电化学表面增强红外光谱的应用与发展
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摘要
表面电化学是电化学和表面化学相交叉的前沿学科,各种高灵敏度和特异性的现场光谱、扫描微探针和石英微天平等技术的广泛应用推动了表面电化学的发展。电极表面吸附构型解析和燃料电池相关电催化反应机理探索和过程跟踪是表面电化学中的重要研究内容。针对这些问题,现场表面振动光谱发挥着重要作用:它可有效地鉴别电化学催化过程的中问物种,推断电极表面吸附物种的取向和键合等。近年来表面光谱电化学的研究对象从本体光亮电极表面,逐步拓展到具有纳米结构的电极表面。针对这些特殊电极表面的光谱电化学研究,表面增强红外光谱(SEIRAS)与表面增强拉曼光谱(SERS)和反常红外光谱(AIREs)都是重要研究工具。
配以衰减全反射(ATR)模式的ATR-SEIRAS较SERS表面选律简单,便以讨论分子吸附取向;而与外反射AIREs相比ATR-SEIRAS具有表面信号强、传质不受阻和本体溶液干扰小等优点,便于丌展机理和动态过程研究。然而电化学ATR-SEIRAS无论从研究体系和方法本身都存在不足之处,有必要加以发展。
本论文工作首先利用传统ATR-SEIRAS技术研究了芳香小分子在电极表面吸附构型以及CO、有机小分子在电极表面催化反应过程。随后,重点针对传统ATR-SEIRAS技术检测限不够宽的局限性,根据“衰势波穿透”和“平面波棱柱-膜耦合理论”改进了电化学ATR-SEIRAS技术,将高质量频谱检测范围拓宽到700 cm~(-1),实现了甲醇电催化活性中间体的可靠鉴定以及芳香分子吸附构型的详细解析;最后,针对单纯ATR-SEIRAS光谱装置无法检测溶液相反应产物及难于评估金属纳米薄膜的增强效应的弱点,设计了内、外反射可切换的表面红外光谱附件系统。本学位论文主要内容摘要如下:
I-1.异烟酸在Au电极上吸附构型的研究
异烟酸(即4-吡啶羧酸,INA)在不同pH值水溶液中可以不同离子形式存在,从而可提供三种可能与金属表面作用的吸附端:羧酸根、吡啶N原子和芳香环兀键,因此INA是研究金属电极表面吸附构型的理想模型分子。有关碱性溶液中异烟酸分子在Au电极上的吸附构型以及特性吸附离子效应尚不得知。本文应用传统ATR-SEIRAS结合电化学循坏伏安法和微分电容法研究了0.1 mol·L~(-1) KCl0_4和0.1 mol·L~(-1)KCI碱性化溶液(pH 10)中,异烟酸(INA)在Au电极表面的吸附取向和结构。结果表明:-0.5～0.2 V(vs.SCE)问INA阴离子(INA)通过其羧酸根上的两个氧原子垂直吸附在Au电极表面;特性吸附C1-对上述吸附结构无实质影响。表面增强拉曼光谱的测试进一步表明即使在-0.8～-0.5 V,极少量吸附的INA~-很可能仍维持上述基本构型。
1-2.芳香小分子在Ag电极上吸附构型的研究
吡啶和苯甲酸分子是研究金属电极表面吸附构型的理想模型分子,也是SERS研究经典的体系。鉴于SERS选律复杂,我们利用ATR-SEIRAS结合电化学技术研究吡啶和苯甲酸在银电极表面的吸附模式,微分电容测试结果表明在0.1M NaF+10 mM吡啶溶液中,吡啶在-1.0 V(vs.SCE)时丌始吸附,在-0.65 V时吸附达到饱和,随后由于银的部分氧化或者表面氢氧化物的形成,吸附丌始减弱。红外光谱表明,吡啶的吸收峰以A1模式为主,B2模式(定义为面内)极弱,并且992 cm~(-1)(vI)蓝移至1004 cm~(-1)处,这些结果表明吡啶分子通过N端几乎垂直或者轻微倾斜的吸附在银电极表面,与SERS研究结果一致。类似地,微分电容测量结果表明:在0.1 M NaClO_4+10 mM苯甲酸溶液中,苯甲酸在-0.9 V附近发生吸附,在-0.4 v发生相转移变化,随着电位正移,吸附逐渐增强。红外光谱结果表明苯甲酸吸附以A_1模式为主,并且v_s(COO)最强,这些结果表明苯甲酸分子通过羧酸根的两个O原子垂直等位吸附在银电极表面。
1-3.具有催化及SEIRA活性的Pd膜的制备与应用
在甲酸燃料电池中Pd电极对甲酸有着良好的催化活性,为了在分子水平上利用ATR-SEIRAS技术研究Pd电极表面氧化甲酸的反应过程,必须在硅红外窗口反射面上成功制备具有SEIRA效应的Pd薄膜电极。本文改进了用于ATR-SEIRAS技术Si上Pd纳米薄膜的制备方法,即利用“种子生长法”化学镀成功在硅基上制备了具有良好结合力和典型电化学特性的Pd膜电极,其催化稳定性好,表面红外信号强且无反常倒峰和扭曲峰的存在,适合于电催化氧化CO和甲酸等的ATR-SEIRAS研究。另外本文还利用ATR-SEIRAS初步研究了甲酸在Pd表面氧化过程,(Ⅰ)澄清甲酸在Pd表面氧化是否产生CO毒性中间体;(Ⅱ)验证与补充甲酸在Pd表面氧化的“双路径机理”,即是否存在第三种氧化路径。
Ⅱ.实用型宽频检测ATR-SEIRAS装置的研制及应用(论文重点)
