离子液体/金属电极界面结构的现场电化学SERS研究
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摘要
室温离子液体作为一种新型非水溶剂，具有宽的电化学窗口、低的蒸汽压以及良好导电性等特点，已被广泛用于电化学领域。由于离子液体提供了一种完全不同于传统水溶液和有机溶剂的离子环境，“离子液体/金属电极”界面的性质及结构与以往研究的体系存在一定差别，为此研究“离子液体/金属电极”界面结构对于拓宽其应用范围具有重要的理论意义。
本文将具有高灵敏度的表面增强拉曼光谱（SERS）与电化学技术结合，通过关联离子液体中离子或分子的光谱与电化学控制的关系，从分子水平上解析“离子液体/金属”界面结构、性质，为“离子液体/金属电极”界面新理论的建立提供依据，主要研究内容和结果如下：
1、发展适合离子液体/金属电极体系的电化学SERS技术，以4-氰基吡啶（4-CNPy）为探针，并结合SERS的表面选律、电化学Stark效应等手段，研究其在离子液体中Pt、Au电极表面上的吸附行为。研究结果表明，较正电位下4-CNPy通过吡啶环上的氮原子与电极表面作用；较负电位下，咪唑阳离子以倾斜甚至平躺方式吸附在电极表面，4-CNPy则以平躺方式吸附在电极表面。相对于水溶液体系，离子液体中氰基伸缩振动谱峰的电化学Stark系数较小，主要由于“离子液体/金属”界面极高的离子强度及咪唑阳离子的共吸附。
2、考察[BMIM]BF4离子液体中[BMIM]SCN在Au电极表面的吸附及水对界面结构的影响。结果表明，离子液体中SCN-在较宽的电位范围内吸附在Au电极上，在-0.4V~-0.8V区间内，以S端吸附为主；而在-0.8V~-2.0V区间内，以N端吸附为主。在离子液体中加入水后， C≡N的Stark位移明显增大，且咪唑阳离子的吸附情况发生显著变化。说明水分子进入到离子液体/电极界面双电层中，影响阴阳离子排布。
3、探索[BMIM]BF4中CO在Pt电极表面的吸附行为并研究含水浓度变化的影响，采用循环伏安法研究了水的加入对离子液体界面结构和CO在Pt电极上的电化学性质影响。由于水的存在为CO氧化和Pt电极氧化提供氧源，水含量越多，氧化峰电位负移，CO的氧化反应更易发生。水的引入还使CO在Pt电极上[BMIM]BF4中的吸附方式多样化，同时存在线性吸附和桥式吸附，并导致COL的Stark位移较纯[BMIM]BF4增大。
4、初步研究了采用恒电位技术在[BMIM]BF4离子液体中获得不同组成和形貌的铜沉积物，考察了表面沉积层组成及结构与沉积电位的关系，并以吡啶为探针分子，研究了沉积膜的SERS效应、催化活性以及SERS信号的均匀性。
As a non-aqueous solvent, room temperature ionic liquids (RTILs) have distinctadvantages, such as wide electrochemical window, vanishingly low vapor pressure, highconductivity, and other designable physical and chemical properties. RTILs have beenwidely used in various fields including electrochemistry. RTILs are composed pure ionsin the liquid state, which is different from the traditional aqueous or organic solvents.Therefore，deeper insight to the interfacial structure of “RTILs/metal electrode” is highdesired because it is beyond the description of classical electrochemical theory for thedilute aqueous electrolyte/metal electrode system. The investigation of the interfacialstructure of RTILs/metal electrode is beneficial to extend the application of RTILs.
The high sensitive surface enhanced Raman spectroscopy (SERS) combined withelectrochemical methods provides a powerful tool for probing the adsorption of chemicalspecies and RTILs themselves. The information of the surface structure, properties, andadsorption behavior can be probed at the molecular level. The main results are outlinedas follows:
1. To develop the proper electrochemical SERS technique for exploring of RTILs/metalelectrode system. By using4-cyanopyridines (4-CNPy) as probe, its adsorption behaviorwas resolved based at Pt or Au electrode based on SERS surface selection rules andelectrochemical Stark effect. The results showed that4-CNPy bounded to the Au surfacethrough the N atom of the Py ring in the slightly negative potential region. While in themore negative potential region, the4-CNPy molecules lay flat on the surface whichresulted in the decrease of surface coverage. In addition, a relative low Stark tuning ratein ionic liquid was measured by comparison to the aqueous systems. It was originatedfrom the unique RTILs/Au interfacial structure and the coadsorption of RTILs and 4-CNPy.
