电化学原位红外光谱研究铂电极上有机小分子吸附和氧化的反应机理和动力学
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摘要
直接甲醇燃料电池(即Direct Methanol Fuel Cell,简称为DMFC)被认为是解决能源紧缺和环境问题的重要方案之一。它具有启动速度快,操作温度低、燃料来源广和环境污染小等许多优点,十分适合在日常的生产生活中广泛应用。DMFC的大规模商业化面临两个问题。一是,甲醇氧化反应中生成的中间物CO在阳极催化剂上有很强的吸附作用,造成电流密度减小和输出电压降低等问题；二是,目前应用最广泛的商业催化剂是铂(Pt)基催化剂。作为地球上贮量有限的重要贵金属Pt,它的可用量十分有限,不仅制约了直接甲醇燃料电池的产量,使之难以大规模推广使用,而且还使得DMFC的价格居高不下。从分子水平上揭示甲醇反应的机理以及各因素对其反应动力学的影响是设计高效、低Pt担载的甲醇氧化电催化剂的前提。
本实验室发展了电化学衰减全内反射红外光谱与流动电解池联用技术,可以在排除传质条件影响下,系统地研究干净Pt电极上电化学反应最初阶段的反应机理和反应动力学,并探讨电位、PH值和电极表面组成等对反应的影响。结合本实验室的优势条件并且针对目前DMFC中的难题,本博士论文主要研究甲醇、一氧化碳(CO)和氰根(CN-)在Pt或者PtRu电极上吸附和氧化的反应机制和动力学过程。
各个部分的主要内容和结论总结如下：1.甲醇在Pt电极上的氧化反应
利用电化学原位ATR-FTIR与排除传质影响的流动电解池联用技术,研究在Pt电极上各个不同的恒电位时0.1MHC104+2M CH3OH甲醇的氧化反应过程。结合CO吸附的红外光谱和氧化电量,计算CO的表面覆盖度,进而定量分析在一系列不同的CO覆盖度下甲醇氧化的反应途径的电流效率和Tafel斜率对应的决速步骤。结果表明：(i)在恒电位下,随着COad在电极表面的堆积并达到最大的覆盖度0.5单层的过程中,甲醇脱氢反应速率随之降低而COad氧化速率随之增加;(ii)在固定的COad覆盖度下,甲醇分解生成COad速率和COad氧化速率在0.3V到0.7V(vs.RHE)之间随着电势的增加而增加,甲醇脱氢的Tafel斜率大约是440±30mV/dec,而且不随COad覆盖度改变而改变。(iii)在0.6和0.7V时甲醇氧化反应中CO反应途径的电流效率在20%以下,而且随着电势的升高而降低。甲醇氧化反应的机制和电极电势变化引起的不同反应途径的动力学的变化也有简要的讨论。
2.氰根(Cyanide)和CO在Pt电极上的吸附
利用衰减全内反射电化学原位红外光谱与薄层流动电解池联用技术研究在0.1MHC104+0.01M KCN体系中CN-在Pt膜电极表面的吸附的电位效应和动力学过程。首次在酸性电解质体系中研究CN-在Pt电极上的吸附过程,并发挥流动电解池可以持续控制电位和快速切换的优势,在CN-吸附饱和的Pt表面引入C0,探讨在一系列电位下两种分子吸附时的相互作用。从时间分辨红外光谱的数据结果可以推测出：随着吸附时电极电势的改变,CN-在Pt电极上的吸附构型表现出三种不同的伸缩振动。在0.05V,1639cm-1和1493cm-1的峰,归属于trans-(HN=CH)表面物种。2100cm-1左右的峰,归属于N-端吸附的Pt-NC,在2150cm-1的峰,归属于C-端吸附的Pt-CN,而Pt-NC的Stark斜率是Pt-CN的3倍多。CNad在电极表面上吸附的构型朝向的识别可以通过在饱和CN吸附的Pt电极上引入CO共吸附的红外光谱的行为进一步得到证实。引入CO后可以发现对Pt-NC和Pt-CN两种构型的红外光谱有不同的影响：Pt-NC的C-N伸缩振动峰频发生了蓝移但峰强并没有明显变化;而Pt-CN的峰强有明显的增大,但频率却没有发生变化。C-N振动峰的变化揭示了在Pt电极表面上CN-最初的吸附构型是Pt-NCHad。然后,它氧化成了Pt-NC,随着反应时间的增加慢慢地改变成Pt-CN。基于DFT理论计算的结果发现,偶极耦合效应,空间挤压作用和电子效应可以用来解释CN-及其与CO共吸附的红外光谱变化的电极电势效应。
3.甲醇在PtRu电极上的氧化反应
利用电化学-ATR-FTIR技术研究了纯Pt与PtxRu,电极上甲醇氧化反应的动力学和反应机理。利用流动电解池切换到Ru溶液中沉积不同时间后,再切换回支持电解质清洗电解池,可以很方便地构建一系列不同覆盖度的PtxRuy电极。Ru沉积在Pt电极表面后,明显抑制了欠电位沉积H的吸脱附反应,因此通过计算沉积Ru前后的欠电位沉积H吸脱附反应的总电量可得到Ru在Pt电极表面上的覆盖度。引入Ru后,Pt电极的催化活性有明显提高。PtxRuy电极上甲醇氧化反应活性与Ru的覆盖度呈火山型曲线,实验表明Pt61Ru39电极的催化活性最好。在高覆盖度下,当Ru覆盖度超过39%时,CO会吸附在Ru上使得PtxRu,电极的活性降低。在低覆盖度下,由于Ru与Pt相互作用促进了甲醇脱氢反应,使得Pt上CO密度增大。Pt61Ru39电极上一系列不同电位(0.3V、0.4V、0.5V和0.6V)的甲醇氧化实验,表明甲醇脱氢生成CO和CO氧化的反应途径在总反应电流中的贡献有明显的电位效应。将甲醇在纯Pt电极和Pt61Ru39电极上的氧化反应进行比较,可以发现在低电位下Ru对Pt电极的氧化活性的促进效应比在高电位下明显得多。
