發(fā)布時(shí)間：2017-12-26 18:20

  本文關(guān)鍵詞：銀納米顆粒的表面改性及SERS性能研究　出處：《中北大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 銀納米顆粒 SERS 核殼結(jié)構(gòu) SiO_2 Parylene-C

【摘要】：表面增強(qiáng)拉曼散射(Surface Enhanced Raman Scattering,SERS)技術(shù)是一種高靈敏度、高分辨率的分析檢測(cè)技術(shù),目前已經(jīng)被廣泛應(yīng)用到生物醫(yī)學(xué)、材料科學(xué)、食品檢驗(yàn)、環(huán)境監(jiān)測(cè)等領(lǐng)域。隨著納米技術(shù)的發(fā)展,具有可調(diào)的表面等離子體共振特性的金屬納米顆粒襯底越來(lái)越受到各界的關(guān)注,制備出性能良好的襯底是SERS技術(shù)領(lǐng)域最為關(guān)鍵的研究?jī)?nèi)容之一。性能良好的SERS襯底不僅要有高靈敏度,還應(yīng)該具備很好穩(wěn)定性,本文主要針對(duì)銀(Ag)納米顆粒SERS襯底在應(yīng)用過(guò)程中存在的穩(wěn)定性較差的問(wèn)題,圍繞銀納米顆粒SERS襯底的制備和顆粒的表面改性展開(kāi),探討表面改性對(duì)銀納米顆粒襯底的SERS活性和穩(wěn)定性的影響:提出了采用核殼結(jié)構(gòu)增強(qiáng)襯底穩(wěn)定性的方法,研究了二氧化硅(SiO_2)包覆和聚氯代對(duì)二甲苯(Parylene-C)薄膜包覆的銀納米顆粒襯底的SERS活性,分析了核殼結(jié)構(gòu)對(duì)銀納米顆粒襯底穩(wěn)定性的增強(qiáng)效果。結(jié)果發(fā)現(xiàn)本文制備的核殼結(jié)構(gòu)襯底在增強(qiáng)銀納米顆粒襯底的SERS活性,增加襯底穩(wěn)定性或可重復(fù)利用性方面效果顯著。論文首先簡(jiǎn)要介紹了納米材料,然后探討了采用磁控濺射工藝和退火工藝獲得粒徑分布均勻、納米粒子排布致密的銀納米顆粒陣列的工藝參數(shù),并以結(jié)晶紫分子為探針表征了銀納米顆粒陣列作為SERS活性襯底的增強(qiáng)作用,通過(guò)計(jì)算得到襯底的增強(qiáng)因子為2.15×106。本文然后采用化學(xué)氣相淀積法制備得到不同二氧化硅包覆厚度的二維Ag@SiO_2核殼結(jié)構(gòu)傳感襯底。采用結(jié)晶紫分子為探針表征了Ag@SiO_2核殼結(jié)構(gòu)襯底對(duì)拉曼信號(hào)的增強(qiáng)作用。實(shí)驗(yàn)結(jié)果表明,基于Ag@SiO_2核殼結(jié)構(gòu)的SERS襯底活性隨二氧化硅的包覆厚度的增加呈先增強(qiáng)后減弱趨勢(shì),在包覆厚度為10 nm時(shí),襯底的SERS活性最強(qiáng),其增強(qiáng)因子可達(dá)6.62×106,對(duì)結(jié)晶紫分子的檢測(cè)限達(dá)10-12 M。在此基礎(chǔ)上,采用去離子水浸泡實(shí)驗(yàn)評(píng)估了Ag@SiO_2納米結(jié)構(gòu)SERS襯底的穩(wěn)定性,結(jié)果表明,浸泡在水溶液中的基于Ag@SiO_2納米結(jié)構(gòu)襯底的穩(wěn)定性可由0.5 h延長(zhǎng)至24 h,且在浸泡72 h后襯底的SERS活性的衰減幅度小于25%。針對(duì)二氧化硅包覆材料存在的可重復(fù)利用性較差的問(wèn)題,采用Parylene-C薄膜對(duì)銀納米顆粒進(jìn)行包覆,詳細(xì)闡述了Parylene-C薄膜的沉積工藝,對(duì)比了制備過(guò)程中不同包覆厚度的Parylene-C薄膜對(duì)襯底的包覆效果和SERS活性的影響。在此基礎(chǔ)上制備了簡(jiǎn)易的微流體溝道,并與Ag@Parylene-C納米結(jié)構(gòu)襯底集成,表征Ag@Parylene-C納米結(jié)構(gòu)襯底對(duì)拉曼信號(hào)的增強(qiáng)效果,以及襯底在液相環(huán)境下的穩(wěn)定性。本文發(fā)現(xiàn)在沉積膜厚為100 nm時(shí)襯底的包覆效果好且SERS活性強(qiáng),對(duì)結(jié)晶紫分子的檢測(cè)限可達(dá)10-10 M,與微流體溝道集成后,襯底的可重復(fù)利用次數(shù)由20次增加到了500次,且Ag@Parylene-C納米結(jié)構(gòu)襯底的SERS活性在此過(guò)程中的衰減幅度小于10%,驗(yàn)證了Ag@Parylene-C納米結(jié)構(gòu)SERS基底在微流體檢測(cè)應(yīng)用中的可行性。
[Abstract]:Surface Enhanced Raman Scattering (SERS) technology is a highly sensitive and high-resolution analytical technology. It has been widely applied in biomedicine, material science, food inspection, environmental monitoring and other fields. With the development of nanotechnology, the surface of metal nanoparticles with tunable surface plasmon resonance has attracted more and more attentions from all walks of life. It is one of the most important research contents to prepare good performance substrates in the field of SERS technology. SERS substrate with good performance not only have high sensitivity, but also have good stability, in this paper, silver (Ag) poor stability problems in the application process of SERS nanoparticles on the substrate, the surface of silver nanoparticles SERS substrate preparation and particle modification, to investigate the effect of surface modification of silver nanoparticle substrate SERS activity and stability is proposed using core-shell structure method to enhance the