2. In situ SERS investigation on adsorption behavior of [BMIM]SCN at [BMIM]BF4/Auelectrode was performed. It was found that [BMIM]SCN adsorbed on the Au surfacewithin a wide potential region. In the potential range of-0.4V to-0.8V, SCN-wasadsorbed mainly through S atom onto the Au electrode while in the range of-0.8V to-2.0V, it was oriented mainly through N atom. The effect of water on the reorientation ofionic liquids and SCN-was investigated. In this case, the increase of Stark tuning ratewas measured. The results showed that water may penetrate into the double layer of[BMIM]BF4/Au interface to affect the distribution of cation and anions.
3. In the system of “[BMIM]BF4/Pt”, the electrochemical properties of CO and interfacestructure are studied through cyclic voltammetry with the change in the concentration ofwater. The onset potential of the CO oxidation negatively shifted with the increase of thewater concentration, suggesting that CO was oxidized more easily in [BMIM]BF4ionicliquid by the adding water, which acted as the source of oxygen atom. In addition, theintroduction of water resulted in the multi-adsorption configuration of CO, i.e. thecoexistence of linear and bridge adsorption. The increase of water concentrationmagnified the Stark tuning rate of CO in [BMIM]BF4solution
4. The electrodeposition of Cu layer was preliminary investigated in [BMIM]BF4on ITOelectrodes by constant potential method. The composition and surface morphology of thedeposition layers were characterized, indicating that they were strongly depended on theapplied potentials. With negative movement of applied potential, the catalytic activity ofthe deposition layers in the reduction of p-nitrophenol to p-aminophenol increased. Byusing pyridine as probe, the SERS performance of the deposited layer was studied. Theresults revealed that the Cu film deposited at appropriate potential exhibited high SERSactivity and uniformity, which would be become a potential SERS substrate.
本文将具有高灵敏度的表面增强拉曼光谱（SERS）与电化学技术结合，通过关联离子液体中离子或分子的光谱与电化学控制的关系，从分子水平上解析“离子液体/金属”界面结构、性质，为“离子液体/金属电极”界面新理论的建立提供依据，主要研究内容和结果如下：
1、发展适合离子液体/金属电极体系的电化学SERS技术，以4-氰基吡啶（4-CNPy）为探针，并结合SERS的表面选律、电化学Stark效应等手段，研究其在离子液体中Pt、Au电极表面上的吸附行为。研究结果表明，较正电位下4-CNPy通过吡啶环上的氮原子与电极表面作用；较负电位下，咪唑阳离子以倾斜甚至平躺方式吸附在电极表面，4-CNPy则以平躺方式吸附在电极表面。相对于水溶液体系，离子液体中氰基伸缩振动谱峰的电化学Stark系数较小，主要由于“离子液体/金属”界面极高的离子强度及咪唑阳离子的共吸附。
2、考察[BMIM]BF4离子液体中[BMIM]SCN在Au电极表面的吸附及水对界面结构的影响。结果表明，离子液体中SCN-在较宽的电位范围内吸附在Au电极上，在-0.4V~-0.8V区间内，以S端吸附为主；而在-0.8V~-2.0V区间内，以N端吸附为主。在离子液体中加入水后， C≡N的Stark位移明显增大，且咪唑阳离子的吸附情况发生显著变化。说明水分子进入到离子液体/电极界面双电层中，影响阴阳离子排布。
3、探索[BMIM]BF4中CO在Pt电极表面的吸附行为并研究含水浓度变化的影响，采用循环伏安法研究了水的加入对离子液体界面结构和CO在Pt电极上的电化学性质影响。由于水的存在为CO氧化和Pt电极氧化提供氧源，水含量越多，氧化峰电位负移，CO的氧化反应更易发生。水的引入还使CO在Pt电极上[BMIM]BF4中的吸附方式多样化，同时存在线性吸附和桥式吸附，并导致COL的Stark位移较纯[BMIM]BF4增大。
4、初步研究了采用恒电位技术在[BMIM]BF4离子液体中获得不同组成和形貌的铜沉积物，考察了表面沉积层组成及结构与沉积电位的关系，并以吡啶为探针分子，研究了沉积膜的SERS效应、催化活性以及SERS信号的均匀性。
As a non-aqueous solvent, room temperature ionic liquids (RTILs) have distinctadvantages, such as wide electrochemical window, vanishingly low vapor pressure, highconductivity, and other designable physical and chemical properties. RTILs have beenwidely used in various fields including electrochemistry. RTILs are composed pure ionsin the liquid state, which is different from the traditional aqueous or organic solvents.Therefore，deeper insight to the interfacial structure of “RTILs/metal electrode” is highdesired because it is beyond the description of classical electrochemical theory for thedilute aqueous electrolyte/metal electrode system. The investigation of the interfacialstructure of RTILs/metal electrode is beneficial to extend the application of RTILs.
