小分子在模型催化剂表面的吸附与反应

英文题名：Adsorption and Reaction of Small Molecules on Model Catalyst Surfaces
作者：许令顺
论文级别：博士
学科专业名称：物理化学
中文关键词：模型催化剂 ; 小分子 ; 吸附 ; 表面反应 ; 碳物种 ; 羟基 ; 氧缺陷
英文关键词：Model catalyst ; Small molecules ; Adsorption ; Surface reaction ;
英文关键词：Carbon deposite ; Hydroxyl ; Oxygen vacancy
学位年度：2012
导师：黄伟新
学科代码：070304
学位授予单位：中国科学技术大学
论文提交日期：2012-04-01

摘要

尽管存在着“物质鸿沟”和“压力鸿沟”,在超高真空体系中原位制备结构规整的模型催化剂,并相应开展表面化学研究,为微观角度上了解实际多相催化体系提供了重要的研究手段。在本论文中,我们从金属单晶、薄膜氧化物到金属单晶担载的金属氧化物倒载模型催化剂三个不同层次的模型催化剂出发,分别选择Co(0001).FeO(111)/Pt(111)单层薄膜及FeO(111)/Pt(111)单层岛屿倒载模型催化剂三个研究体系,系统研究CP、H2、H2O等小分子在其表而的吸附与反应,取得如下研究结果：
     (1)研究了在清洁的Co(0001)模型表面上CO和H2的共吸附：CO(a)和H(a)之间存在较强的排斥作用。CO的吸附完全可以阻止H2的吸附,而H2的吸附虽然不能完全阻止CO的吸附,但可以在一定程度上改变其吸附行为。Co(0001)表面预覆盖不同种类的碳物种对H2和CO的吸附行为有着显著的影响。在原子碳覆盖的表面,CO吸附可以诱导其扩散至体相,而脱附以后又可逆的扩散至表面。H：则在表面解离后与原子碳直接反应生成CH。而表面预吸附的石墨烯物种对CO和H2的吸附的影响主要归结为位阻效应。(2)考察了H20在Co(0001)模型表面的吸附行为：在低温下,H20主要以分子形式吸附。而在室温下,H2O则解离成H和O,并氧化Co(0001)表面；Co(0001)表面氧物种的存在对H2O的吸附有很大影响,在0.45ML O(a)覆盖的Co(0001)表面,在130K时H2O的吸附发生2H20(a)+O(a)→-3OH(a)+H(a)表面反应,形成OH(a)+H(a)的共吸附层,但在对Co(0001)表面进行氧化生成CoO表面后,即使在室温H2O也以分子形式吸附。
     (3)研究了Co(0001)表面C2H4和C2H2的吸附和分解：低温下,C2H4在干净的Co(0001)表面的吸附与反应行为受到表面空位浓度的控制。在低覆盖度下,C2H4解离成C2H2和H,随着表面覆盖度的增加,C2H4分子吸附在表面。表面预覆盖碳可以抑制C2H4的解离从而使得C2H4发生分子吸附。表面预吸附O原子对C2H4的吸附也主要是位阻效应,O的存在改变了C2H4的吸附位置。另外,在C2H4解离的过程中,O可以与其中间体发生反应。在Co(0001)表面,相对于C2H4的吸附,C2H2的吸附与反应行为受表面覆盖度和温度的影响更加明显。在130K,C2H2在表面以分子形式吸附,升温过程中既可以直接脱H形成C2,也可以聚合形成碳环以后脱H形成石墨化碳,对这两种反应通道的选择性依赖于表面覆盖度。较高的初始覆盖度有利于生成石墨化碳的反应通道。通过C2H4不同温度下的吸附可以在Co(0001)表面制备不同种类的碳物种(如碳原子C1,双原子簇C2以及石墨烯),研究了C1,C2转化为石墨化碳的动力学和热力学,计算了其反应活化能和反应焓,发现虽然C1与C2转化为石墨烯的反应焓比较接近,但它们的反应活化能却相差较大。这些结果与目前有关石墨烯生长机理的理论计算结果基本一致,在实验上为理论计算提供了重要的参考。
     (4)考察了原子氢(氘)和H2O(D2O)与不同还原程度的FeO(111)/Pt(111)单层薄膜模型表面的相互作用：原子D与表面O可以生成表面羟基OD(a),在剂量比的FeO(111)单层薄膜表面,OD(a)倾向于生成D2O进而在表面产生O缺陷(OD(a)+OD(a)→D2O(g)+OL+Ov);随着O缺陷浓度的增加,生成D20的通道受到抑制,在FeO0.67的表面,OD(a)选择性地生成D2(OD(a)+OD(a)→D2(g)+2OL).这些结果揭示了O缺陷控制表面羟基反应性能的新概念：即O缺陷的浓度控制羟基生成D2O和D2的反应选择性。低温下,剂量比的FeO/Pt(111)单层薄膜表面上,D2O的吸附是可逆的。当表面存在O缺陷时,D2O部分解离在O缺陷位生成OD(a),部分以分子形式吸附在O缺陷位。吸附在缺陷位上的D2O可以在加热过程中解离。很有趣的是,我们在实验中,发现一个低温产生氢气的通道(反应温度<200K),我们推测其可能来自于O缺陷和氢键等共同作用,即吸附在缺陷位上的D2O可能由于与其他吸附的D2O分子形成氢键而发生解离(D2O(a)+Ov→OD(a)+D),解离产生的D原子进入水层中,在分子水脱附时以D2形式脱附。此外还考察了HCOOH在FeO(111)/Pt(111)单层薄膜模型表面上的吸附。在剂量比的FeO表面,HCOOH可以与表面O发生反应最终还原FeO。另外,在O缺陷的表面,HCOOH更加容易解离,并且HCOO-可以稳定存在很高的温度(>500K), HCOO在与表面O共同作用下解离主要生成CO2, CO和H2。
     (5)研究了FeO(111)/Pt(111)单层岛屿反转模型催化剂表面的吸附和反应行为。在表面暴露原子D,除了空白Pt(111)表面上的D并合脱附和上面提到的FeO表面上OD的反应脱附,而在Pt-FeO界面处,实验中观察到新的反应通道,即Pt上吸附的D原子与FeO表面上的OD发生反应(D(a)+OD(a)→D20)。与Pt(111)和完整的FeO表面上的分子吸附不同,在Pt-FeO界面处,由于暴露有配为不饱和Fe2+,D2O可以发生解离,生成OD。在界面处,我们同样首次在实验中观察到,加热过程中在Pt(111)表而吸附的CO可以和FeO表面吸附的OD发生界面反应生成CO2,该反应性能也受到FeO表面O缺陷的控制。在剂量比的FeO表面,OD与OD更容易反应生成D2O。表面O缺陷的存在抑制了OD生成D2O的反应,从而有利于上述CO-OD的界面反应的发生。这些结果不仅为Pt/氧化物催化剂界面处CO与OD的界面低温氧化反应提供了直接的证据,而且表明具有一定O缺陷的FeO单层结构是该反应的可能活性结构。
     总之,在超高真空体系原位制备不同结构层次的模型催化剂,并考察小分子在模型催化剂表面上的吸附与反应行为,一方面能够在原子分子层次理解固体表面组成和结构对其吸附与反应性能的影响；另一方面通过与实际催化反应相关联,加深了我们对与这些模型催化剂相关的包括费托合成,水汽变换和富氢条件下CO氧化等实际催化反应体系的基础理解。
Despite the existence of so call "materials gap" and "pressure gap", surface science studies of well-defined model surfaces prepared in-situ in ultra-high vacuum (UHV) conditions have been proved to be a useful approach for the fundamental understaning of real catalytic systems at a microscopic level. In this thesis, Co (0001), FeO(111) mono layer film grown on Pt (111) and inverse FeO(111)/Pt(111) model catalysts have been fabricated and their interaction with small molecules such as CO, H2and H2O have been systematically investigated. The main results are summarized in the following:
     (1) Coadsorption of CO and H2on Co(0001) has been investigated:there exists strong repulse interaction between CO(a) and H(a) on clean Co (0001) surface. The pre-adsorption of CO largely suppresses the adsorption of H2while the pre-adsorption of H2does not suppress the CO adsorption much but changes its adsorption behavior to a certain extent. The presence of various types of carbon species significantly influences the adsorption behavior of CO and H2. On atomic carbon-covered Co(0001), atomic carbon diffuses into the bulk upon CO adsorption and diffuses back to the surface after CO desorption. The formation of CH(a) was observed after H2adsorption at130K. On graphitic carbon-covered Co(0001), only the site-blocking effect exists for the adsorption of CO and H2.
     (2) The adsorption and reaction of water on Co(0001) surface have been investigated:H2O molecularly adsorb on Co(0001) at130K, forming an intact, non-wetting and3-dimensional layer on Co(0001) that desorbs molecularly upon heating. At300K, H2O adsorbs dissociatively on Co(0001), forming O(a) and H(a). Upon heating, H(a) forms H2desorbing from the surface whereas O(a) remains on the surface. The presence and nature of oxygen species on Co(0001) exert great influences on its reactivity towards H2O. On0.45ML O(a)-covered Co(0001), H2O adsorption forms a mixture layer of OH(a) and H(a) via the reaction of2H2O(a)+O(a)→3OH(a)+H(a) at130K. However, on oxide-like Co(0001) surface, H2O only molecularly adsorbs even at RT.
     (3) The adsorption and reaction of C2H4and C2H2on Co(0001) surface have been studied:At low temperature, the adsorption and reaction of C2H4on clean Co (0001) surface are controlled by the available free surface sites. C2H4dehydrogenate to C2H2(a) and H(a) at low coverage, and molecularly adsorb with the increasing of the surface coverage. The presence of atomic carbon on Co(0001) suppresses the dissociation of C2H4due to site-blocking effect. Pre-covered O(a) exerts the similar site-blocking effect on C2H4adsorption but further affects the C2H4adsorption site. During heating, O(a) coan interact with the surface intermediate produced formed by C2H4(a) decomposition. The adsorption and reaction of C2H2on Co (0001) surface is also controlled by the surface coverage and temperature. At130K. C2H2molecularly adsorbs on the surface. During heating, C2H2(a) undergoes two competing reaction pathways eventually to form carbon deposite:one is the direct dehydrogenation into C2clusters and the other is the polymerization of C2H2(a) into surface intermediate with a likely ring structure followed by further dehydrogenation into graphic carbon. The reaction pathway to graphic carbon is preferred at higher C2H2(a) surface coverage. Three different carbon species, atomic carbon(C1), C2carbon clusters and graphic carbon, have been prepared on Co (0001) by C2H4adsorption at different surface temperatures. The apparent reaction activation energy and reaction enthalpy for the formation of graphic carbon from C1and C2have been successfully determined. The activation energies of the C1-to-graphic carbon and C2-to-graphic carbon transformations vary much but the reaction enthalpies are similar, agreeing with the predicted results by theoritical calculations.
     (4) The interaction and reaction of atomic hydrogen (Deuterium) and H2O(D2O) on FeO(111)/Pt(111) monolayer films with different concentrations of oxygen vacancies have been investigated:surface hydroxyls (OH(a)) readily form on inert FeO(111) by the reaction of between H(g) and lattice oxygen (OL). On the stoichiometric FeO(111) monolayer film, OH(a) selectively reacts to form H2O, creating one oxygen vacancies (Ov) on the surface (OH(a)+OH(a)→H2O(g)+Ov+OL). With the increasing concentration of the oxygen vacancy concentration in the FeO(111) monolayer film, the above reaction pathway of OH(a) to form H2O get gradually suppressed while the reaction pathway of OH(a) to form