stability of silica substrate, coating (SiO_2) and poly chloro-p-xylylene (Parylene-C) activity of SERS thin film coated silver nanoparticles substrate, analyzed the enhancement effect of core-shell structure on silver nanoparticles substrate stability. It is found that the core shell structure prepared in this paper is effective in enhancing SERS activity, increasing substrate stability and reusing of silver nanoparticles. The paper first briefly introduces the nano materials, and then discusses the process parameters of silver nanoparticle array with uniform particle size distribution, compact arrangement of nanoparticles obtained by magnetron sputtering and annealing process, and the crystal violet probe molecules for characterization of silver nanoparticle arrays as the enhancement of SERS activity of the substrate, the substrate through the calculation of the enhancement factor 2.15 x 106. In this paper, a two-dimensional Ag@SiO_2 core shell structure sensing substrate with different silica coating thickness was prepared by chemical vapor deposition (CVD). The crystal violet is used as a probe to characterize the enhancement of the Raman signal by the Ag@SiO_2 core - shell structure. The experimental results show that the Ag@SiO_2 core-shell structure SERS substrate with active silica coating thickness increases firstly increased and then decreased trend based on the coating thickness is 10 nm, the SERS activity of the substrate, the enhancement factor of 6.62 * 106, the detection limit of 10-12 crystal violet molecules M. On this basis, using deionized water immersion test in evaluating stability, Ag@SiO_2 nano structure SERS substrate. The results showed that soaking stability of Ag@SiO_2 nano structure substrate can be extended from 0.5 h to 24 h in aqueous solution, and after soaking for 72 h SERS active substrate attenuation rate of less than 25%. The silica coated materials are reused on the problem of the poor, silver nanoparticles were coated with Parylene-C film, describes the deposition process of Parylene-C films, influence the coating effect of SERS and the activity of Parylene-C films with different thickness of coating were compared in the process of the preparation of the substrate. On this basis, a simple microfluidic channel was fabricated and integrated with Ag@Parylene-C nanostructured substrate to characterize the enhancement effect of Ag@Parylene-C nanostructure substrate on Raman signal and the stability of substrate in liquid phase. This article found in the deposited film thickness is 100 nm when the effect of coating substrate is good and the activity of SERS, the detection limit of 10-10 crystal violet molecules M, and micro channel integration, the substrate can be reused number from 20 to 500, the attenuation rate of less than 10% SERS and Ag@Parylene-C activity in this process the nano structure of the substrate in the validation of the Ag@Parylene-C nano structure SERS substrate in the feasibility of the application in the detection of micro fluid.
【學(xué)位授予單位】：中北大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TB383.1

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