环境高分辨电子显微术及其在化学科学中的应用
Environmental high resolution electron microscopy and applications to chemical science
摘要:
本文介绍了一种环境池高分辨电子显微镜(EHREM),用于在原子尺度上原位研究动态化学反应。它允许进入催化剂的亚稳中间相和与催化剂的活化、失活和中毒相关的可逆微观结构和化学发展序列。通过空气运输的材料可以被恢复或重建,并且可以保存被常规电子显微镜中的通常真空环境损坏的样品,例如,被脱水损坏的样品。Philips C M30 HRTEM和STEM系统已在我们的实验室中进行了广泛的修改,以增加在0至50 mbar压力的气体或蒸汽的受控气氛中进行原位气-固反应研究的设施,而不是常规的TEM高真空环境。集成的新环境单元功能与原始的0.23 nm TEM分辨率、STEM成像(亮场和环形暗场)以及化学和晶体学显微分析相结合。使用常规的样品架,包括高于1000 ℃的热台。应用实例包括直接研究负载金属颗粒催化剂的动态反应、实际复合氧化物催化剂体系在操作条件下的缺陷和结构变化以及碳微结构。
英文摘要:
An environmental cell high resolution electron microscope (EHREM) has been developed for in situ studies of dynamic chemical reactions on the atomic scale. It allows access to metastable intermediate phases of catalysts and to sequences of reversible microstructural and chemical development associated with the activation, deactivation and poisoning of a catalyst. Materials transported through air can be restored or recreated and samples damaged, e.g. by dehydration, by the usual vacuum environment in a conventional electron microscope can be preserved. A Philips C M30 HRTEM and STEM system has been extensively modified in our laboratory to add facilities for in situ gas-solid reaction studies in controlled atmospheres of gas or vapor at pressures of 0 to 50 mbar, instead of the regular TEM high vacuum environment. The integrated new environmental cell capability is combined with the original 0.23 nm TEM resolution, STEM imaging (bright field and annular dark field) and chemical and crystallographic microanalyses. Regular sample holders are used and include hot stages to higher than 1000 C. Examples of applications include direct studies of dynamic reactions with supported metal particle catalysts, the generation of defects and structural changes in practical complex oxide catalyst systems under operating conditions and carbon microstructures.
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