H2(OD(a)+OD(a)→D2(g)+2OL) appears; on the FeOo67(111) monolayer film, OH(a) selectively form H2. These results reveal a novel concept of oxygen vacancy-controlled reactivity of surface hydroxyls in which the thermodynamically favorable reactions switches from reactions to form H2O and oxygen vacancies on the stoichiometric metal oxide surface to those to form H2on the partially-reduced metal oxide surface with an appropriate amount of oxygen vacancies. On the stoichiometric FeO surface, H2O molecular adsorption at130K is revisible. When the surface is with oxygen vacancies, for example, on FeOo67surface, H2O both dissociates on the O vacancies to form OH(a) and and molecularly adsorbs on the oxygen vacancies. Upon heating, part of H2O(a) on the oxygen vacancies dissociates to OD(a) and others desorbs molecularly. We observed an interesting novel H2production channel at low temperature (<200K) accompanying molecular H2O desorption. This might be ascribed to interplay between oxygen vacancies and hydrogen bond within adsorbed layer. The Ov-adsorbed HoO(a) can undergo dissociation reaction induced by the formation of hydrogen bond with co-adsorbed H2O(a), in which the formed H(a) might enter the H2O(a) layer and desorb simultaneously with the H2O(a) layer. In addition, We have also studied the adsorption and reaction of HCOOH on FeO(111) monolayer film. On the stoichiometric FeO(111) monolayer film, HCOOH decomposes and partially reduces the surface. In the presence of O vacancies, HCOOH dissociates more easily on the oxygen-vacancy sites and the formed HCOO(a) remains stable even above500K and then eventually decomposes into CO2, CO and H2at higher temperature.
     (5) The chemisorption and surface reactivity of FeOx(111)/Pt(111) inverse model catalysts with various surface coverages of FeOx(111) monolayer islands have been studied:Hydroxyls were produced on FeOx(111) monolayer islands employing atomic hydrogen and were found to be capable of oxidizing CO(a) on Pt(111) to produce CO2between RT and400K, and their reactivity are also controlled by the oxygen vacancy concentration in FeOx(111) monolayer islands. Hydroxyls on FeO058(111) monolayer islands with the highest oxygen vacancy concentration undergoes reactions to produce D2and CO2whereas hydroxyls on stoichiometric FeO(111) monolayer islands undergoes reactions to produce D2and D2O. Such an oxygen vacancy-controlled reactivity of hydroxyls on FeOx(111) monolayer islands can be attributed to the fact that the reaction pathway of OH(a) to produce H2O thermodynamically gets suppressed with the increase of oxygen vacancy concentration, thus opening other hydroxyls-involved reaction pathways. The interfacial oxidation of CO(a) by OH(a) to produce CO2at FeOx(111)-Pt(111) interface is not supressed by either excess CO(a) or excess H(a) on FeOx(111)/Pt(111) inverse model catalyst surface. These results not only provide solid experimental evidence for the low temperature interfacial oxidation of CO with hydroxyls at Pt-oxide interface but also demonstrate that FeO(111) monolayer islands with certain amount of oxygen vacancies are the active structure for such an elementary reaction.
     In summary, by studying the adsorption and reaction of small molecules on model catalyst surfaces, on one hand, we have unambiguously understood the influence of surface composition and structure of these surfaces on their chemisorption and surface reactivity at a molecular level; on the other hand, the fundamental understanding of revelant real catalytic reactions including Fischer-Tropsch synthesis, water gas shift reaction(WGS) and preferential oxidation of CO in H2-rich gases (PROX) has also been deepened.

引文

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