目前传统表面增强红外光谱装置中常用的红外窗口是硅、锗和硒化锌柱。硅柱在1000 cm~(-1)。以下有较强的吸收信号,无法给出相应的红外信号;锗和硒化锌在1000 cm~(-1)以下吸收较弱,但是这两种基底表面的金属薄膜主要依靠真空干法制备,更为严重的是锗和硒化锌基底在酸性溶液不稳定,容易造成金属膜在使用过程中的脱落,并且其上金属膜的电化学响应往往偏离本体金属电极的特征,不适于现场光谱电化学的研究。为此,本文根据“衰势波穿透深度原理”和“平面波棱柱一膜耦合理论”,在两个不同折射率的硒化锌柱体和硅片红外窗口间引入超薄水层,研制出一种简单易行的用于电化学内反射ATR-SEIRAS的装置。超薄水层的引入至关重要,大大增加了红外光在硒化锌柱和硅片之间的光通量。以CO和对硝基苯甲酸(PNBA)为探针分子对改进型ATR-SEIRAS装置实验参数进行测试,结果表明该装置以ZnSe/water/Si wafer为红外窗口,70°入射条件下可获得最强的吸附CO信号,并且在1000-700 cm~(-1)区问也可测得高质量的红外光谱;该装置可采用不同的工作电极,可用于动力学采谱,实时监测电极表面吸附物种随电位变化。利用这种改进型ATR-SEIRAS可同时检测到甲酸根对称伸缩振动v_s(COO)和剪式振动δ(OCO),确认铂电极上甲醇氧化活性中间体为吸附甲酸根;根据700-850 cm~(-1)的面外振动(b_1)和1000-1700 cm~(-1)。面内振动(a1和b2)模式谱峰强度,可估算出吸附PNBA分子平面与电极表面之间的二面央角(α),分子平面内旋转前后C2轴之间的夹角(β)以及电极表面法线与分子C2轴之间的央角(γ),从而全面判定电极表面芳香小分子PNBA吸附构型。
Ⅲ.内、外反射模式可切换的表面红外光谱装置的研制及应用
由于单纯的内反射ATR-SEIRAS技术无法检测到溶液中的反应产物,也难于合理评估表面增强红外吸收效应,所以有必要对其进行改进和发展。本文提出一种新型表面红外光谱池设计,利用相同的光路系统和光谱池装置,可实现内、外反射模式之间简便转换。两种光谱技术的联用可提供更多有关反应机理等的信息,利用这种设计按需可检测到在电极上CO_(ad)动态氧化过程,也可检测到溶液相中氧化产物CO_2的信号。也由于两种模式的入射角接近,便于考察ATR红外增强效果。该装置还可为异常红外效应(AIRES)的产生与解释提供实验上的证据,实验结果表明AIRES不仅与金属膜厚度和形貌有关,还很可能与用以制备金属薄膜基底的种类(即基底的反射率差异)有关。
总之,本论文工作是应用现场ATR-SEIRAS对电极表面吸附与电催化若干重要体系作了有益的研究,同时针对该项技术的不足之处作出改进,进一步揭示了ATR-SEIRAS方法是表面电化学、分析化学和纳米科学研究领域中的重要工具。
Surface electrochemistry is the frontier inter-discipline concerned with the interrelation of electrochemistry and surface chemistry,and the development of surface electrochemistry has been promoted by extensive applications of in-situ spectroscopies, scanning probe microscopes and electrochemical quartz crystal microbalance with high sensitivity and unique specificity.Many interesting topics in surface electrochemistry include the determination of adsorption configuration of aromatic compounds on coinage metal electrodes and of the mechanisms associated with electro-catalytic oxidization of small organic molecules on Pt electrode.In-situ surface vibrational spectroscopies play an important role in investigating the above topics.Recent development of surface spectroelectrochemistry calls for an increasing interest in adsorption and reaction on nano-structured electrodes.Along with this trend, surface-enhanced IR absorption spectroscopy(SEIRAS),surface enhanced Raman spectroscopy(SERS) and abnormal IR spectroscopy(AIREs) are deemed as important analytical tools to offer structural information at electrode/electrolyte interfaces.