Direct Methanol Fuel Cell (DMFC) has been seen as one of the solutions to the worldwide energy shortage and environmental protection problems. DMFC has plenty of adventages such as rapid starting speed, facile operating temperature, wide fuel source and little pollution. It is very propitious for DMFC to be largely used in socical life and industrial production. There are two problems which restrict the large-scale commercialization of DMFC. Firstly, the reaction intermediate CO from methanol oxidation reaction displays a strong adsorption at Pt-based anodic catalyst, which leads to the decrease of current density and output voltage; Secondly, at present the most worldwide DMFC catalyst is Pt-based materials. As an important expensive metal with a finite storage in planet, the Pt not only restricts the productivity of DMFC but also raises the price. Demonstrating the reaction mechanism and the influence on the dynamics from all kinds of factors in molecular level is the premise of designing DMFC anodic electrocatalyst with high performance and low Pt load.
Electrochemical in situ ATR-FRIT spectroscopy with flow cell technique devoloped in our lab, allows the systematic research of initial reaction mechanism and dynamics of electrochemical reaction at clean Pt electrode without the influence of mass tranfer, and then to probe potential, PH and electrode compostion effects on the reaction. Aiming the current DMFC problems and combining the advantage in our lab, this thesis focuses on the research on the reaction mechanism and dynamic process of methanol, carbon monoxide and cyanide adsorption and oxidation at Pt or PtRu electrode.
The main content and conclusion of each part is listed as follow:
1. Methanol oxidation reaction at Pt electrode
Methanol (MeOH) oxidation reaction (MOR) at Pt electrodes under potentiostatic conditions has been investigated by electrochemical in situ FTIR spectroscopy (FTIRS) in attenuated-total-reflection configuration under controlled flow conditions in0.1M HClO4with2M MeOH, where the mass transport effects are largely eliminated using a flow cell. Our results reveal that (ⅰ) at constant potentials, the methanol dehydrogenation rate decreases while the COad oxidation rate increases with the accumulation of COad until the maximum COad coverage (ca.0.5ML i.e., the steady state) is reached;(ⅱ) at fixed COad coverage, the rates for MeOH decomposition to COad and COad oxidation increases with potential from0.3to0.7V (vs. RHE), with Tafel slopes for MeOH dehydrogenation of ca.440±30mV/dec, which is independent of COad coverage;(iii) the current efficiency of the CO pathway in MOR at0.6and0.7V is below20%and it decreases toward higher potentials. The mechanisms as well as the potential induced change in the kinetics of different pathways involved in MOR are briefly discussed.
