电化学与质谱/红外光谱联用的电催化研究
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摘要
燃料电池是一种高效清洁的能源利用方式,有望解决人类当下所面临的环境和能源危机。目前发展相对成熟的质子交换膜型燃料电池使用氢气作为燃料,然而氢气的储运仍存在未解决的技术问题。其他潜在的可取代氢气的燃料包括了氨、甲醇、乙醇等,但相应的电化学反应动力学缓慢,相关的电催化机理和催化剂研究仍是当前的研究热点。本论文工作构建了两类用于电催化反应机理研究的谱学电化学方法,即差分电化学质谱和电化学在线红外光谱,并对氨氧化反应、甲醇氧化反应和乙醇氧化反应进行了研究。取得的主要研究进展如下：
1.差分电化学质谱(DEMS)方法的构建
我们构建了两种DEMS系统：膜电极DEMS系统和盘电极DEMS系统。在膜电极DEMS系统中,工作电极为含PTFE的碳膜,同时利用其疏水透气性这一特点将其作为真空采样管路与电解池之间的膜接口。在碳膜上下表面的压力差作用下,电化学反应生成的挥发性产物一旦生成即被抽入质谱仪中被检测。在盘电极DEMS系统中,由疏水透气的毛细管采样口对盘电极表面生成的挥发性物种进行采样；另外为了对非水体系的气体产物进行检测,我们还引入了产物富集罩的设计,解决了采样口无法在非水体系中直接进样的难题。
2.氨电氧化反应的DEMS研究
我们利用构建的盘电极DEMS系统,对水体系和非水体系氨氧化反应进行对比研究。发现水溶液中Pt和Pd氨氧化反应的抑制现象与表面含氧物种的大量生成存在关联,而在非水体系中表面含氧物种不存在的情况下,Pt和Pd表现出了随电势正移不断增长的催化活性,由此推断出水体系中表面含氧物种作为毒物抑制氨氧化反应的证据。另外,在非水体系中Pd催化氨氧化活性比Pt更高,在水体系中无催化氨氧化活性的Au在非水体系中也表现出了较明显的活性。
3.电化学与红外光谱联用方法的构建
电化学与红外光谱的联用方法可以与DEMS系统形成互补。我们首先构建了常规的电化学与反射红外光谱联用的方法,实验发现,电极与棱镜之间薄层溶液会造成离子传导阻碍、反应物补充不及时以及难以获得定量的数据等问题。因此我们构建了电化学和透射红外光谱的联用系统,该系统通过附带离子交换膜的工作电极采样罩的设计,使富集的产物流动至透射红外液体池进行检测。此方法具备以下几个优点：电化学行为正常、反应物及时补充、可定量获得产物浓度、可开展变温实验。
4.碱性体系中Pt和Pd催化甲醇氧化反应的研究
在碱性体系中,Pt和Pd均表现出了远高于酸性体系的甲醇氧化催化活性,并且Pd的催化活性与Pt接近。二者表面的形貌组成均会对催化甲醇氧化活性产生影响,表面原子配位数较低的Pt(110)和Pd(110)晶面更有利于甲醇氧化反应的发生。另外,在Pt和Pd表面修饰Ru之后,其甲醇氧化催化活性得到了明显提高,提高的程度随着Ru覆盖度的增长呈现了先增大后减小的趋势。最后,利用在线电化学流动透射红外光谱对碱性体系Pt催化甲醇氧化产物进行检测,发现CO32-的电流效率随着反应温度的升高明显增大。
5.碱性体系中Pt和Pd催化乙醇氧化反应的研究
在碱性体系中,Pt和Pd均表现出了远高于酸性体系的乙醇氧化催化活性。二者表面的形貌组成均会对催化乙醇氧化活性产生影响,表面原子配位数较低的Pt(110)和Pd(110)晶面不仅有利于表面含氧物种的生成,还可能有利于碳碳键断裂过程的发生。电沉积制备的表面(110)晶面比例较高的Pd的乙醇氧化催化活性甚至高于Pt。利用在线电化学流动透射红外光谱对碱性体系电催化乙醇氧化反应进行研究,发现较高的温度以及较厚的催化层均有利于完全氧化产物CO32-的电流效率的提高,而且乙醛氧化生成CO32-的电流效率比乙醇作为反应物时更高。
As a clean and efficient energy convertor, fuel cells can solve the current environment and energy crisis. The hydrogen-fueled proton exchange membrane fuel cell is relatively matured, yet there are some technical problems in the storage and transportation of hydrogen. The hydrogen gas can be replaced by several alternative fuels, such as ammonia, methanol and ethanol, which, however, suffer from slow reaction kinetics. Therefore, research efforts have been focused on the catalysts and the reaction mechanism of the oxidation of these fuels. In this thesis, two types of spectroelectrochemical methods were constructed for electrocatalysis study, namely, the differential electrochemical mass spectrometry and the on-line electrochemical infrared spectroscopy. These two methods were applied to the study of the electrooxidation reactions of ammonia, methanol and ethanol. Major results of this work are summerized as follows:
1. Construction of differential electrochemical mass spectrometry (DEMS)
Two types of DEMS were constructed:DEMS system for membrane electrodes and DEMS system for disk electrodes. In the design of DEMS system for membrane electrodes, a PTFE-containing carbon film functions as the working electrode, which is also the membrane inlet connecting the vacuum sampling pipe and the electrochemical cell. Driven by the pressure between the two sides of the carbon film, volatile species, once formed during electrochemical reactions, can be sampled by MS. In the set-up of DEMS system for disk electrodes, volatile products formed on the surface of disk electrodes were sampled by a hydrophobic capillary probe. Besides, the disk electrode is capped by a polyethylene mini-hood for the detection of gaseous products produced by reactions in nonaqueous media.
