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有机薄膜中电子束损伤的定量分析。

Quantitative Analysis of Electron Beam Damage in Organic Thin Films.

作者信息

Leijten Zino J W A, Keizer Arthur D A, de With Gijsbertus, Friedrich Heiner

机构信息

Laboratory of Materials and Interface Chemistry, Department of Chemical Engineering and Chemistry, and Centre for Multiscale Electron Microscopy, Eindhoven University of Technology, Het Kranenveld 14, Postbus 513-5600 MB, Eindhoven, The Netherlands.

Institute for Complex Molecular Systems, Eindhoven University of Technology, De Zaale, 5612 AJ Eindhoven, The Netherlands.

出版信息

J Phys Chem C Nanomater Interfaces. 2017 May 18;121(19):10552-10561. doi: 10.1021/acs.jpcc.7b01749. Epub 2017 May 9.

Abstract

In transmission electron microscopy (TEM) the interaction of an electron beam with polymers such as P3HT:PCBM photovoltaic nanocomposites results in electron beam damage, which is the most important factor limiting acquisition of structural or chemical data at high spatial resolution. Beam effects can vary depending on parameters such as electron dose rate, temperature during imaging, and the presence of water and oxygen in the sample. Furthermore, beam damage will occur at different length scales. To assess beam damage at the angstrom scale, we followed the intensity of P3HT and PCBM diffraction rings as a function of accumulated electron dose by acquiring dose series and varying the electron dose rate, sample preparation, and the temperature during acquisition. From this, we calculated a critical dose for diffraction experiments. In imaging mode, thin film deformation was assessed using the normalized cross-correlation coefficient, while mass loss was determined via changes in average intensity and standard deviation, also varying electron dose rate, sample preparation, and temperature during acquisition. The understanding of beam damage and the determination of critical electron doses provides a framework for future experiments to maximize the information content during the acquisition of images and diffraction patterns with (cryogenic) transmission electron microscopy.

摘要

在透射电子显微镜(TEM)中,电子束与诸如P3HT:PCBM光伏纳米复合材料之类的聚合物相互作用会导致电子束损伤,这是限制在高空间分辨率下获取结构或化学数据的最重要因素。束流效应会因诸如电子剂量率、成像期间的温度以及样品中水分和氧气的存在等参数而有所不同。此外,束流损伤会在不同的长度尺度上发生。为了评估埃尺度下的束流损伤,我们通过获取剂量系列并改变电子剂量率、样品制备方法以及采集期间的温度,跟踪了P3HT和PCBM衍射环的强度随累积电子剂量的变化。据此,我们计算出了衍射实验的临界剂量。在成像模式下,使用归一化互相关系数评估薄膜变形,而通过平均强度和标准偏差的变化确定质量损失,同时在采集期间也改变电子剂量率、样品制备方法和温度。对束流损伤的理解以及临界电子剂量的确定为未来实验提供了一个框架,以便在使用(低温)透射电子显微镜获取图像和衍射图案时最大化信息含量。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/027b/5442601/a38a9a0f5e31/jp-2017-01749q_0001.jpg

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