2. Cyanide and Carbon monoxide adsorption at Pt electrode
The adsorption of cyanide at Pt film electrode in0.1M HClO4is examined by electrochemical in situ infrared spectroscopy under attenuated total reflection configuration. The time-resolved IR spectral features reveal that depending on the adsorption potential, cyanide adsorbates display three modes of C-N stretching vibration. At0.05V, a trans-(HN=CH) surface species is identified for the appearance of1639and1493cm-1bands. The band with peak frequency below2100cm-1is attributed to N-bound Pt-NC and another band with peak frequency at ca.2150cm-1is attributed to C-bound Pt-CN; the Stark slope of the former is ca.3times larger than that the latter. The identification of the orientation of CNad is further confirmed by the spectral behavior of co-adsorption of CO onto the saturated cyanide adlayer; it causes a blue shift in C-N stretching frequency for Pt-NC without intensity change and an increase in CN band intensity for Pt-CN. The evolution of C-N vibration band demonstrates that the initial adsorption state of cyanide is in the form of Pt-NCHad. And then it is oxidized to Pt-NC, and Pt-NC will slowly reorient to Pt-CN at longer adsorption time. Dipole-dipole coupling effects, inter-space compression and electronic effect are found to be responsible for potential-dependent spectral behavior with and without co-adsorbed CO based on calculations using density functional theory.
3. Methanol oxidation reaction at PtRu electrodes The reaction mechanism and dynamic process of methanol oxidation reaction at Pt and PtRu electrodes under potentiostatic conditions has been investigated by electrochemical in situ ATR-FTIR spectroscopy with flow cell in0.1M HC1O4+0.2M MeOH solution. After the deposition of Ru at Pt electrode, it is clearly found that the adsorption and desorption of under potential deposited H (UPD-H) has been restrained. Therefore, the coverage of Ru at Pt could be calculated by the total charge of the adsorption and desorption of UPD-H before and after introduction of Ru. After the deposition of Ru at Pt, the catalytic activity of Pt is clearly increased. The relationship between current density of methanol oxidation at PtxRuy electrodes and Ru coverages displays a volcano curve. The Pt61Ru39has the best catalytic activity towards MOR. In high Ru coverages, which the coverage exceeds39%, the CO can adsorb at Ru atom which leads to decrease of catalytic activity of PtxRuy electrodes. In low Ru coverages, the interaction between Ru and Pt promotes the methanol oxidation reaction and increase the density of CO at Pt. The methanol oxidation reaction at Pt61Ru39electrode under series of different constant potentials (0.3V,0.4V,0.5V and0.6V) indicates that the contribution of methanol dehydrogenation to CO and CO oxidation in totle reaction current displays clear potential effect. Comparing methanol oxidation reation at Pt and Pt61Ru39electrodes, it can be found that the enhancement of Ru to Pt catalytic activity is clearly stronger in lower potentials than that in higher potentials.
