Electron Microscopy for Materials Science (EMAT) and NANOlab Center of Excellence, University of Antwerp, 2020 Antwerp, Belgium.
Electron Microscopy for Materials Science (EMAT) and NANOlab Center of Excellence, University of Antwerp, 2020 Antwerp, Belgium; Laboratory for Chemistry of Novel Materials, Materials Research Institute, University of Mons, 7000 Mons, Belgium.
Micron. 2023 Jun;169:103444. doi: 10.1016/j.micron.2023.103444. Epub 2023 Mar 21.
High-resolution transmission electron microscopy (TEM) of organic crystals, such as Lead Phthalocyanine (PbPc), is very challenging since these materials are prone to electron beam damage leading to the breakdown of the crystal structure during investigation. Quantification of the damage is imperative to enable high-resolution imaging of PbPc crystals with minimum structural changes. In this work, we performed a detailed electron diffraction study to quantitatively measure degradation of PbPc crystals upon electron beam irradiation. Our study is based on the quantification of the fading intensity of the spots in the electron diffraction patterns. At various incident dose rates (e/Å/s) and acceleration voltages, we experimentally extracted the decay rate (1/s), which directly correlates with the rate of beam damage. In this manner, a value for the critical dose (e/Å) could be determined, which can be used as a measure to quantify beam damage. Using the same methodology, we explored the influence of cryogenic temperatures, graphene TEM substrates, and graphene encapsulation in prolonging the lifetime of the PbPc crystal structure during TEM investigation. The knowledge obtained by diffraction experiments is then translated to real space high-resolution TEM imaging of PbPc.
高分辨率透射电子显微镜(TEM)对有机晶体,如酞菁铅(PbPc)的成像非常具有挑战性,因为这些材料容易受到电子束损伤,在研究过程中导致晶体结构的破坏。为了实现 PbPc 晶体的高分辨率成像,同时最小化结构变化,对损伤进行定量分析是至关重要的。在这项工作中,我们进行了详细的电子衍射研究,以定量测量 PbPc 晶体在电子束辐照下的降解情况。我们的研究基于对电子衍射图谱中斑点强度衰减的定量测量。在不同的入射剂量率(e/Å/s)和加速电压下,我们通过实验提取了衰减率(1/s),该衰减率与束损伤速率直接相关。通过这种方式,可以确定临界剂量(e/Å)的值,作为衡量束损伤的指标。我们使用相同的方法,研究了低温、石墨烯 TEM 衬底和石墨烯封装对延长 PbPc 晶体结构在 TEM 研究过程中的寿命的影响。然后,将衍射实验获得的知识转化为 PbPc 的实空间高分辨率 TEM 成像。