本文選題：呼吸圖技術(shù) + 蜂窩狀多孔薄膜　； 參考：《江蘇科技大學(xué)》2017年碩士論文

【摘要】：表面增強(qiáng)拉曼散射作為一種獨(dú)特的光譜檢測(cè)技術(shù),自發(fā)現(xiàn)以來便在檢測(cè)極微量小分子方面發(fā)揮了極大的作用。因此,被逐漸應(yīng)用到環(huán)境監(jiān)測(cè)、食品安全、醫(yī)療健康、光電傳感器等諸多領(lǐng)域。眾所周知,活性基底的制備是獲得SERS(Surface Enhanced Raman Scattering)信號(hào)的前提,為了使SERS技術(shù)更好地應(yīng)用于定量分析,所制備的SERS基底應(yīng)具有增強(qiáng)能力強(qiáng)且均一性好、易于制備和存儲(chǔ)、使用方便等優(yōu)點(diǎn)。因此,SERS活性基底的制備方法尤為重要。國內(nèi)外研究者在SERS活性基底的制備及其表面增強(qiáng)拉曼性能的研究方面已開展了大量的工作并取得了較大的進(jìn)展,但是仍缺乏成本低廉、均勻、穩(wěn)定、重復(fù)性好、增強(qiáng)能力強(qiáng)的通用SERS活性基底。基于現(xiàn)狀,本文以蜂窩狀多孔結(jié)構(gòu)薄膜為模板,制備Au、Au-Ag、Ag納米顆粒薄膜,并對(duì)其SERS性能進(jìn)行系統(tǒng)研究。本論文主要研究結(jié)果如下:(1)采用靜態(tài)呼吸圖方法,制備聚苯乙烯-嵌段-聚(4-乙烯基)吡啶(PS-b-P4VP)蜂窩狀多孔結(jié)構(gòu)薄膜。研究溶劑、聚合物濃度、分子量對(duì)蜂窩狀多孔結(jié)構(gòu)薄膜形成的影響。結(jié)果表明:對(duì)于PS(122k)-b-P4VP(22k),以CHCl3為溶劑,當(dāng)聚合物溶液濃度為30 mg/m L時(shí)所形成的蜂窩狀多孔薄膜具備規(guī)整且孔徑均一的有序結(jié)構(gòu),孔徑約為2.87μm。濃度偏高或者偏低都會(huì)形成不規(guī)整的孔結(jié)構(gòu)。三種不同嵌段比的嵌段共聚物中,當(dāng)嵌段比為5:1時(shí),獲得的多孔結(jié)構(gòu)薄膜的有序性最佳。以CS2為溶劑時(shí),PS(122k)-b-P4VP(22k)的濃度為10~ mg/mL時(shí)即可形成規(guī)整結(jié)構(gòu)的多孔薄膜,但孔徑較大,約為4.27μm,隨著濃度的不斷增加,孔結(jié)構(gòu)逐漸消失。(2)上述蜂窩狀多孔結(jié)構(gòu)薄膜經(jīng)處理后作為模板,結(jié)合光化學(xué)還原途徑制備Au納米顆粒薄膜。HAuCl_4溶液濃度為0.025 mol/L(V水:V乙醇=1:1),紫外燈光照3 h的條件下所制備的Au納米顆粒薄膜作為SERS活性基底具備最佳的SERS性能,對(duì)R6G(羅丹明6G)分子的增強(qiáng)因子可達(dá)6.50×10~6,其檢測(cè)極限低達(dá)10~-8 mol/L,對(duì)CV(結(jié)晶紫)分子也具有良好的SERS增強(qiáng)效果,增強(qiáng)因子達(dá)6.03×10~4。(3)以上述制備的Au納米顆粒薄膜作為模板,同樣采用光化學(xué)還原途徑制備Au-Ag納米顆粒薄膜。AgNO_3溶液(V水:V乙醇=1:1)濃度為0.05 mol/L,紫外燈光照2 h的條件下所制備的Au-Ag納米顆粒薄膜作為SERS活性基底具備最佳的SERS性能,對(duì)R6G分子的增強(qiáng)因子可達(dá)1.05×10~7,其檢測(cè)極限低達(dá)10~-9mol/L,對(duì)CV分子的增強(qiáng)因子達(dá)2.41×10~6。并且該基底具備良好的穩(wěn)定性,其拉曼信號(hào)的RSD(相對(duì)標(biāo)準(zhǔn)偏差)低于20%。(4)采用類似的方法制備Ag納米顆粒陣列薄膜。Ag NO_3溶液濃度為0.05 mol/L(V_水:V_乙醇=1:1),紫外燈光照3 h的條件下所制備的Ag納米顆粒陣列薄膜作為SERS活性基底具備最佳的SERS性能,對(duì)R6G分子的增強(qiáng)因子可達(dá)1.31×10~9,其檢測(cè)極限低達(dá)10~-10~mol/L。對(duì)CV分子的增強(qiáng)因子達(dá)8.46×10~5。另外,相比較而言,Ag納米顆粒陣列薄膜以浸泡方式吸附R6G具有更好的穩(wěn)定性,其拉曼信號(hào)的RSD低于13%。
[Abstract]:Surface enhanced Raman scattering (SERS), as a unique spectral detection technique, has played an important role in the detection of very small molecules since it was discovered. Therefore, it has been gradually applied to many fields, such as environmental monitoring, food safety, medical health, photoelectric sensors and so on. It is well known that the preparation of active substrates is the prerequisite for obtaining SERS(Surface Enhanced Raman Scattering) signals. In order to make the SERS technology more suitable for quantitative analysis, the prepared SERS substrates should have strong enhancement and good uniformity, and be easy to prepare and store. Advantages such as ease of use. Therefore, the preparation method of SERS active substrate is particularly important. Researchers at home and abroad have carried out a lot of work and made great progress in the preparation of SERS active substrates and their surface-enhanced Raman properties, but there is still a lack of low cost, uniform, stable and reproducible. Enhanced ability of the universal SERS active substrate. Based on the present situation, Au-Ag-Ag nano-particle films were prepared by using honeycomb porous films as templates, and their SERS properties were systematically studied. The