SEIRAS with the Kretschmann ATR configuration(ATR-SEIRAS) has the merits of simpler surface selection rules as compared to SERS,and thus is convenient for discussing the adsorption configurations of aromatic compounds.In addition,with the advantages of higher surface signals and free problems otherwise caused by the thin-layer electrolyte structure with AIREs,ATR-SEIRAS is preferable for dynamically identifying and monitoring intermediates of irreversible reactions.Nevertheless,there is still a large space to be filled in terms of research systems and technique improvement before ATR-SEIRAS becomes perfect.
In this thesis,firstly traditional ATR-SEIRAS has been applied to reinvestigate the adsorption configuration of typical aromatic molecules at electrodes and the reaction processes of CO as well as small organic molecules on Pd electrodes;Secondly, ATR-SEIRAS with a new optical window is proposed,based on the penetration of evanescent waves and the theory of "prism-film coupler for plane wave" to surmount the frequency detection limit of traditional ATR-SEIRAS.Thirdly,new design in IR optics switchable for internal and external modes on demand is proposed to take full advantage of the two modes.The main results and conclusions are summarized as follows:
Ⅰ-1.Investigation of adsorption configuration of isonicotinic acid on Au electrode
Isonicotinic acid has three possible sites for attaching the electrode surface,viz. -COOH,N atom andπbond,and thus taken as a model molecule for the study of adsorption geometries.ATR-SEIRAS combined with cyclic voltammetry and differential capacitance measurement has been applied to investigate the adsorption configuration of isonicotinate(INA~-) species on Au electrodes in alkalinized 0.1 mol·L~(-1) KClO_4 and 0.1 mol·L~(-1) KCl solutions(pH10).The results indicate that INA~- is nearly vertically adsorbed on the Au surface through the two oxygen atoms of its carboxylate group between -0.4 and 0.2 V(SCE).The presence of Cl~- in supporting electrolyte dose not changes the adsorption configuration of INA~- on Au electrodes. Further supporting information from surface-enhanced Raman spectroscopy suggests that at negative potentials from -0.8 to -0.5 V,INA~- species adsorbed on Au electrode of a very low coverage is likely to remain the nearly same configuration as that revealed at more positive potentials.
Ⅰ-2.Investigation for adsorption configuration of aromatic molecules on Ag electrode surface
Pyridine(Py) and benzoic acid(BA) molecules are the classic model molecules for studying adsorption configuration on metal surface,especially by SERS.Due to complicated nature of SERS surface selection rules,ATR-SEIRAS combined with cyclic voltammetry and differential capacitance measurement has been applied to investigate the adsorption configuration of Py and BA species on Ag electrodes.In the presence of 10 mM pyridine in 0.1 M NaF,the result of capacitance curve measurement suggests that adsorption of Py starts at the potential of ca.-1.0 V,and increases up to -0.65 V and then decreases at higher potentials due to partial oxidation of Ag electrodes.The ATR-SEIRA spectra are dominated with vibrational modes having A_1 symmetry,while those having B_2(in-plane) symmetry are hardly observed.It is noteworthy that spectral features for the adsorbed and the bulk pyridine are different in terms of relative band intensity and position.The totally symmetric ring breathing mode(ν_1) blue-shifts from 992 to 1004 cm~(-1),suggestive of the adsorption via N end. On the basis of the surface selection rule of SEIRAS,the adsorbed pyridine molecules are bound to the Ag electrode with its ring plane perpendicular or slightly tilted to the local surface without significantly rotating its C_2 axis about the surface normal consistent with the conclusion drawn by SERS in the literature.In 0.1 M NaClO_4+10 mM BA,the capacitance curve measurement suggests that BA adsorbs on Ag surface at ca.-0.9 V and undergoes phase transition at ca.-0.4 V.The ATR-SEIRA spectra are dominated by vibrational modes having A_1 symmetry and the intensity ofν_s(OCO) is the most strong,indicating that benzoic acid at positive potentials higher than -0.4 V is bound to the electrode surface through the carboxylate oxygen atoms with a bridging coordination.
