,为TNT提供富集抓手。实验证明经对巯基苯胺修饰的银-钼酸银复合基底有很好的SERS增强能力,并且对TNT具有很强的选择识别能力,对TNT检测限为10-12 M。有趣的
Because of nanoparticle having unique optic and electric property, ideal enhanced effect was observed on definite-size Au or Ag nanoparticles, and its enhancement factor can reach to 1014 on some“hot spot”between nanoparticles, which attracted extensive attention of scientists. DNA as biomacromolecules can be utilized as templates to build novel hybrid nanostructures. DNA has been exploited as a template for the fabrication of metallic nano-materials. It was found that the DNA acted as templates and reducing agent in formation of the novel nanostructure,so DNA was used in this article as an soft template for fabricating SERS substrate. Utilizing Tungstosilicate acid ion to synthesize nanoparticles was another an important method. Tungstosilicate acid could be as photocatalyst, stabilizer, oxidation agent, reducing agent and template. Basing on Tungstosilicate acid hard template, shape and size controlled synthesis of SERS sensitive substrate. Using these substrates, Ultrasensitive SERS Detection of TNT can be realized. The main results are summarized as follows
1 We reported a very simple and novel one-step in-situ method to synthesize silver-core-gold-shell or silver-gold alloy nanoparticles by sunlight-reducing in AgNO3 solution and NaAuCl4 solution in the presence of DNA. It was found that the DNA acted as template and reducing agent in formation of the novel nanostructure. The Ag-DNA could be formed from reduction of cationic silver absorbed on DNA template by sunlight. The silver-core-gold-shell or silver-gold alloy nanostructures were prepared by seeding with Ag-DNA in the absence of any surfactants, which could be used as active surface enhanced Raman scattering (SERS) substrates. 2,4,6-trinitrotoluene (TNT) was studied on these substrates with very low concentration (10-12 M), and great enhancement factors (3.1×1011-1.5×1012). It was found that the enhancement ability was affected by the structures of the gold and silver nanoparticles on the DNA strands. The results showed that these SERS substrates could achieve current the lowest detection limits of TNT.
2 Trace-detection of TNT is reported in this work basing on p-aminothiophenol functionalized Ag nanoparticles covered on Silver molybdate nanowires by using surface-enhanced Raman scattering (SERS).π-donor-acceptor interactions betweenπ- acceptor TNT andπ-donor p,p′-dimercaptoazobenzene (DMAB)-cross-linked Ag nanoparticles linked to the Silver molybdate nanowires, the optimal imprint molecule contours, and DMAB forming imprint molecule sites at SERS hot spots where the analyte can be allocated, these lead to a giant intensification of the Raman emission of the TNT molecule. This article demonstrates that TNT concentrations as low as 10-12 M can be accurately detected using the described SERS assay. Most impressively, acting as new-style SERS substrate, Ag-Silver molybdate nanowires complex can yield new Ag nanoparticles during detection process which made the Raman signals very stabilization. A detailed mechanism for SERS intensity change has been discussed. Our experiments show that TNT can be detected quickly and accurately with high trace-concentration. These results reported here not only can find many applications in SERS techniques but also can form the new concept of a molecularly imprinting strategy.
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