摘要
纳米材料具有许多不同于常规材料的特殊性质，引起了材料、化学、物理、生物、工程等众多学科的广泛兴趣，是纳米科技的核心问题。铂族金属由于催化活性高、性能稳定而被作为电催化剂广泛应用于能源转换、绿色合成等重要领域。研制纳米尺度的金属材料电催化剂是电催化的热点课题之一。
本论文以化学法合成金属Pt纳米粒子(Pt_n)。UV-vis光谱和TEM研究表明，Pt_n主要是在加热回流的开始阶段形成。利用双硫醇把合成的Pt_n组装到金基底上，用Fe(CN)_6~(4-／3-)氧化还原电对作探针反应研究了组装过程中电子传导能力，结果表明，二硫醇单层膜阻碍Au基底与Fe(CN)_6~(4-／3-)之间的异相电子传递，但进一步组装Pt_n后，由于量子隧穿效应使得电子的传递能力提高。分别用AFM和XPS对组装体系的表面形貌和组成进行了分析。原位FTIRS和CV结果显示，与本体Pt相比，吸附于Pt_n上的CO有显著的增强红外吸收。同时，由于表面效应和小尺寸效应，CO在Pt_n上的氧化电位较高，呈现出较多的吸附状态。
本文首次发现，无论在固／液或固／气界面，处于离散状态的Pt纳米粒子表现出增强红外吸收，而团聚的Pt纳米粒子则具有异常红外效应。本文还首次运用透射红外光谱对不同聚集状态Pt纳米粒子的红外性能进行了研究。结果表明，随着Pt纳米粒子从分散态到不同程度的聚集态，吸附CO分子的红外吸收特征给出从增强红外吸收到Fano类型光谱，再到异常红外效应的转化。进一步证明异常红外效应是纳米材料所固有的普遍现象并与纳米材料的尺寸和聚集状态密切相关。研究还发现团聚态的Pt纳米粒子对甲醇氧化具有较好电催化特性。
本论文研究结果对于深入认识金属纳米粒子性能以及探索异常红外效应产生的根源等具有重要意义，同时对研制直接燃料电池电催化剂有应用价值。
As a new rising discipline, nanomaterial has attracted multidisciplinary interests from material science, chemistry, physics, biology and engineering, etc. because of their unusual properties that could not possessed by corresponding bulk materials. Nanomaterial is the core subject of nano- science and technology. Platinum group metals are widely used in energy conversion and green synthesis duo to their high electrocatalytic activity and stability. The research and preparation of metal electrocatalyst at nanometer scale is one of the key subjects in electrocatalysis.
In this paper, Pt nanoparticles (Ptn) were prepared by chemical reduction method. The results of UV-vis and TEM showed that Ptn are formed mainly at the initial stage of refluxing. The prepared Pt nanoparticles were then self-assembled on Au substrate using dithiol as cross-linkers. The ability of electronic transfer during the self-assembly of dithiol and Ptn was studied in the presence of redox active probe Fe (CN) 64-/3- couple. The result indicates that the dithiol monolayer serves as a large barrier for the electron transfer. The redox current is increased significantly when Pt nanoparticles are self-assembled on the top of the dithiol monolayer assembly electrode. The surface morphology and composition of assembly electrode were analyzed by AFM and XPS. In situ FTIRS results illustrated that CO adsorbed on Ptn exhibit enhanced IR absorption, and exhibited more adsorption states in comparison with COad on bulk platinum. Electrochemical CV results illustrated that COad oxidized at higher potential becaus
e of the surface structural effect and nano-size effect of Pt nanoparticles.
In this paper, for the first time, we have revealed that dispersed Pt nanoparticles for CO adsorption display enhanced IR absorption at either solid | electrolyte or solid | gas interface. However abnormal infrared effects (AIREs) was observed for
CO adsorbed on agglomerates of Pt nanoparticles. In order to investigate the origin of the AIREs of nanomaterials, transmission IR spectroscopy was applied to study CO adsorption on Pt nanoparticles with different agglomeration states. The results illustrated that along with the increase of the degree of agglomeration of Pt nanoparticles, the IR spectral patterns of CO adsorbates were transformed from enhanced IR absorption bands to Fano-like spectral line shapes, and further to abnormal anti-absorption IR features. It was demonstrated that the AIREs is a general phenomena of nanomaterials and it is closely related to the size and agglomeration state of nanomaterials. The agglomerates of Pt nanoparticles have also been found to exhibit significant electrocatalytic activity for the oxidation of methanol.
The investigation in the current paper has contributed to understand deeply the nature of the metal nanomaterials, and is of significant importance in understanding the origin of special optical properties of nanometer materials.
引文
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