本实验室发展了电化学衰减全内反射红外光谱与流动电解池联用技术,可以在排除传质条件影响下,系统地研究干净Pt电极上电化学反应最初阶段的反应机理和反应动力学,并探讨电位、PH值和电极表面组成等对反应的影响。结合本实验室的优势条件并且针对目前DMFC中的难题,本博士论文主要研究甲醇、一氧化碳(CO)和氰根(CN-)在Pt或者PtRu电极上吸附和氧化的反应机制和动力学过程。
各个部分的主要内容和结论总结如下：1.甲醇在Pt电极上的氧化反应
利用电化学原位ATR-FTIR与排除传质影响的流动电解池联用技术,研究在Pt电极上各个不同的恒电位时0.1MHC104+2M CH3OH甲醇的氧化反应过程。结合CO吸附的红外光谱和氧化电量,计算CO的表面覆盖度,进而定量分析在一系列不同的CO覆盖度下甲醇氧化的反应途径的电流效率和Tafel斜率对应的决速步骤。结果表明：(i)在恒电位下,随着COad在电极表面的堆积并达到最大的覆盖度0.5单层的过程中,甲醇脱氢反应速率随之降低而COad氧化速率随之增加;(ii)在固定的COad覆盖度下,甲醇分解生成COad速率和COad氧化速率在0.3V到0.7V(vs.RHE)之间随着电势的增加而增加,甲醇脱氢的Tafel斜率大约是440±30mV/dec,而且不随COad覆盖度改变而改变。(iii)在0.6和0.7V时甲醇氧化反应中CO反应途径的电流效率在20%以下,而且随着电势的升高而降低。甲醇氧化反应的机制和电极电势变化引起的不同反应途径的动力学的变化也有简要的讨论。
2.氰根(Cyanide)和CO在Pt电极上的吸附
利用衰减全内反射电化学原位红外光谱与薄层流动电解池联用技术研究在0.1MHC104+0.01M KCN体系中CN-在Pt膜电极表面的吸附的电位效应和动力学过程。首次在酸性电解质体系中研究CN-在Pt电极上的吸附过程,并发挥流动电解池可以持续控制电位和快速切换的优势,在CN-吸附饱和的Pt表面引入C0,探讨在一系列电位下两种分子吸附时的相互作用。从时间分辨红外光谱的数据结果可以推测出：随着吸附时电极电势的改变,CN-在Pt电极上的吸附构型表现出三种不同的伸缩振动。在0.05V,1639cm-1和1493cm-1的峰,归属于trans-(HN=CH)表面物种。2100cm-1左右的峰,归属于N-端吸附的Pt-NC,在2150cm-1的峰,归属于C-端吸附的Pt-CN,而Pt-NC的Stark斜率是Pt-CN的3倍多。CNad在电极表面上吸附的构型朝向的识别可以通过在饱和CN吸附的Pt电极上引入CO共吸附的红外光谱的行为进一步得到证实。引入CO后可以发现对Pt-NC和Pt-CN两种构型的红外光谱有不同的影响：Pt-NC的C-N伸缩振动峰频发生了蓝移但峰强并没有明显变化;而Pt-CN的峰强有明显的增大,但频率却没有发生变化。C-N振动峰的变化揭示了在Pt电极表面上CN-最初的吸附构型是Pt-NCHad。然后,它氧化成了Pt-NC,随着反应时间的增加慢慢地改变成Pt-CN。基于DFT理论计算的结果发现,偶极耦合效应,空间挤压作用和电子效应可以用来解释CN-及其与CO共吸附的红外光谱变化的电极电势效应。
3.甲醇在PtRu电极上的氧化反应
利用电化学-ATR-FTIR技术研究了纯Pt与PtxRu,电极上甲醇氧化反应的动力学和反应机理。利用流动电解池切换到Ru溶液中沉积不同时间后,再切换回支持电解质清洗电解池,可以很方便地构建一系列不同覆盖度的PtxRuy电极。Ru沉积在Pt电极表面后,明显抑制了欠电位沉积H的吸脱附反应,因此通过计算沉积Ru前后的欠电位沉积H吸脱附反应的总电量可得到Ru在Pt电极表面上的覆盖度。引入Ru后,Pt电极的催化活性有明显提高。PtxRuy电极上甲醇氧化反应活性与Ru的覆盖度呈火山型曲线,实验表明Pt61Ru39电极的催化活性最好。在高覆盖度下,当Ru覆盖度超过39%时,CO会吸附在Ru上使得PtxRu,电极的活性降低。在低覆盖度下,由于Ru与Pt相互作用促进了甲醇脱氢反应,使得Pt上CO密度增大。Pt61Ru39电极上一系列不同电位(0.3V、0.4V、0.5V和0.6V)的甲醇氧化实验,表明甲醇脱氢生成CO和CO氧化的反应途径在总反应电流中的贡献有明显的电位效应。将甲醇在纯Pt电极和Pt61Ru39电极上的氧化反应进行比较,可以发现在低电位下Ru对Pt电极的氧化活性的促进效应比在高电位下明显得多。
Direct Methanol Fuel Cell (DMFC) has been seen as one of the solutions to the worldwide energy shortage and environmental protection problems. DMFC has plenty of adventages such as rapid starting speed, facile operating temperature, wide fuel source and little pollution. It is very propitious for DMFC to be largely used in socical life and industrial production. There are two problems which restrict the large-scale commercialization of DMFC. Firstly, the reaction intermediate CO from methanol oxidation reaction displays a strong adsorption at Pt-based anodic catalyst, which leads to the decrease of current density and output voltage; Secondly, at present the most worldwide DMFC catalyst is Pt-based materials. As an important expensive metal with a finite storage in planet, the Pt not only restricts the productivity of DMFC but also raises the price. Demonstrating the reaction mechanism and the influence on the dynamics from all kinds of factors in molecular level is the premise of designing DMFC anodic electrocatalyst with high performance and low Pt load.
