本文選題：表面增強(qiáng)拉曼散射　切入點(diǎn)：柔性襯底　出處：《中國科學(xué)技術(shù)大學(xué)》2017年博士論文　論文類型：學(xué)位論文

【摘要】：高毒性的持久性有機(jī)污染物嚴(yán)重威脅人類生存環(huán)境與健康。因此,對其快速痕量檢測至關(guān)重要。表面增強(qiáng)拉曼散射效應(yīng)(SERS)技術(shù)具有靈敏度高、響應(yīng)快和"指紋"識別等優(yōu)點(diǎn),在快速檢測有毒污染物方面具有潛在的應(yīng)用前景。應(yīng)用SERS檢測技術(shù)的關(guān)鍵是構(gòu)筑高質(zhì)量的SERS襯底。本文以有毒污染物的快速痕量檢測為導(dǎo)向,采用幾種柔性材料作為支撐結(jié)構(gòu)負(fù)載貴金屬納米結(jié)構(gòu),構(gòu)筑了幾種柔性SERS襯底;并提出了一種新型的SERS檢測盒器件,系統(tǒng)研究了柔性SERS襯底和原型器件的SERS性能及其對有毒有機(jī)污染物的SERS敏感性。本論文的主要研究內(nèi)容和創(chuàng)新性如下:1.利用氣-液界面自組裝方法,制備了由單層Ag納米立方體組成的薄膜,再將其轉(zhuǎn)移到柔性透明的聚乙烯膜上,獲得了 Ag納米立方體修飾聚乙烯膜的復(fù)合SERS襯底。該柔性透明SERS襯底在大面積范圍內(nèi)信號均勻、穩(wěn)定、重復(fù)性好和靈敏度高。尤其是該SERS襯底具有良好的透明性,入射光能從該透明SERS襯底背面穿過直接作用在Ag納米立方體上。因此,這種柔性透明SERS襯底能直接貼在受污染的水果表面,實(shí)現(xiàn)了對被污染桔子表面10 pmol甲基對硫磷的快速原位檢測。2.通過化學(xué)法在銅絲網(wǎng)上的每根銅絲的表面原位生長三維Cu(OH)2納米線陣列,在其表面濺射修飾Ag納米顆粒,形成Ag納米顆粒修飾的Cu(OH)2納米線/銅絲網(wǎng)分級陣列。Cu(OH)2納米線陣列在三維空間內(nèi)為貴金屬納米顆粒提供大量的負(fù)載位點(diǎn),這些Ag納米顆粒能產(chǎn)生大量的"熱點(diǎn)"。因此,該SERS襯底對羅丹明R6G濃度低至0.1 pM時仍然敏感,且能快速識別10 nM的福美雙分子。3.采用銀鏡還原法在海綿表面原位生長Ag膜,獲得多孔Ag膜修飾的海綿。海綿的多孔結(jié)構(gòu)能增加單位體積內(nèi)的SERS活性單元。該Ag膜修飾的海綿具有很好的吸水特性,能直接浸沒在待測溶液中與待測分子充分接觸。利用手持式便攜拉曼儀和該SERS襯底,實(shí)現(xiàn)了對1 nM的腺嘌呤和10 nM福美雙水溶液的原位快速檢測。4.利用銀鏡還原法在明列子的3D網(wǎng)絡(luò)上修飾Ag納米顆粒,獲得Ag納米顆粒修飾的明列子。將明列子的SERS基底置于器件的凹槽內(nèi),與一次性滴管結(jié)合吸取液體樣品,獲得滴管式SERS器件。干燥的SERS基底吸水膨脹填滿凹槽空間,排出器件內(nèi)多余的液體,減少了液體對入射光散射所導(dǎo)致的信號強(qiáng)度降低;同時能避免從牛奶中提取三聚氰胺的復(fù)雜步驟。采用該滴管式SERS器件,實(shí)現(xiàn)了快速檢測牛奶中1 μ的三聚氰胺。
[Abstract]:Highly toxic persistent organic pollutants (pops) pose a serious threat to human living environment and health. Therefore, rapid trace detection is very important. Surface enhanced Raman scattering (SERS) technique has the advantages of high sensitivity, fast response and "fingerprint" recognition. It has a potential application prospect in rapid detection of toxic pollutants. The key to the application of SERS detection technology is to construct high-quality SERS substrates. This paper is directed by the rapid trace detection of toxic pollutants. Several kinds of flexible SERS substrates are constructed by using several flexible materials as supporting structures to support noble metal nanostructures, and a new type of SERS detection box device is proposed. The SERS properties of flexible SERS substrates and prototype devices and their SERS sensitivity to toxic organic pollutants are systematically studied. The main contents and innovations of this thesis are as follows: 1. Using the gas-liquid interface self-assembly method, A thin film composed of a monolayer Ag nano-cube was prepared and transferred to a flexible and transparent polyethylene film. A composite SERS substrate modified with Ag nanocrystalline cubic polyethylene film was obtained. The flexible transparent SERS substrate has the advantages of uniform signal, stable signal, good reproducibility and high sensitivity in a large area. Especially, the SERS substrate has good transparency. The incident light passes through the surface of the transparent SERS substrate directly onto the Ag nanoscale cube. Therefore, the flexible transparent SERS substrate can be directly attached to the contaminated fruit surface. The rapid in situ detection of 10 pmol methyl parathion on the surface of contaminated orange was achieved. The three-dimensional Cu(OH)2 nanowire array was grown on the surface of each copper wire on the copper wire by chemical method, and the Ag nanoparticles were modified by sputtering on the surface. The Cu(OH)2 nanowire / copper wire mesh grading array. CuOH2 nanowire array modified with Ag nanoparticles provides a large number of loading sites for noble metal nanoparticles in three dimensional space, and these Ag nanoparticles can produce a large number of "hot spots". The SERS substrate is still sensitive to the concentration of Rhodamine R6G as low as 0.1 pm, and can quickly recognize 10 nm of Formet bimolecule. Silver mirror reduction method is used to grow Ag film on sponge surface in situ. A porous Ag membrane modified sponge was obtained. The porous structure of the sponge can increase the SERS active unit in the unit volume. The Ag membrane modified sponge has a good water absorption property. Can be directly immersed in the solution to be tested in full contact with the molecules to be tested, using hand-held portable Raman spectroscopy and the SERS substrate, In situ rapid detection of 1 nm adenine and 10 nm Fu Mei aqueous solution was carried out. Silver mirror reduction method was used to modify Ag nanoparticles on the 3D network of Minglezi. The SERS substrate of the silver nanoparticles was prepared by placing the SERS substrate in the grooves of the device, and then combining with the disposable dropper to absorb the liquid sample to obtain the SERS device. The dry SERS substrate was filled with water swelling to fill the grooves. Removing excess liquid from the device reduces the signal intensity caused by the liquid scattering from the incident light, and avoids the complicated steps of extracting melamine from milk. The rapid detection of 1 渭 m melamine in milk was achieved.
【學(xué)位授予單位】：中國科學(xué)技術(shù)大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：X830.2;O657.37

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