He Qianping, Chen Jihua, Keffer David J, Joy David C
Department of Chemical and Biomolecular Engineering, University of Tennessee, Knoxville, Tennessee.
Scanning. 2014 May-Jun;36(3):338-46. doi: 10.1002/sca.21117. Epub 2013 Jul 29.
Electron microscopy is an essential tool for the evaluation of microstructure and properties of the catalyst layer (CL) of proton exchange membrane fuel cells (PEMFCs). However, electron microscopy has one unavoidable drawback, which is radiation damage. Samples suffer temporary or permanent change of the surface or bulk structure under radiation damage, which can cause ambiguity in the characterization of the sample. To better understand the mechanism of radiation damage of CL samples and to be able to separate the morphological features intrinsic to the material from the consequences of electron radiation damage, a series of experiments based on high-angle annular dark-field-scanning transmission scanning microscope (HAADF-STEM), energy filtering transmission scanning microscope (EFTEM), and electron energy loss spectrum (EELS) are conducted. It is observed that for thin samples (0.3-1 times λ), increasing the incident beam energy can mitigate the radiation damage. Platinum nanoparticles in the CL sample facilitate the radiation damage. The radiation damage of the catalyst sample starts from the interface of Pt/C or defective thin edge and primarily occurs in the form of mass loss accompanied by atomic displacement and edge curl. These results provide important insights on the mechanism of CL radiation damage. Possible strategies of mitigating the radiation damage are provided.
电子显微镜是评估质子交换膜燃料电池(PEMFC)催化剂层(CL)微观结构和性能的重要工具。然而,电子显微镜有一个不可避免的缺点,即辐射损伤。在辐射损伤下,样品的表面或整体结构会发生暂时或永久性变化,这可能导致样品表征出现模糊性。为了更好地理解CL样品的辐射损伤机制,并能够将材料固有的形态特征与电子辐射损伤的后果区分开来,开展了一系列基于高角度环形暗场扫描透射显微镜(HAADF-STEM)、能量过滤透射扫描显微镜(EFTEM)和电子能量损失谱(EELS)的实验。观察到对于薄样品(0.3-1倍λ),增加入射束能量可以减轻辐射损伤。CL样品中的铂纳米颗粒会加剧辐射损伤。催化剂样品的辐射损伤从Pt/C界面或有缺陷的薄边缘开始,主要以质量损失的形式发生,伴有原子位移和边缘卷曲。这些结果为CL辐射损伤机制提供了重要见解。还提供了减轻辐射损伤的可能策略。