2. DEMS study of ammonia oxidation reaction (AOR)
A comparative DEMS study of AOR in both aqueous and nonaqueous media revealed that the inhibition of ammonia oxidation reaction catalyzed by Pt or Pd could be due to the surface blocking of oxygenated species. It was found that, during AOR in nonaqueous media where no surface oxygenated species exist, the catalytic activity of Pt and Pd increases with the increasing potential, which proves the inhibition role of surface oxygenated species in AOR in aqueous media. In addition, Pd shows an even higher activity toward AOR than Pt in nonaqueous media, and the oxidation of ammonia can proceed on Au which is inactive in aqueous media.
3. The combination of electrochemistry and infrared spectroscopy
As the complementation of DEMS, the combination of electrochemistry and infrared spectroscopy was set up for electrochemical mechanism studies. First of all, a conventional electrochemical FTIR reflection spectroscopy was constructed. However, several issues were caused by the thin layer electrolyte between the disk electrode and prism, such as poor ionic conduction, exhaustion of reactants and inapplicability of quantitative analysis. Consequently, a new system combining electrochemistry and FTIR transmission spectroscopy was set up. By the design of a sampling system attached with an ion-exchange membrane for the working electrode, enriched products can be sampled and then detected in the transmission IR cell. The new system possesses several advantages, such as normal electrochemical behaviors, supplement of reactants, quantitative analysis of concentration, and controllable reacting temperature.
4. The study of methanol oxidation reaction (MOR) on Pt and Pd in alkaline media
In alkaline media, the MOR activity of Pt and Pd is remarkably higher than that in acidic media, and Pd shows a comparable activity with Pt. MOR on both Pt and Pd is a structure-sensitive reaction which is favored on low-coordinated Pt(110) and Pd(110) sites. Besides, the MOR activity of Pt and Pd can be further enhanced by the decoration of Ru, and there is a maximum of the enhancement of MOR activity in a wide range of Ru coverage. Lastly, the products of MOR on Pt in alkaline media were detected by on-line electrochemical flowing FTIR transmission spectroscopy, showing that the efficiency of carbonate formation increases with temperature.
5. The study of ethanol oxidation reaction (EOR) on Pt and Pd in alkaline media
The EOR activity of Pt and Pd in alkaline media is remarkably higher than that in acidic media. The effect of surface morphology on the catalytic activities of Pt and Pd indicates that low-coordinated Pt(110) and Pd(110) sites favor the formation of surface oxygenated species and the split of C-C bond. The electrodeposited Pd with a large number of (110) sites shows an even higher activity toward EOR than Pt. After the investigation of products of EOR in alkaline media by on-line electrochemical flowing FTIR transmission spectroscopy, it was found that the efficiency of carbonate formation is higher at elevated temperatures and thick catalyst layers. Additionally, the efficiency of carbonate formation is much higher in acetaldehyde oxidation reaction than that in EOR.