Electrochemical in situ ATR-FRIT spectroscopy with flow cell technique devoloped in our lab, allows the systematic research of initial reaction mechanism and dynamics of electrochemical reaction at clean Pt electrode without the influence of mass tranfer, and then to probe potential, PH and electrode compostion effects on the reaction. Aiming the current DMFC problems and combining the advantage in our lab, this thesis focuses on the research on the reaction mechanism and dynamic process of methanol, carbon monoxide and cyanide adsorption and oxidation at Pt or PtRu electrode.
The main content and conclusion of each part is listed as follow:
1. Methanol oxidation reaction at Pt electrode
Methanol (MeOH) oxidation reaction (MOR) at Pt electrodes under potentiostatic conditions has been investigated by electrochemical in situ FTIR spectroscopy (FTIRS) in attenuated-total-reflection configuration under controlled flow conditions in0.1M HClO4with2M MeOH, where the mass transport effects are largely eliminated using a flow cell. Our results reveal that (ⅰ) at constant potentials, the methanol dehydrogenation rate decreases while the COad oxidation rate increases with the accumulation of COad until the maximum COad coverage (ca.0.5ML i.e., the steady state) is reached;(ⅱ) at fixed COad coverage, the rates for MeOH decomposition to COad and COad oxidation increases with potential from0.3to0.7V (vs. RHE), with Tafel slopes for MeOH dehydrogenation of ca.440±30mV/dec, which is independent of COad coverage;(iii) the current efficiency of the CO pathway in MOR at0.6and0.7V is below20%and it decreases toward higher potentials. The mechanisms as well as the potential induced change in the kinetics of different pathways involved in MOR are briefly discussed.
2. Cyanide and Carbon monoxide adsorption at Pt electrode
The adsorption of cyanide at Pt film electrode in0.1M HClO4is examined by electrochemical in situ infrared spectroscopy under attenuated total reflection configuration. The time-resolved IR spectral features reveal that depending on the adsorption potential, cyanide adsorbates display three modes of C-N stretching vibration. At0.05V, a trans-(HN=CH) surface species is identified for the appearance of1639and1493cm-1bands. The band with peak frequency below2100cm-1is attributed to N-bound Pt-NC and another band with peak frequency at ca.2150cm-1is attributed to C-bound Pt-CN; the Stark slope of the former is ca.3times larger than that the latter. The identification of the orientation of CNad is further confirmed by the spectral behavior of co-adsorption of CO onto the saturated cyanide adlayer; it causes a blue shift in C-N stretching frequency for Pt-NC without intensity change and an increase in CN band intensity for Pt-CN. The evolution of C-N vibration band demonstrates that the initial adsorption state of cyanide is in the form of Pt-NCHad. And then it is oxidized to Pt-NC, and Pt-NC will slowly reorient to Pt-CN at longer adsorption time. Dipole-dipole coupling effects, inter-space compression and electronic effect are found to be responsible for potential-dependent spectral behavior with and without co-adsorbed CO based on calculations using density functional theory.
3. Methanol oxidation reaction at PtRu electrodes The reaction mechanism and dynamic process of methanol oxidation reaction at Pt and PtRu electrodes under potentiostatic conditions has been investigated by electrochemical in situ ATR-FTIR spectroscopy with flow cell in0.1M HC1O4+0.2M MeOH solution. After the deposition of Ru at Pt electrode, it is clearly found that the adsorption and desorption of under potential deposited H (UPD-H) has been restrained. Therefore, the coverage of Ru at Pt could be calculated by the total charge of the adsorption and desorption of UPD-H before and after introduction of Ru. After the deposition of Ru at Pt, the catalytic activity of Pt is clearly increased. The relationship between current density of methanol oxidation at PtxRuy electrodes and Ru coverages displays a volcano curve. The Pt61Ru39has the best catalytic activity towards MOR. In high Ru coverages, which the coverage exceeds39%, the CO can adsorb at Ru atom which leads to decrease of catalytic activity of PtxRuy electrodes. In low Ru coverages, the interaction between Ru and Pt promotes the methanol oxidation reaction and increase the density of CO at Pt. The methanol oxidation reaction at Pt61Ru39electrode under series of different constant potentials (0.3V,0.4V,0.5V and0.6V) indicates that the contribution of methanol dehydrogenation to CO and CO oxidation in totle reaction current displays clear potential effect. Comparing methanol oxidation reation at Pt and Pt61Ru39electrodes, it can be found that the enhancement of Ru to Pt catalytic activity is clearly stronger in lower potentials than that in higher potentials.
引文
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