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基于模板法的銀納米結(jié)構(gòu)的可控制備及其SERS性能調(diào)控研究

發(fā)布時(shí)間:2018-05-06 00:45

  本文選題:超薄氧化鋁模板 + 銀點(diǎn)陣; 參考:《上海大學(xué)》2015年碩士論文


【摘要】:超薄氧化鋁模板(ultra-thin alumina mask,UTAM)作為多孔氧化鋁模板的一種特殊結(jié)構(gòu),具有大面積、結(jié)構(gòu)參數(shù)(大小、間距、形貌)可控、超高密度、高產(chǎn)出、低設(shè)備投入等優(yōu)點(diǎn)。這些優(yōu)點(diǎn)使得UTAM表面納米制備方法被認(rèn)為是很有前景的表面納米陣列結(jié)構(gòu)制備技術(shù);谘趸X模板開發(fā)的鋁凹坑陣列模板法同樣具有上述優(yōu)點(diǎn),其也具有易操作、不需轉(zhuǎn)移、不需去除模板等獨(dú)有的優(yōu)點(diǎn)。表面增強(qiáng)拉曼散射(Surface-enhanced Raman Scattering,SERS)目前被廣泛認(rèn)為是檢測和表征低濃度生物和化學(xué)試劑分子最強(qiáng)大的光譜工具。已被廣泛用于生物、化學(xué)傳感技術(shù)中痕量分析物的檢測,表面增強(qiáng)拉曼光譜技術(shù)克服了普通拉曼光譜技術(shù)低靈敏度的缺點(diǎn)。在生物、化學(xué)、醫(yī)學(xué)應(yīng)用以及環(huán)境監(jiān)測的領(lǐng)域有著廣泛的應(yīng)用。目前,具有大量可控的“熱點(diǎn)”、信號(hào)均一、可重復(fù)性好、大面積、低成本、性能可靠的SERS活性基底的制備仍是SERS研究中的巨大挑戰(zhàn)。本論文首次利用調(diào)控超薄氧化鋁模板的高徑比來制備不同結(jié)構(gòu)形貌的金屬銀納米點(diǎn)陣作為SERS基底,得到了羅丹明6G(Rhodamine 6G,R6G)分子水溶液在金屬銀納米點(diǎn)陣基底上的SERS光譜,并探索了其SERS性能。UTAM具有高度有序的緊密六角排列、超高密度的納米孔陣列的結(jié)構(gòu),在制備UTAM的過程中,經(jīng)過一次氧化之后去除氧化層得到的具有規(guī)則有序的六邊形納米陣列結(jié)構(gòu)的鋁基底是制備UTAM的必要條件。本論文首次利用了經(jīng)過一次氧化之后去除氧化層的鋁基底為模板,制備了結(jié)構(gòu)新穎的大面積有序的嵌入式金屬銀納米陣列,用R6G分子水溶液作為探針分子,對(duì)其SERS性能進(jìn)行研究,并且考察了其制備條件對(duì)結(jié)構(gòu)的影響。具體內(nèi)容歸納如下:1.在溫度2℃條件下濃度0.3 M草酸電解質(zhì)溶液中采用兩步陽極氧化法制備了結(jié)構(gòu)高度有序的UTAM,通過改變氧化電壓,擴(kuò)孔時(shí)間,二次氧化時(shí)間制備了一系列結(jié)構(gòu)參數(shù)可調(diào)可控的UTAM。利用掃描電子顯微鏡(SEM)對(duì)這些不同結(jié)構(gòu)參數(shù)的UTAM進(jìn)行形貌表征。2.我們利用通過改變二次氧化時(shí)間制備的UTAM作為蒸發(fā)掩模板,采用真空鍍膜技術(shù)制備了大面積高度有序的銀納米點(diǎn)陣。首次利用調(diào)控超薄氧化鋁模板的高徑比來制備不同結(jié)構(gòu)形貌的金屬銀納米點(diǎn)陣作為SERS基底,得到了R6G分子水溶液在金屬銀納米點(diǎn)陣基底上的SERS光譜,并探索了其SERS性能。3.利用UTAM一次氧化后去除氧化層留下的具有有序凹坑陣列的鋁基底為模板,采用真空氣相沉積技術(shù),成功制備了新型的有序嵌入式銀納米點(diǎn)陣結(jié)構(gòu)。選用R6G作為探針分子,探索嵌入式銀納米點(diǎn)陣基底的SERS性能。結(jié)果表明,這種新型的嵌入型納米結(jié)構(gòu)具有很高的SERS活性,R6G分子濃度為10-10 M時(shí)增強(qiáng)因子高達(dá)3.74×1010,檢出濃度低至10-11 M。因此這種基底可用于化學(xué)物質(zhì)和生物分子的痕量檢測和分析。與此同時(shí)我們還研究了制備條件(氧化電壓、蒸發(fā)厚度、蒸發(fā)速率)對(duì)這種嵌入式納米點(diǎn)陣的結(jié)構(gòu)及其SERS性能的影響,最終得到制備這種結(jié)構(gòu)的最佳優(yōu)化條件。
[Abstract]:Ultra-thin alumina mask (UTAM), as a special structure of porous alumina template, has the advantages of large area, controllable structure parameters (size, spacing, morphology), high density, high yield, low input and so on. These advantages make the nano preparation method of UTAM surface is considered as a promising surface nanoarray junction. The aluminum concave pit array template based on alumina template also has the advantages mentioned above. It also has the advantages of easy operation, no transfer, and no need to remove the template. Surface enhanced Raman scattering (Surface-enhanced Raman Scattering, SERS) is currently widely considered to be the detection and characterization of low concentration biological and chemical tests. The most powerful spectroscopic tools have been widely used in the detection of trace analytes in biological and chemical sensing techniques. Surface enhanced Raman spectroscopy has overcome the disadvantages of low sensitivity in common Raman spectroscopy. It has been widely used in the fields of biology, chemistry, medical applications and environmental monitoring. The preparation of SERS active substrates with high signal uniformity, good repeatability, large area, low cost and reliable performance is still a great challenge in the study of SERS. In this paper, the high diameter ratio of ultrathin alumina templates was used for the first time to prepare metallic silver nanoparticles with different structure morphology as the SERS substrate, and Luo Danming 6G (Rhodamine 6G, R6G) was obtained. The SERS spectra of the molecular water solution on the metal silver nanoparticle substrate, and explore the structure of the highly ordered compact six angle array, the ultrahigh density nanoscale array of the SERS property.UTAM, and the regular ordered hexagonal nanoarray structure obtained after the oxidation layer was removed after one oxidation. The aluminum substrate is a necessary condition for the preparation of UTAM. In this paper, a novel and highly ordered embedded metallic silver nanoarray has been prepared by using the aluminum substrate of the oxidation layer after one oxidation. The R6G molecular water solution is used as a probe molecule, and its SERS properties are studied and the preparation conditions are investigated. The specific content of the structure is summarized as follows: 1. a highly ordered UTAM was prepared by two step anodizing in the concentration of 0.3 M oxalic acid electrolyte at 2 centigrade temperature. A series of adjustable UTAM. using scanning electron microscope (SEM) was prepared by changing the oxidation voltage, reaming time, and two times of oxidation time. UTAM morphology characterization of these different structural parameters.2. we use UTAM as an evaporative mask by changing the two times of oxidation time to prepare a large area and highly ordered silver nano lattice by vacuum coating technology. For the first time, the high diameter ratio of ultra-thin alumina template is used to prepare metal silver nanoscale with different structure morphology. As the SERS substrate, the SERS spectra of the R6G molecule water solution on the metal silver nano lattice base are obtained. The aluminum substrate with the ordered concave array with the ordered concave array left by the UTAM first oxidation after the UTAM one oxidation is explored, and the new type of ordered embedded silver nanostructure is successfully prepared by vacuum vapor deposition. R6G is used as a probe to explore the SERS properties of embedded silver nanolattice substrates. The results show that this new type of embedded nanostructure has high SERS activity. When the concentration of R6G is 10-10 M, the enhancement factor is up to 3.74 x 1010 and the detection concentration is low to 10-11 M., so this substrate can be used in chemical and raw materials. At the same time, we also studied the influence of the preparation conditions (oxidation voltage, evaporation thickness, evaporation rate) on the structure of the embedded nanolattice and its SERS properties, and finally obtained the optimal optimization conditions for the preparation of this structure.