Ⅰ-3.Fabrication and application of SEIRA-active Pd film electrode
Pd electrode shows a high catalytic activity toward the oxidation of formic acid in direct formic acid fuel acid(DFAFC).In order to clarify the mechanism for HCOOH oxidation on Pd electrodes by ATR-SEIRAS,it is essential to construct SEIRA-active Pd film electrodes on the basal plane of a Si window.Here,an improved protocol has been proposed for electroless plating of Pd on Si,enabling a strong adhesion between the plated Pd film and the Si substrate,even after repetitive electrochemical cycling in an acid solution.Besides,the Pd film electrode exhibit strong SEIRA effect and with unipolar band shape,laying the basis for reliable peak analysis.The electrochemical measurements manifest that Pd film electrode is excellent for the electro-oxidation of formic acid.Furthermore,preliminary study has been carried out on the electro-oxidation of HCOOH on Pd electrode by employing ATR-SEIRAS,1) to clarify whether poisonous CO_(ad) will be formed for HCOOH oxidation on Pd electrodes; 2) to supplement the so-called "dual pathway" mechanism for HCOOH oxidation on Pd electrode.
Ⅱ.Fabrication and application of practically modified ATR-SEIRAS for high-quality frequency-extended detection of surface species at electrodes
In electrochemical ATR-SEIRAS application,the Si prism is the most frequently used IR window to support the film electrodes owing to its stability in acidic electrolytes,as well as readily available mature and economical wet processes for fabricating various metal electrodes on Si surface.However,a Si prism per se suffers from strong IR absorption in the frequency lower than 1000 cm~(-1),preventing the observation of important spectral fingerprints in this region,hence compromises the structural and mechanistic elucidation at electrodes.Nevertheless,metal film electrodes supported on ZnSe and Ge prisms(having much higher IR transmission in the range of 1000-700 cm~(-1) than Si prism) suffer frequently from abnormal electrochemical responses in wide potential excursions especially in strong acid solutions,due to the instability and dissolution of Ge and ZnSe substrate as well as peeling off metal films.To address this issue,primarily based on "the penetration of evanescent wave" and "the theory of prism-film coupler for plane wave",we present here a practically modified ATR-SEIRAS configuration by sandwiching an ultra-thin water interlayer(submicron thick) between a Si wafer and a ZnSe prism.It is very important to introduce water interlayer in this new ATR optics,which significantly enhances the throughput of effective IR beam across the ZnSe/gap/Si/metal film.This new ATR-SEIRAS with ZnSe/water/Si IR window at incidence angle of 70°can yield the strongest surface IR signal down to 700 cm~(-1).The advantages of this modified ATR-SEIRAS have been initially applied to explore two selected systems: wide-ranged in-situ ATR-SEIRA spectra includingν_s(OCO) andδ(OCO) modes provided strong evidence in support of the formate intermediate pathway for methanol electro-oxidation at Pt electrode in an acid solution.In addition,new spectral fingerprints revealed comprehensive orientational information about of the p-nitrobenzoate species at Pt electrode as a result of the dissociative adsorption of p-nitrobenzoic acid molecules from an acid solution.From the in-plane and out-of-plane vibrations obtained from 700-1700 cm~(-1),three parameters associated with the orientation configuration can be evaluated,including the dihedral angle between the molecular plane and local surface plane,the edge-tilted angle of the molecular plane,and the angle between the symmetry axis of the molecular plane and the local surface normal.
Ⅲ.Design and application of an IR spectral cell switchable for internal and external reflection modes
ATR-SEIRAS alone is unable to identify the products in bulk solution and to evaluate IR enhancement.In this thesis,we design a spectral cell convenient for the switching between internal and external reflection modes,favoring the acquisition of full information regarding both the surface and the solution.This switchable IR spectroscopy can be applied to identify CO adsorption and its subsequent oxidation to CO_2,as well as elucidate the origin of abnormal IR effect(AIRES) experimentally. The results show that the AIRES is not only related to the thickness and structure of the metal overfilm but also to the reflectivity of the substrate.
