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Quantitative Analysis of Electron Beam Damage in Organic Thin Films

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      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.

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      Radiation damage in the TEM and SEM.

      We review the various ways in which an electron beam can adversely affect an organic or inorganic sample during examination in an electron microscope. The effects considered are: heating, electrostatic charging, ionization damage (radiolysis), displacement damage, sputtering and hydrocarbon contamination. In each case, strategies to minimise the damage are identified. In the light of recent experimental evidence, we re-examine two common assumptions: that the amount of radiation damage is proportional to the electron dose and is independent of beam diameter; and that the extent of the damage is proportional to the amount of energy deposited in the specimen.
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        Towards automated diffraction tomography: part I--data acquisition.

         U. Kolb,  T Gorelik,  C Kübel (2007)
        The ultimate aim of electron diffraction data collection for structure analysis is to sample the reciprocal space as accurately as possible to obtain a high-quality data set for crystal structure determination. Besides a more precise lattice parameter determination, fine sampling is expected to deliver superior data on reflection intensities, which is crucial for subsequent structure analysis. Traditionally, three-dimensional (3D) diffraction data are collected by manually tilting a crystal around a selected crystallographic axis and recording a set of diffraction patterns (a tilt series) at various crystallographic zones. In a second step, diffraction data from these zones are combined into a 3D data set and analyzed to yield the desired structure information. Data collection can also be performed automatically, with the recent advances in tomography acquisition providing a suitable basis. An experimental software module has been developed for the Tecnai microscope for such an automated diffraction pattern collection while tilting around the goniometer axis. The module combines STEM imaging with diffraction pattern acquisition in nanodiffraction mode. It allows automated recording of diffraction tilt series from nanoparticles with a size down to 5nm.
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          Relation between Photoactive Layer Thickness, 3D Morphology, and Device Performance in P3HT/PCBM Bulk-Heterojunction Solar Cells

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            Author and article information

            Affiliations
            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
            Author notes
            [* ]E-mail h.friedrich@ 123456tue.nl ; phone +31 (0)40 247 3041 (H.F.).
            Journal
            J Phys Chem C Nanomater Interfaces
            J Phys Chem C Nanomater Interfaces
            jy
            jpccck
            The Journal of Physical Chemistry. C, Nanomaterials and Interfaces
            American Chemical Society
            1932-7447
            1932-7455
            09 May 2017
            18 May 2017
            : 121
            : 19
            : 10552-10561
            5442601 10.1021/acs.jpcc.7b01749
            Copyright © 2017 American Chemical Society

            This is an open access article published under a Creative Commons Non-Commercial No Derivative Works (CC-BY-NC-ND) Attribution License, which permits copying and redistribution of the article, and creation of adaptations, all for non-commercial purposes.

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            jp7b01749
            jp-2017-01749q

            Thin films & surfaces

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