1.差分电化学质谱(DEMS)方法的构建
我们构建了两种DEMS系统：膜电极DEMS系统和盘电极DEMS系统。在膜电极DEMS系统中,工作电极为含PTFE的碳膜,同时利用其疏水透气性这一特点将其作为真空采样管路与电解池之间的膜接口。在碳膜上下表面的压力差作用下,电化学反应生成的挥发性产物一旦生成即被抽入质谱仪中被检测。在盘电极DEMS系统中,由疏水透气的毛细管采样口对盘电极表面生成的挥发性物种进行采样；另外为了对非水体系的气体产物进行检测,我们还引入了产物富集罩的设计,解决了采样口无法在非水体系中直接进样的难题。
2.氨电氧化反应的DEMS研究
我们利用构建的盘电极DEMS系统,对水体系和非水体系氨氧化反应进行对比研究。发现水溶液中Pt和Pd氨氧化反应的抑制现象与表面含氧物种的大量生成存在关联,而在非水体系中表面含氧物种不存在的情况下,Pt和Pd表现出了随电势正移不断增长的催化活性,由此推断出水体系中表面含氧物种作为毒物抑制氨氧化反应的证据。另外,在非水体系中Pd催化氨氧化活性比Pt更高,在水体系中无催化氨氧化活性的Au在非水体系中也表现出了较明显的活性。
3.电化学与红外光谱联用方法的构建
电化学与红外光谱的联用方法可以与DEMS系统形成互补。我们首先构建了常规的电化学与反射红外光谱联用的方法,实验发现,电极与棱镜之间薄层溶液会造成离子传导阻碍、反应物补充不及时以及难以获得定量的数据等问题。因此我们构建了电化学和透射红外光谱的联用系统,该系统通过附带离子交换膜的工作电极采样罩的设计,使富集的产物流动至透射红外液体池进行检测。此方法具备以下几个优点：电化学行为正常、反应物及时补充、可定量获得产物浓度、可开展变温实验。
4.碱性体系中Pt和Pd催化甲醇氧化反应的研究
在碱性体系中,Pt和Pd均表现出了远高于酸性体系的甲醇氧化催化活性,并且Pd的催化活性与Pt接近。二者表面的形貌组成均会对催化甲醇氧化活性产生影响,表面原子配位数较低的Pt(110)和Pd(110)晶面更有利于甲醇氧化反应的发生。另外,在Pt和Pd表面修饰Ru之后,其甲醇氧化催化活性得到了明显提高,提高的程度随着Ru覆盖度的增长呈现了先增大后减小的趋势。最后,利用在线电化学流动透射红外光谱对碱性体系Pt催化甲醇氧化产物进行检测,发现CO32-的电流效率随着反应温度的升高明显增大。
5.碱性体系中Pt和Pd催化乙醇氧化反应的研究
在碱性体系中,Pt和Pd均表现出了远高于酸性体系的乙醇氧化催化活性。二者表面的形貌组成均会对催化乙醇氧化活性产生影响,表面原子配位数较低的Pt(110)和Pd(110)晶面不仅有利于表面含氧物种的生成,还可能有利于碳碳键断裂过程的发生。电沉积制备的表面(110)晶面比例较高的Pd的乙醇氧化催化活性甚至高于Pt。利用在线电化学流动透射红外光谱对碱性体系电催化乙醇氧化反应进行研究,发现较高的温度以及较厚的催化层均有利于完全氧化产物CO32-的电流效率的提高,而且乙醛氧化生成CO32-的电流效率比乙醇作为反应物时更高。
As a clean and efficient energy convertor, fuel cells can solve the current environment and energy crisis. The hydrogen-fueled proton exchange membrane fuel cell is relatively matured, yet there are some technical problems in the storage and transportation of hydrogen. The hydrogen gas can be replaced by several alternative fuels, such as ammonia, methanol and ethanol, which, however, suffer from slow reaction kinetics. Therefore, research efforts have been focused on the catalysts and the reaction mechanism of the oxidation of these fuels. In this thesis, two types of spectroelectrochemical methods were constructed for electrocatalysis study, namely, the differential electrochemical mass spectrometry and the on-line electrochemical infrared spectroscopy. These two methods were applied to the study of the electrooxidation reactions of ammonia, methanol and ethanol. Major results of this work are summerized as follows:
1. Construction of differential electrochemical mass spectrometry (DEMS)
Two types of DEMS were constructed:DEMS system for membrane electrodes and DEMS system for disk electrodes. In the design of DEMS system for membrane electrodes, a PTFE-containing carbon film functions as the working electrode, which is also the membrane inlet connecting the vacuum sampling pipe and the electrochemical cell. Driven by the pressure between the two sides of the carbon film, volatile species, once formed during electrochemical reactions, can be sampled by MS. In the set-up of DEMS system for disk electrodes, volatile products formed on the surface of disk electrodes were sampled by a hydrophobic capillary probe. Besides, the disk electrode is capped by a polyethylene mini-hood for the detection of gaseous products produced by reactions in nonaqueous media.
2. DEMS study of ammonia oxidation reaction (AOR)