In summary,conventional ATR-SEIRAS has been applied to investigate the adsorption configuration of prototype molecules on Au and Ag electrodes,as well as the electrocatalytic reaction on Pd and Pt electrodes.We also focus on the improvement of ATR-SEIRAS technique per se for extended detections.The thesis reveals that ATR-SEIRAS is an important analytical tool in surface electrochemistry, analytical chemistry and nanotechnology.This work is expected to contribute to the advancement of electrochemical ATR-SEIRAS.
配以衰减全反射(ATR)模式的ATR-SEIRAS较SERS表面选律简单,便以讨论分子吸附取向;而与外反射AIREs相比ATR-SEIRAS具有表面信号强、传质不受阻和本体溶液干扰小等优点,便于丌展机理和动态过程研究。然而电化学ATR-SEIRAS无论从研究体系和方法本身都存在不足之处,有必要加以发展。
本论文工作首先利用传统ATR-SEIRAS技术研究了芳香小分子在电极表面吸附构型以及CO、有机小分子在电极表面催化反应过程。随后,重点针对传统ATR-SEIRAS技术检测限不够宽的局限性,根据“衰势波穿透”和“平面波棱柱-膜耦合理论”改进了电化学ATR-SEIRAS技术,将高质量频谱检测范围拓宽到700 cm~(-1),实现了甲醇电催化活性中间体的可靠鉴定以及芳香分子吸附构型的详细解析;最后,针对单纯ATR-SEIRAS光谱装置无法检测溶液相反应产物及难于评估金属纳米薄膜的增强效应的弱点,设计了内、外反射可切换的表面红外光谱附件系统。本学位论文主要内容摘要如下:
I-1.异烟酸在Au电极上吸附构型的研究
异烟酸(即4-吡啶羧酸,INA)在不同pH值水溶液中可以不同离子形式存在,从而可提供三种可能与金属表面作用的吸附端:羧酸根、吡啶N原子和芳香环兀键,因此INA是研究金属电极表面吸附构型的理想模型分子。有关碱性溶液中异烟酸分子在Au电极上的吸附构型以及特性吸附离子效应尚不得知。本文应用传统ATR-SEIRAS结合电化学循坏伏安法和微分电容法研究了0.1 mol·L~(-1) KCl0_4和0.1 mol·L~(-1)KCI碱性化溶液(pH 10)中,异烟酸(INA)在Au电极表面的吸附取向和结构。结果表明:-0.5～0.2 V(vs.SCE)问INA阴离子(INA)通过其羧酸根上的两个氧原子垂直吸附在Au电极表面;特性吸附C1-对上述吸附结构无实质影响。表面增强拉曼光谱的测试进一步表明即使在-0.8～-0.5 V,极少量吸附的INA~-很可能仍维持上述基本构型。
1-2.芳香小分子在Ag电极上吸附构型的研究
吡啶和苯甲酸分子是研究金属电极表面吸附构型的理想模型分子,也是SERS研究经典的体系。鉴于SERS选律复杂,我们利用ATR-SEIRAS结合电化学技术研究吡啶和苯甲酸在银电极表面的吸附模式,微分电容测试结果表明在0.1M NaF+10 mM吡啶溶液中,吡啶在-1.0 V(vs.SCE)时丌始吸附,在-0.65 V时吸附达到饱和,随后由于银的部分氧化或者表面氢氧化物的形成,吸附丌始减弱。红外光谱表明,吡啶的吸收峰以A1模式为主,B2模式(定义为面内)极弱,并且992 cm~(-1)(vI)蓝移至1004 cm~(-1)处,这些结果表明吡啶分子通过N端几乎垂直或者轻微倾斜的吸附在银电极表面,与SERS研究结果一致。类似地,微分电容测量结果表明:在0.1 M NaClO_4+10 mM苯甲酸溶液中,苯甲酸在-0.9 V附近发生吸附,在-0.4 v发生相转移变化,随着电位正移,吸附逐渐增强。红外光谱结果表明苯甲酸吸附以A_1模式为主,并且v_s(COO)最强,这些结果表明苯甲酸分子通过羧酸根的两个O原子垂直等位吸附在银电极表面。
1-3.具有催化及SEIRA活性的Pd膜的制备与应用
在甲酸燃料电池中Pd电极对甲酸有着良好的催化活性,为了在分子水平上利用ATR-SEIRAS技术研究Pd电极表面氧化甲酸的反应过程,必须在硅红外窗口反射面上成功制备具有SEIRA效应的Pd薄膜电极。本文改进了用于ATR-SEIRAS技术Si上Pd纳米薄膜的制备方法,即利用“种子生长法”化学镀成功在硅基上制备了具有良好结合力和典型电化学特性的Pd膜电极,其催化稳定性好,表面红外信号强且无反常倒峰和扭曲峰的存在,适合于电催化氧化CO和甲酸等的ATR-SEIRAS研究。另外本文还利用ATR-SEIRAS初步研究了甲酸在Pd表面氧化过程,(Ⅰ)澄清甲酸在Pd表面氧化是否产生CO毒性中间体;(Ⅱ)验证与补充甲酸在Pd表面氧化的“双路径机理”,即是否存在第三种氧化路径。
Ⅱ.实用型宽频检测ATR-SEIRAS装置的研制及应用(论文重点)
