Ortega Eduardo, Ponce Arturo, Santiago Ulises, Alducin Diego, Benitez-Lara Alfredo, Plascencia-Villa Germán, José-Yacamán Miguel
Department of Physics and Astronomy, The University of Texas at San Antonio, One UTSA Circle, San Antonio, TX 78249 USA.
Adv Struct Chem Imaging. 2017;2(1):12. doi: 10.1186/s40679-016-0026-x. Epub 2016 Sep 26.
The present work explores electron diffraction methods for studying the structure of metallic clusters stabilized with thiol groups, which are susceptible to structural damage caused by electron beam irradiation. There is a compromise between the electron dose used and the size of the clusters since they have small interaction volume with electrons and as a consequence weak reflections in the diffraction patterns. The common approach of recording individual clusters using nanobeam diffraction has the problem of an increased current density. Dosage can be reduced with the use of a smaller condenser aperture and a higher condenser lens excitation, but even with those set ups collection times tend to be high. For that reason, the methods reported herein collects in a faster way diffraction patterns through the scanning across the clusters under nanobeam diffraction mode. In this way, we are able to collect a map of diffraction patterns, in areas with dispersed clusters, with short exposure times (milliseconds) using a high sensitive CMOS camera. When these maps are compared with their theoretical counterparts, oscillations of the clusters can be observed. The stability of the patterns acquired demonstrates that our methods provide a systematic and precise way to unveil the structure of atomic clusters without extensive detrimental damage of their crystallinity.
本工作探索了用于研究由硫醇基团稳定的金属团簇结构的电子衍射方法,这些团簇易受电子束辐照引起的结构损伤。由于团簇与电子的相互作用体积小,因此在衍射图案中的反射较弱,所以在使用的电子剂量和团簇尺寸之间存在折衷。使用纳米束衍射记录单个团簇的常用方法存在电流密度增加的问题。使用较小的聚光镜孔径和较高的聚光镜透镜激发可以降低剂量,但即使采用这些设置,采集时间往往也很长。因此,本文报道的方法通过在纳米束衍射模式下扫描团簇以更快的方式收集衍射图案。通过这种方式,我们能够使用高灵敏度CMOS相机在短曝光时间(毫秒)内收集分散团簇区域的衍射图案地图。当将这些地图与其理论对应物进行比较时,可以观察到团簇的振荡。所获取图案的稳定性表明,我们的方法提供了一种系统而精确的方式来揭示原子团簇的结构,而不会对其结晶度造成广泛的有害破坏。