波长检测型表面等离子体共振传感器对硫堇电聚合成膜的原位分析

doi:10.7503/cjcu20160681

高等学校化学学报 ›› 2017, Vol. 38 ›› Issue (4): 567.doi: 10.7503/cjcu20160681

波长检测型表面等离子体共振传感器对硫堇电聚合成膜的原位分析

龚晓庆^1,², 万秀美^1,², 逯丹凤¹, 高然¹, 程进¹, 祁志美^1,³()

1. 中国科学院电子学研究所, 传感技术国家重点实验室, 北京100190
2. 中国科学院大学, 北京 100049
3. 国民核生化灾害防护国家重点实验室, 北京102205

收稿日期:2016-09-26 出版日期:2017-04-10 发布日期:2017-03-23
作者简介:联系人简介: 祁志美, 男, 博士, 研究员, 博士生导师, 主要从事集成光学传感器技术和表/界面光谱表征方法研究. E-mail: zhimei-qi@mail.ie.ac.cn
基金资助:
国家“九七三”计划项目(批准号: 2015CB352100)、国家自然科学基金(批准号: 61377064, 61675203)和中国科学院科研装备研制项目(批准号: YZ201508)资助

Studies of Electrochemical Polymerization of Thionine Using a Wavelength-interrogated Surface Plasmon Resonance Sensor^†

GONG Xiaoqing^1,², WAN Xiumei^1,², LU Danfeng¹, GAO Ran¹, CHENG Jin¹, QI Zhimei^1,^3,^*()

1. State Key Laboratory of Transducer Technology, Institute of Electronics,Chinese Academy of Sciences, Beijing 100190, China
2. University of Chinese Academy of Sciences, Beijing 100049, China
3. State Key Laboratory of NBC Protection for Civilian, Beijing 102205, China

Received:2016-09-26 Online:2017-04-10 Published:2017-03-23
Contact: QI Zhimei E-mail:zhimei-qi@mail.ie.ac.cn
Supported by:
† Supported by the National Key Basic Research Program of China(No.2015CB352100), the National Natural Science Foundation of China(Nos.61377064, 61675203) and the Research Equipment Development Project of Chinese Academy of Sciences(No;YZ201508)

摘要/Abstract

摘要：

利用波长检测型表面等离子体共振(SPR)传感器对硫堇在金膜表面的电化学聚合成膜过程进行了跟踪分析. 结果表明, 在固定入射角下SPR共振波长随循环伏安扫描周数的增加而线性红移, 表明聚硫堇膜的生长是匀速的; 扫描100周后共振波长红移总量为96.6 nm. 对该实验结果进行理论拟合, 得出聚硫堇膜的厚度约为71 nm. 聚硫堇膜在酸性缓冲液中的电化学活性很高, 其电化学反应过程受扩散控制, 在一个完整的循环伏安扫描过程中SPR共振波长的变化完全可逆, 说明聚硫堇膜的氧化反应和还原反应是一对可逆过程. 与还原态聚硫堇膜相比, 氧化态聚硫堇膜对应的SPR共振波长较大, 说明氧化态聚硫堇膜折射率高.

关键词: 表面等离子体共振, 电化学聚合, 聚硫堇, 共振波长, 动力学分析

Abstract:

The electrochemical polymerization of thionine on gold layer was investigated by using a wavelength-interrogated surface plasmon resonance(SPR) sensor that operates at a fixed angle of incidence. The experimental results show that the resonant wavelength of SPR sensor linearly increases with increasing the number of voltammetry scanning cycles and the total redshift of resonance wavelength is 96.6 nm after 100 scanning cycles. The findings indicate that the film growth rate in every scanning cycle is constant and the poly(thionine) film formed after 100 cycles is ca. 71 nm thick based on the best fit of simulation results to the measured data. The poly(thionine) film in acidic buffer solution exhibits high electrochemical activity and its electrochemical reaction is diffusion-controlled. The resonant wavelength of SPR sensor reversibly changes in a voltammetry scanning cycle, indicating the complete reversibility of electrochemical oxidation-reduction reactions for the poly(thionine) film. Compared with the reduced poly(thionine) film, the oxidization of poly(thionine) film leads to a redshift of resonant wavelength, giving a sign that the refractive index of oxidized poly(thionine) film is higher than that of the reduced one.

Key words: Surface plasmon resonance(SPR), Electrochemical polymerization, Poly(thionine), Wavelength interrogation, Kinetic analysis

中图分类号:

O657

TrendMD:

龚晓庆, 万秀美, 逯丹凤, 高然, 程进, 祁志美. 波长检测型表面等离子体共振传感器对硫堇电聚合成膜的原位分析. 高等学校化学学报, 2017, 38(4): 567.

GONG Xiaoqing, WAN Xiumei, LU Danfeng, GAO Ran, CHENG Jin, QI Zhimei. Studies of Electrochemical Polymerization of Thionine Using a Wavelength-interrogated Surface Plasmon Resonance Sensor^†. Chem. J. Chinese Universities, 2017, 38(4): 567.

图/表 9

Fig.1 Schematic diagram of wavelength-interrogated SPR sensor for in situ analysis of electrochemical process

Fig.2 Cyclic voltammograms during the electropolymerization of thionine on gold electrode with the PBS containing 0.05 mmol/L thionine(A) and SPR spectra recorded before the first voltammogram cycle and after the 100th voltammogram cycle(B)Inset in (A): cyclic voltammograms measured in the range of -0.3—0.9 V under the same conditions above.

Fig.3 SPR spectra at the scan potential of 1.0 V during the growth of poly(thionine) film on gold electrode(A) and resonant wavelengths(λR) as a function of cyclic numbers(B)

Fig.4 SPR spectra calculated at various thickness of poly(thionine) film based on Fresnel equation(A) and linear dependences of λR with thickness of poly(thionine) film(B)

Fig.5 Cyclic voltammogram curves and the resonant wavelengths versus the scan potentials at the first cycle(A), second cycle(B) and fiftieth cycle(C) during the thionine electropolymerization process

Fig.6 Cyclic voltammogram curves at various potential scan rates for the poly(thionine) film coated on the gold electrode(A) and linear dependences of the reduction and oxidation peak currents on the square root of the scan rate(B)

Fig.7 Cyclic voltammograms at the scan rate of 50 mV/s and the corresponding SPR resonance wavelengths versus the scan potentials for the poly(thionine) film coated on the gold electrode(A) and the SPR spectra recorded at the scan potential of 1.0 V with different scan rates(B)

Fig.8 Cyclic voltammograms of the poly(thionine) in PBS at different pH values(A) and the cathodic peak potentials and the corresponding resonant wavelengths versus pH values(B)

Fig.9 Raman spectra for thionine(a) and poly(thionine)(b) films coated on the gold electrodes

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波长检测型表面等离子体共振传感器对硫堇电聚合成膜的原位分析

Studies of Electrochemical Polymerization of Thionine Using a Wavelength-interrogated Surface Plasmon Resonance Sensor^†

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波长检测型表面等离子体共振传感器对硫堇电聚合成膜的原位分析

Studies of Electrochemical Polymerization of Thionine Using a Wavelength-interrogated Surface Plasmon Resonance Sensor†

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Studies of Electrochemical Polymerization of Thionine Using a Wavelength-interrogated Surface Plasmon Resonance Sensor^†