目前传统表面增强红外光谱装置中常用的红外窗口是硅、锗和硒化锌柱。硅柱在1000 cm~(-1)。以下有较强的吸收信号,无法给出相应的红外信号;锗和硒化锌在1000 cm~(-1)以下吸收较弱,但是这两种基底表面的金属薄膜主要依靠真空干法制备,更为严重的是锗和硒化锌基底在酸性溶液不稳定,容易造成金属膜在使用过程中的脱落,并且其上金属膜的电化学响应往往偏离本体金属电极的特征,不适于现场光谱电化学的研究。为此,本文根据“衰势波穿透深度原理”和“平面波棱柱一膜耦合理论”,在两个不同折射率的硒化锌柱体和硅片红外窗口间引入超薄水层,研制出一种简单易行的用于电化学内反射ATR-SEIRAS的装置。超薄水层的引入至关重要,大大增加了红外光在硒化锌柱和硅片之间的光通量。以CO和对硝基苯甲酸(PNBA)为探针分子对改进型ATR-SEIRAS装置实验参数进行测试,结果表明该装置以ZnSe/water/Si wafer为红外窗口,70°入射条件下可获得最强的吸附CO信号,并且在1000-700 cm~(-1)区问也可测得高质量的红外光谱;该装置可采用不同的工作电极,可用于动力学采谱,实时监测电极表面吸附物种随电位变化。利用这种改进型ATR-SEIRAS可同时检测到甲酸根对称伸缩振动v_s(COO)和剪式振动δ(OCO),确认铂电极上甲醇氧化活性中间体为吸附甲酸根;根据700-850 cm~(-1)的面外振动(b_1)和1000-1700 cm~(-1)。面内振动(a1和b2)模式谱峰强度,可估算出吸附PNBA分子平面与电极表面之间的二面央角(α),分子平面内旋转前后C2轴之间的夹角(β)以及电极表面法线与分子C2轴之间的央角(γ),从而全面判定电极表面芳香小分子PNBA吸附构型。
Ⅲ.内、外反射模式可切换的表面红外光谱装置的研制及应用
由于单纯的内反射ATR-SEIRAS技术无法检测到溶液中的反应产物,也难于合理评估表面增强红外吸收效应,所以有必要对其进行改进和发展。本文提出一种新型表面红外光谱池设计,利用相同的光路系统和光谱池装置,可实现内、外反射模式之间简便转换。两种光谱技术的联用可提供更多有关反应机理等的信息,利用这种设计按需可检测到在电极上CO_(ad)动态氧化过程,也可检测到溶液相中氧化产物CO_2的信号。也由于两种模式的入射角接近,便于考察ATR红外增强效果。该装置还可为异常红外效应(AIRES)的产生与解释提供实验上的证据,实验结果表明AIRES不仅与金属膜厚度和形貌有关,还很可能与用以制备金属薄膜基底的种类(即基底的反射率差异)有关。
总之,本论文工作是应用现场ATR-SEIRAS对电极表面吸附与电催化若干重要体系作了有益的研究,同时针对该项技术的不足之处作出改进,进一步揭示了ATR-SEIRAS方法是表面电化学、分析化学和纳米科学研究领域中的重要工具。
Surface electrochemistry is the frontier inter-discipline concerned with the interrelation of electrochemistry and surface chemistry,and the development of surface electrochemistry has been promoted by extensive applications of in-situ spectroscopies, scanning probe microscopes and electrochemical quartz crystal microbalance with high sensitivity and unique specificity.Many interesting topics in surface electrochemistry include the determination of adsorption configuration of aromatic compounds on coinage metal electrodes and of the mechanisms associated with electro-catalytic oxidization of small organic molecules on Pt electrode.In-situ surface vibrational spectroscopies play an important role in investigating the above topics.Recent development of surface spectroelectrochemistry calls for an increasing interest in adsorption and reaction on nano-structured electrodes.Along with this trend, surface-enhanced IR absorption spectroscopy(SEIRAS),surface enhanced Raman spectroscopy(SERS) and abnormal IR spectroscopy(AIREs) are deemed as important analytical tools to offer structural information at electrode/electrolyte interfaces.