The high sensitive surface enhanced Raman spectroscopy (SERS) combined withelectrochemical methods provides a powerful tool for probing the adsorption of chemicalspecies and RTILs themselves. The information of the surface structure, properties, andadsorption behavior can be probed at the molecular level. The main results are outlinedas follows:
1. To develop the proper electrochemical SERS technique for exploring of RTILs/metalelectrode system. By using4-cyanopyridines (4-CNPy) as probe, its adsorption behaviorwas resolved based at Pt or Au electrode based on SERS surface selection rules andelectrochemical Stark effect. The results showed that4-CNPy bounded to the Au surfacethrough the N atom of the Py ring in the slightly negative potential region. While in themore negative potential region, the4-CNPy molecules lay flat on the surface whichresulted in the decrease of surface coverage. In addition, a relative low Stark tuning ratein ionic liquid was measured by comparison to the aqueous systems. It was originatedfrom the unique RTILs/Au interfacial structure and the coadsorption of RTILs and 4-CNPy.
2. In situ SERS investigation on adsorption behavior of [BMIM]SCN at [BMIM]BF4/Auelectrode was performed. It was found that [BMIM]SCN adsorbed on the Au surfacewithin a wide potential region. In the potential range of-0.4V to-0.8V, SCN-wasadsorbed mainly through S atom onto the Au electrode while in the range of-0.8V to-2.0V, it was oriented mainly through N atom. The effect of water on the reorientation ofionic liquids and SCN-was investigated. In this case, the increase of Stark tuning ratewas measured. The results showed that water may penetrate into the double layer of[BMIM]BF4/Au interface to affect the distribution of cation and anions.
3. In the system of “[BMIM]BF4/Pt”, the electrochemical properties of CO and interfacestructure are studied through cyclic voltammetry with the change in the concentration ofwater. The onset potential of the CO oxidation negatively shifted with the increase of thewater concentration, suggesting that CO was oxidized more easily in [BMIM]BF4ionicliquid by the adding water, which acted as the source of oxygen atom. In addition, theintroduction of water resulted in the multi-adsorption configuration of CO, i.e. thecoexistence of linear and bridge adsorption. The increase of water concentrationmagnified the Stark tuning rate of CO in [BMIM]BF4solution
4. The electrodeposition of Cu layer was preliminary investigated in [BMIM]BF4on ITOelectrodes by constant potential method. The composition and surface morphology of thedeposition layers were characterized, indicating that they were strongly depended on theapplied potentials. With negative movement of applied potential, the catalytic activity ofthe deposition layers in the reduction of p-nitrophenol to p-aminophenol increased. Byusing pyridine as probe, the SERS performance of the deposited layer was studied. Theresults revealed that the Cu film deposited at appropriate potential exhibited high SERSactivity and uniformity, which would be become a potential SERS substrate.
引文
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