一种保护层可揭除的新鲜多级银SERS活性基底

doi:10.7503/cjcu20180366

高等学校化学学报 ›› 2018, Vol. 39 ›› Issue (12): 2752.doi: 10.7503/cjcu20180366

一种保护层可揭除的新鲜多级银SERS活性基底

徐蔚青¹, 管树霖², 王祎¹, 王馨楠¹, 陶艳春¹(), 徐抒平¹

1. 吉林大学超分子结构与材料国家重点实验室, 理论化学研究所, 长春 130012
2. 延边大学理学院化学系, 延吉 133002

收稿日期:2018-05-17 出版日期:2018-12-03 发布日期:2018-09-29
作者简介:
联系人简介: 陶艳春, 女, 高级工程师, 主要从事光谱分析研究. E-mail: taoyc@jlu.edu.cn
基金资助:
国家自然科学基金(批准号: 21573087, 21573092, 201873039)资助.

Fresh Hierarchical Periodic Silver SERS-active Substrate with the Band-aid Protecting Layer^†

XU Weiqing¹, GUAN Shulin², WANG Yi¹, WANG Xinnan¹, TAO Yanchun^1,^*(), XU Shuping¹

1. State Key Laboratory of Supramolecular Structure and Materials, Institute of Theoretical Chemistry,Jilin University, Changchun 130012, China
2. Department of Chemistry, College of Science, Yanbian University, Yanji 133002, China

Received:2018-05-17 Online:2018-12-03 Published:2018-09-29
Contact: TAO Yanchun E-mail:taoyc@jlu.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(Nos.21573087, 21573092, 201873039).

摘要/Abstract

摘要：

以多级结构的阳极氧化铝(AAO)为模板, 通过真空蒸镀金属银层拷贝AAO的多级结构, 获得了以AAO及铝基为保护层的银多级微纳结构. 该保护层可在基底用于表面增强拉曼散射(SERS)检测时直接揭除. 此方法解决了传统银材质纳米结构作为SERS基底使用时表面易被氧化及污染的问题, 可最大程度保证基底的新鲜度, 做到即用即揭.

关键词: 表面增强拉曼散射基底, 阳极氧化铝模板, 保护层

Abstract:

A novel band-aid like, hierarchical periodic structured, multilayered surface-enhanced Raman scattering(SERS) substrate was developed, which allows a fresh silver surface when peeling off the protector. It was prepared by the vacuum deposition of a thick Ag layer(600 nm) on a hierarchical periodic structured anodic alumina(AAO) that was achieved by anodizing a pre-patterned Al base by means of the nanoimprint lithography with a hard Ni mask, while the AAO layer plays a role of surface protector. Then, the Ag side was glued to a glass slide. When it is used for SERS, the AAO layer can be peeled off to allow for a naked, fresh Ag surface for SERS measurements. This method solves the problem of oxidation and pollution of traditional Ag SERS substrates, ensuring the freshness of the SERS substrate. The AAO preparation steps are largely simplified compared with other AAO preparation procedures. Owing to the use of the nanoimprint lithography, the periodic structure of the Ni stamp can be well copied, which insures the reducibility of the final SERS substrate in SERS measurements. Apparently, the substrate preparation is time-saving and easier, which makes this band-aid like SERS substrate promising for being a commercial SERS substrate.

Key words: Surface-enhanced Raman scattering(SERS) substrate, Anodic alumina(AAO) template, Protective layer

中图分类号:

O647
O657

TrendMD:

徐蔚青, 管树霖, 王祎, 王馨楠, 陶艳春, 徐抒平. 一种保护层可揭除的新鲜多级银SERS活性基底. 高等学校化学学报, 2018, 39(12): 2752.

XU Weiqing,GUAN Shulin,WANG Yi,WANG Xinnan,TAO Yanchun,XU Shuping. Fresh Hierarchical Periodic Silver SERS-active Substrate with the Band-aid Protecting Layer^†. Chem. J. Chinese Universities, 2018, 39(12): 2752.

图/表 8

Fig.1 SEM images of patterns on Al and Ag surfaces during the substrate preparation(A) Patterned Al foil after Ni nano-stamping; (B) the achieved AAO after 15 min anodization; (C) AAO after pore size widening; (D) Ag surface copied from the patterned AAO.

Fig.2 SEM images of the AAO templates(A1—D1) and their resulted Ag substrates(A2—D2)with different pore-widen time(A1—D1) AAO templates achieved with the pore-widen time of 40, 70, 100 and 130 min, respectively;(A2—D2) the achieved Ag substrates with the gaps between rods of 69, 29, 19 and 9 nm, respectively.

Fig.3 SERS intensities of 4-Mpy on different SERS substrates with different gap distances between rods5.0 μL of 4-Mpy solution(1.0×10-4 mol/L) was dripped on the substrates and SERS measurement was carried out from five spots on each substrate. Laser power was set as 1.0 μW/cm2 with the accumulation time of 10 s.

Fig.4 SERS spectra from randomly selected 10 points on the same substrate(A) and the intensities of two different peaks at 10 points on one substrate(B)

Fig.5 Comparison of SERS and normal Raman spectra of 4-Mpy5.0 μL of 4-Mpy solution(1.0×10-4 mol/L) was dripped on the substrate to form a 2.40 mm-diameter casting film for recording SERS. 5.0 μL of 4-Mpy solution(0.5 mol/L) was dripped on a silica slide to form a 2.90 mm-diameter casting film for Raman spectrum.

Fig.6 SERS spectra of 4-Mpy(1.0×10-4 mol/L) with the enhancement of fresh Ag nanorod substrate(a) and the air condition exposed(8 month) Ag nanorod substrate(b)

Fig.7 SERS detection of thiramInset: structure of thiram. 5.0 μL of thiram solutions of 6.11×10-4(a), 6.11×10-5(b) and 6.11×10-6 mol/L(c) were dripped on the substrate and dried for SERS measurements.

Fig.8 Scheme 1 Preparation of the hierarchical AAO-based Ag SERS substrate(Ⅰ) and the utilization of this band-aid SERS substrate for measurements(Ⅱ)

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一种保护层可揭除的新鲜多级银SERS活性基底

Fresh Hierarchical Periodic Silver SERS-active Substrate with the Band-aid Protecting Layer^†

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一种保护层可揭除的新鲜多级银SERS活性基底

Fresh Hierarchical Periodic Silver SERS-active Substrate with the Band-aid Protecting Layer†

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Fresh Hierarchical Periodic Silver SERS-active Substrate with the Band-aid Protecting Layer^†