SEIRAS with the Kretschmann ATR configuration(ATR-SEIRAS) has the merits of simpler surface selection rules as compared to SERS,and thus is convenient for discussing the adsorption configurations of aromatic compounds.In addition,with the advantages of higher surface signals and free problems otherwise caused by the thin-layer electrolyte structure with AIREs,ATR-SEIRAS is preferable for dynamically identifying and monitoring intermediates of irreversible reactions.Nevertheless,there is still a large space to be filled in terms of research systems and technique improvement before ATR-SEIRAS becomes perfect.
In this thesis,firstly traditional ATR-SEIRAS has been applied to reinvestigate the adsorption configuration of typical aromatic molecules at electrodes and the reaction processes of CO as well as small organic molecules on Pd electrodes;Secondly, ATR-SEIRAS with a new optical window is proposed,based on the penetration of evanescent waves and the theory of "prism-film coupler for plane wave" to surmount the frequency detection limit of traditional ATR-SEIRAS.Thirdly,new design in IR optics switchable for internal and external modes on demand is proposed to take full advantage of the two modes.The main results and conclusions are summarized as follows:
Ⅰ-1.Investigation of adsorption configuration of isonicotinic acid on Au electrode
Isonicotinic acid has three possible sites for attaching the electrode surface,viz. -COOH,N atom andπbond,and thus taken as a model molecule for the study of adsorption geometries.ATR-SEIRAS combined with cyclic voltammetry and differential capacitance measurement has been applied to investigate the adsorption configuration of isonicotinate(INA~-) species on Au electrodes in alkalinized 0.1 mol·L~(-1) KClO_4 and 0.1 mol·L~(-1) KCl solutions(pH10).The results indicate that INA~- is nearly vertically adsorbed on the Au surface through the two oxygen atoms of its carboxylate group between -0.4 and 0.2 V(SCE).The presence of Cl~- in supporting electrolyte dose not changes the adsorption configuration of INA~- on Au electrodes. Further supporting information from surface-enhanced Raman spectroscopy suggests that at negative potentials from -0.8 to -0.5 V,INA~- species adsorbed on Au electrode of a very low coverage is likely to remain the nearly same configuration as that revealed at more positive potentials.
Ⅰ-2.Investigation for adsorption configuration of aromatic molecules on Ag electrode surface
Pyridine(Py) and benzoic acid(BA) molecules are the classic model molecules for studying adsorption configuration on metal surface,especially by SERS.Due to complicated nature of SERS surface selection rules,ATR-SEIRAS combined with cyclic voltammetry and differential capacitance measurement has been applied to investigate the adsorption configuration of Py and BA species on Ag electrodes.In the presence of 10 mM pyridine in 0.1 M NaF,the result of capacitance curve measurement suggests that adsorption of Py starts at the potential of ca.-1.0 V,and increases up to -0.65 V and then decreases at higher potentials due to partial oxidation of Ag electrodes.The ATR-SEIRA spectra are dominated with vibrational modes having A_1 symmetry,while those having B_2(in-plane) symmetry are hardly observed.It is noteworthy that spectral features for the adsorbed and the bulk pyridine are different in terms of relative band intensity and position.The totally symmetric ring breathing mode(ν_1) blue-shifts from 992 to 1004 cm~(-1),suggestive of the adsorption via N end. On the basis of the surface selection rule of SEIRAS,the adsorbed pyridine molecules are bound to the Ag electrode with its ring plane perpendicular or slightly tilted to the local surface without significantly rotating its C_2 axis about the surface normal consistent with the conclusion drawn by SERS in the literature.In 0.1 M NaClO_4+10 mM BA,the capacitance curve measurement suggests that BA adsorbs on Ag surface at ca.-0.9 V and undergoes phase transition at ca.-0.4 V.The ATR-SEIRA spectra are dominated by vibrational modes having A_1 symmetry and the intensity ofν_s(OCO) is the most strong,indicating that benzoic acid at positive potentials higher than -0.4 V is bound to the electrode surface through the carboxylate oxygen atoms with a bridging coordination.
