【摘要】：表面增強拉曼散射(Surface-enhanced Raman Scattering,SERS)作為一種高靈敏度檢測手段,基底制備是關(guān)鍵環(huán)節(jié),活性強、穩(wěn)定性好、可重復(fù)使用的基底對于應(yīng)用和基礎(chǔ)研究都具有重要意義。本文主要將膠體球有序模板和磁控濺射技術(shù)相結(jié)合,制備(SiO2-Ag)復(fù)合型納米圖紋結(jié)構(gòu)陣列,構(gòu)筑有序度好、穩(wěn)定性高的SERS活性基底體系,使之適用于高靈敏度SERS效應(yīng)的應(yīng)用檢測。研究基底構(gòu)型、顆粒尺寸、縫隙密度、表面形態(tài)等因素對基底表面電磁場分布和等離子體耦合的調(diào)制作用,探索SERS效應(yīng)的物理增強機制。首先,利用磁控濺射系統(tǒng)制備Si O2-Ag平面復(fù)合型SERS基底,SiO2-Ag復(fù)合基底比單純Ag膜的表面粗糙度更大。通過共濺射的方法改變材料的構(gòu)型實現(xiàn)對SERS基底表面粗糙度的調(diào)控,從而實現(xiàn)了對SERS活性基底的“熱點”密度及其增強性能的控制。其次,以不同直徑的聚苯乙烯膠體球陣列為襯底,利用雙靶共濺射Ag和SiO2的方法制備網(wǎng)狀“楊梅”型結(jié)構(gòu)陣列。每個“楊梅”是由無定形的SiO2包裹的Ag納米粒子所構(gòu)成的,Ag納米粒子大小為10-20 nm,SiO2厚度為2-5 nm,這種結(jié)構(gòu)基底提供了更多的“熱點”。SiO2-Ag納米帽子呈現(xiàn)各向異性生長的特點,縱向生長速度大于橫向生長速度。隨著SiO2-Ag薄膜厚度的增加,薄膜的表面粗糙度以及相鄰“楊梅”之間的距離都隨之變化,改變了相鄰局域電磁場的耦合,從而實現(xiàn)對SERS增強能力的調(diào)控。不同激發(fā)光波長對樣品測試SERS的實驗結(jié)果表明:“楊梅”型SiO2-Ag納米結(jié)構(gòu)陣列在可見到近紅外光激發(fā)下均表現(xiàn)出較高的增強能力,且整個樣品表面具有較好的穩(wěn)定性和均勻性。最后,利用膠體球模板和物理沉積技術(shù)相結(jié)合,制備了[Ag 30 nm/SiO2 5 nm]n(n=1-4)多層膜納米結(jié)構(gòu)陣列,SEM形貌測試顯示多層膜陣列沿縱向生長,形成納米“柱-帽”對結(jié)構(gòu),并且具有良好的SERS增強性能。熱處理結(jié)果表明,[Ag/SiO2]n(n=4)多層膜陣列隨著熱處理溫度的升高表面形貌發(fā)生巨大的變化;其中熱處理600度后的樣品SERS增強最大。SERS光譜測試表明,熱處理600度后,隨著周期數(shù)的增加,拉曼峰得到明顯的增強。SiO2層不僅可以對拉曼具有較好的增強效果,并且提高了SERS基底的穩(wěn)定性。
[Abstract]:Surface enhanced Raman scattering (Surface-enhanced Raman scattering) is a high sensitivity detection method. Substrate preparation is a key link with strong activity and good stability. The reusable substrate is of great significance for application and basic research. In this paper, the colloidal sphere ordered template was combined with magnetron sputtering technique to fabricate (SiO2-Ag) composite nanogram structure array to construct a SERS active substrate system with good order and high stability, which makes it suitable for the application of high sensitivity SERS effect detection. The modulation effects of substrate configuration, particle size, gap density and surface morphology on the electromagnetic field distribution and plasma coupling on the substrate surface are studied, and the physical enhancement mechanism of the SERS effect is explored. Firstly, the surface roughness of Si O2-Ag planar composite SERS substrate SiO2-Ag is higher than that of pure Ag film by magnetron sputtering system. The surface roughness of SERS substrate can be controlled by changing the configuration of the material by co-sputtering, thus controlling the "hot spot" density of SERS active substrate and its enhancement performance. Secondly, using polystyrene colloidal sphere arrays with different diameters as substrates, reticulated "bayberry" arrays were prepared by co-sputtering Ag and SiO2 with double targets. Each "Myrica" is composed of amorphous Ag nanoparticles wrapped in SiO2. The size of Ag nanoparticles is 10-20 nm / Sio _ 2 and the thickness of Sio _ 2 is 2-5 nm. This structure substrate provides more "hot spots". SiO2-Ag nanometers exhibit anisotropic growth characteristics. The longitudinal growth rate is higher than the transverse growth rate. With the increase of the thickness of SiO2-Ag films, the surface roughness of the films and the distance between the adjacent "Myrica rubra" changes, which changes the coupling of adjacent local electromagnetic fields and realizes the regulation of the enhancement ability of SERS. The experimental results of SERS measurements with different excitation wavelengths show that the "Myrica rubra" type SiO2-Ag nanostructure array exhibits high enhancement ability under near-infrared light excitation, and the whole surface of the sample has good stability and uniformity. Finally, the [Ag 30 nm/SiO2 5 nm] n (ng 1-4) multilayer nanostructure array was prepared by using the colloid sphere template and physical deposition technique. The results showed that the multilayer film array grew along the longitudinal direction and formed a "column-cap" pair of nanocrystalline films. And has the good SERS enhancement performance. The results of heat treatment show that the surface morphology of [Ag/SiO2] n (nni4) multilayer array changes greatly with the increase of heat treatment temperature, and the maximum SERS enhancement of the sample after heat treatment of 600C shows that the number of cycles increases with the heat treatment of 600C. The Raman peak can not only enhance the Raman spectra, but also improve the stability of SERS substrate.
【學(xué)位授予單位】：吉林師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：TB33

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