【學(xué)位授予單位】:上海大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:O614.122;TB383.1

【共引文獻(xiàn)】

相關(guān)期刊論文 前3條

1 陳宗強(qiáng);齊繼偉;楊明;孫騫;;AAO為模板軟印模法構(gòu)建大面積高性能SERS基底(英文)[J];南開大學(xué)學(xué)報(bào)(自然科學(xué)版);2014年01期

2 王沙沙;付群;周懿;張鴻超;吳明紅;雷勇;;高拉曼增強(qiáng)銀納米帽陣列活性基底的模板法制備及其性能[J];上海大學(xué)學(xué)報(bào)(自然科學(xué)版);2013年04期

3 吳寶平;曲典;王燕;陶薔;劉文艷;滿梓焱;;表面增強(qiáng)拉曼光譜檢測系統(tǒng)在實(shí)驗(yàn)教學(xué)中的應(yīng)用[J];實(shí)驗(yàn)技術(shù)與管理;2014年05期

相關(guān)博士學(xué)位論文 前5條

1 李rc;氧化鋁模板自還原法制備金屬及合金納米線的表征與應(yīng)用[D];中國科學(xué)技術(shù)大學(xué);2013年

2 張念椿;納米微晶纖維素/金屬/電介質(zhì)雜化材料的制備與性能研究[D];華南理工大學(xué);2013年

3 夏煒煒;硅納米線陣列物性研究及其在表面拉曼增強(qiáng)中的應(yīng)用[D];浙江大學(xué);2013年

4 趙文寧;幾種柔性SERS基底的研究[D];華中科技大學(xué);2014年

5 陳守慧;金銀納米材料的可控合成及其在表面增強(qiáng)拉曼光譜檢測中的應(yīng)用[D];上海交通大學(xué);2014年

相關(guān)碩士學(xué)位論文 前6條

1 韋娜;拉曼光譜法檢測辣椒制品中羅丹明B和摻兌地溝油的花生油[D];沈陽農(nóng)業(yè)大學(xué);2013年

2 王純子;界面附近金屬納米顆粒的表面等離子體特征及其應(yīng)用[D];廈門大學(xué);2014年

3 洪玉;二維片層ZnO及其復(fù)合材料的可控合成和性能研究[D];黑龍江大學(xué);2014年

4 郭偉麗;魚肉中抗生素的表面增強(qiáng)拉曼光譜研究[D];中國海洋大學(xué);2014年

5 郇楠;蘆薈苷及其水解產(chǎn)物蘆薈大黃素的光譜檢測[D];江南大學(xué);2014年

6 吳宇鵬;ZnO/Ag復(fù)合基底材料及蛋白質(zhì)SERS的研究[D];吉林大學(xué);2014年

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