Ⅰ-3.Fabrication and application of SEIRA-active Pd film electrode
Pd electrode shows a high catalytic activity toward the oxidation of formic acid in direct formic acid fuel acid(DFAFC).In order to clarify the mechanism for HCOOH oxidation on Pd electrodes by ATR-SEIRAS,it is essential to construct SEIRA-active Pd film electrodes on the basal plane of a Si window.Here,an improved protocol has been proposed for electroless plating of Pd on Si,enabling a strong adhesion between the plated Pd film and the Si substrate,even after repetitive electrochemical cycling in an acid solution.Besides,the Pd film electrode exhibit strong SEIRA effect and with unipolar band shape,laying the basis for reliable peak analysis.The electrochemical measurements manifest that Pd film electrode is excellent for the electro-oxidation of formic acid.Furthermore,preliminary study has been carried out on the electro-oxidation of HCOOH on Pd electrode by employing ATR-SEIRAS,1) to clarify whether poisonous CO_(ad) will be formed for HCOOH oxidation on Pd electrodes; 2) to supplement the so-called "dual pathway" mechanism for HCOOH oxidation on Pd electrode.
Ⅱ.Fabrication and application of practically modified ATR-SEIRAS for high-quality frequency-extended detection of surface species at electrodes
In electrochemical ATR-SEIRAS application,the Si prism is the most frequently used IR window to support the film electrodes owing to its stability in acidic electrolytes,as well as readily available mature and economical wet processes for fabricating various metal electrodes on Si surface.However,a Si prism per se suffers from strong IR absorption in the frequency lower than 1000 cm~(-1),preventing the observation of important spectral fingerprints in this region,hence compromises the structural and mechanistic elucidation at electrodes.Nevertheless,metal film electrodes supported on ZnSe and Ge prisms(having much higher IR transmission in the range of 1000-700 cm~(-1) than Si prism) suffer frequently from abnormal electrochemical responses in wide potential excursions especially in strong acid solutions,due to the instability and dissolution of Ge and ZnSe substrate as well as peeling off metal films.To address this issue,primarily based on "the penetration of evanescent wave" and "the theory of prism-film coupler for plane wave",we present here a practically modified ATR-SEIRAS configuration by sandwiching an ultra-thin water interlayer(submicron thick) between a Si wafer and a ZnSe prism.It is very important to introduce water interlayer in this new ATR optics,which significantly enhances the throughput of effective IR beam across the ZnSe/gap/Si/metal film.This new ATR-SEIRAS with ZnSe/water/Si IR window at incidence angle of 70°can yield the strongest surface IR signal down to 700 cm~(-1).The advantages of this modified ATR-SEIRAS have been initially applied to explore two selected systems: wide-ranged in-situ ATR-SEIRA spectra includingν_s(OCO) andδ(OCO) modes provided strong evidence in support of the formate intermediate pathway for methanol electro-oxidation at Pt electrode in an acid solution.In addition,new spectral fingerprints revealed comprehensive orientational information about of the p-nitrobenzoate species at Pt electrode as a result of the dissociative adsorption of p-nitrobenzoic acid molecules from an acid solution.From the in-plane and out-of-plane vibrations obtained from 700-1700 cm~(-1),three parameters associated with the orientation configuration can be evaluated,including the dihedral angle between the molecular plane and local surface plane,the edge-tilted angle of the molecular plane,and the angle between the symmetry axis of the molecular plane and the local surface normal.
Ⅲ.Design and application of an IR spectral cell switchable for internal and external reflection modes
ATR-SEIRAS alone is unable to identify the products in bulk solution and to evaluate IR enhancement.In this thesis,we design a spectral cell convenient for the switching between internal and external reflection modes,favoring the acquisition of full information regarding both the surface and the solution.This switchable IR spectroscopy can be applied to identify CO adsorption and its subsequent oxidation to CO_2,as well as elucidate the origin of abnormal IR effect(AIRES) experimentally. The results show that the AIRES is not only related to the thickness and structure of the metal overfilm but also to the reflectivity of the substrate.
In summary,conventional ATR-SEIRAS has been applied to investigate the adsorption configuration of prototype molecules on Au and Ag electrodes,as well as the electrocatalytic reaction on Pd and Pt electrodes.We also focus on the improvement of ATR-SEIRAS technique per se for extended detections.The thesis reveals that ATR-SEIRAS is an important analytical tool in surface electrochemistry, analytical chemistry and nanotechnology.This work is expected to contribute to the advancement of electrochemical ATR-SEIRAS.
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