main results of this thesis are as follows: (1) the honeycomb porous structure films of polystyrene-block poly (4-vinylpyridine) pyridine (PS-b-P4VP) were prepared by using static respiration method. The effects of solvent, polymer concentration and molecular weight on the formation of honeycomb porous films were studied. The results show that the honeycomb porous films formed by using CHCl3 as solvent and the concentration of polymer solution at 30 mg/m L have regular ordered structure and uniform pore size, and the pore size is about 2.87 渭 m. An irregular pore structure is formed when the concentration is on the high side or on the low side. Among the three kinds of block copolymers with different block ratios, when the block ratio is 5:1, the order of porous films is the best. When CS2 was used as solvent, the porous films with regular structure could be formed at the concentration of 10 ~ mg/mL, but the pore size was larger, about 4.27 渭 m. With the increasing of the concentration, the pore structure gradually disappeared. Au nanocrystalline thin films were prepared by photochemical reduction method. The solution concentration of 0.025 mol/L(V water: v ethanol was 1: 1. The au nanocrystalline films were prepared by UV lamp irradiation for 3 h. The au nanoparticles films were prepared as SERS active substrates with the best SERS properties. The enhancement factor of R6G (Rhodamine 6G) molecule is 6.50 脳 10 ~ (-6), the detection limit is 10 ~ (-8) mol / L, and the enhancement factor is 6.03 脳 10 ~ (4) C ~ (-3). The au nanocrystalline film prepared above is used as a template, and the enhancement factor is 6.03 脳 10 ~ (4) C ~ (-1), and the detection limit is 10 ~ (-8) mol 路L ~ (-1). Au-Ag nanoparticles thin films were prepared by photochemical reduction method. The concentration of Au-Ag nanoparticles was 0.05 mol / L in aqueous solution V: v ethanol: 1: 1. The Au-Ag nanocrystalline films prepared by UV lamp irradiation for 2 h had the best SERS properties as active SERS substrates. The enhancement factor for R6G molecule is 1.05 脳 10 ~ (7), the detection limit is 10 ~ (-9) mol / L, and the enhancement factor for CV molecule is 2.41 脳 10 ~ (6) mol 路L ~ (-1). And the substrate has good stability, The RSDs (relative standard deviation) of the Raman signal is lower than 20. 4) the Ag nanoparticles array films were prepared by a similar method. The concentration of Ag NO_3 solution was 0. 05 mol / L water: v _ ethanol 1: 1 and UV lamp illumination for 3 h. The Ag nanoparticles array was prepared under the condition of 0. 05 mol 路L ~ (-1) 路L ~ (-1) V _ (1) O _ (2) O _ (1) O _ 2 solution. The column films have the best SERS properties as SERS active substrates. The enhancement factor of R6G molecule can reach 1.31 脳 10 ~ (9), and its detection limit is 10 ~ 10 ~ (-1) mol 路L ~ (-1). The enhancement factor of CV molecule is 8.46 脳 10 ~ (5). In addition, the adsorption of R6G on Ag nanocrystalline array films by immersion has better stability, and the RSD of Raman signal is lower than 13%.
【學(xué)位授予單位】：江蘇科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O657.37

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相關(guān)會(huì)議論文 前1條

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本文編號(hào)：1900685