A comparative DEMS study of AOR in both aqueous and nonaqueous media revealed that the inhibition of ammonia oxidation reaction catalyzed by Pt or Pd could be due to the surface blocking of oxygenated species. It was found that, during AOR in nonaqueous media where no surface oxygenated species exist, the catalytic activity of Pt and Pd increases with the increasing potential, which proves the inhibition role of surface oxygenated species in AOR in aqueous media. In addition, Pd shows an even higher activity toward AOR than Pt in nonaqueous media, and the oxidation of ammonia can proceed on Au which is inactive in aqueous media.
3. The combination of electrochemistry and infrared spectroscopy
As the complementation of DEMS, the combination of electrochemistry and infrared spectroscopy was set up for electrochemical mechanism studies. First of all, a conventional electrochemical FTIR reflection spectroscopy was constructed. However, several issues were caused by the thin layer electrolyte between the disk electrode and prism, such as poor ionic conduction, exhaustion of reactants and inapplicability of quantitative analysis. Consequently, a new system combining electrochemistry and FTIR transmission spectroscopy was set up. By the design of a sampling system attached with an ion-exchange membrane for the working electrode, enriched products can be sampled and then detected in the transmission IR cell. The new system possesses several advantages, such as normal electrochemical behaviors, supplement of reactants, quantitative analysis of concentration, and controllable reacting temperature.
4. The study of methanol oxidation reaction (MOR) on Pt and Pd in alkaline media
In alkaline media, the MOR activity of Pt and Pd is remarkably higher than that in acidic media, and Pd shows a comparable activity with Pt. MOR on both Pt and Pd is a structure-sensitive reaction which is favored on low-coordinated Pt(110) and Pd(110) sites. Besides, the MOR activity of Pt and Pd can be further enhanced by the decoration of Ru, and there is a maximum of the enhancement of MOR activity in a wide range of Ru coverage. Lastly, the products of MOR on Pt in alkaline media were detected by on-line electrochemical flowing FTIR transmission spectroscopy, showing that the efficiency of carbonate formation increases with temperature.
5. The study of ethanol oxidation reaction (EOR) on Pt and Pd in alkaline media
The EOR activity of Pt and Pd in alkaline media is remarkably higher than that in acidic media. The effect of surface morphology on the catalytic activities of Pt and Pd indicates that low-coordinated Pt(110) and Pd(110) sites favor the formation of surface oxygenated species and the split of C-C bond. The electrodeposited Pd with a large number of (110) sites shows an even higher activity toward EOR than Pt. After the investigation of products of EOR in alkaline media by on-line electrochemical flowing FTIR transmission spectroscopy, it was found that the efficiency of carbonate formation is higher at elevated temperatures and thick catalyst layers. Additionally, the efficiency of carbonate formation is much higher in acetaldehyde oxidation reaction than that in EOR.
引文
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