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Imaging Beam‐Sensitive Materials by Electron Microscopy REVIEW www.advmat.de Imaging Beam-Sensitive Materials by Electron Microscopy Qiaoli Chen, Christian Dwyer, Guan Sheng, Chongzhi Zhu, Xiaonian Li, Changlin Zheng,* and Yihan Zhu* materials science and associated research Electron microscopy allows the extraction of multidimensional fields. A major challenge in these fields lies spatiotemporally correlated structural information of diverse materials down in the direct observation of the intrinsic to atomic resolution, which is essential for figuring out their structure– and dynamic properties of diverse mate- property relationships. Unfortunately, the high-energy electrons that carry this rials in multidimensions and at the atomic scale, including their structures, chemical important information can cause damage by modulating the structures of the compositions, electronic states, and spins. materials. This has become a significant problem concerning the recent boost Accordingly, the roadmap of TEM tech- in materials science applications of a wide range of beam-sensitive materials, nological and methodological innovations including metal–organic frameworks, covalent–organic frameworks, organic– has involved great efforts devoted to the inorganic hybrid materials, 2D materials, and zeolites. To this end, developing pursuit of higher spatial resolution, more electron microscopy techniques that minimize the electron beam damage for correlated structural information and less electron beam damage. In the aspect of the extraction of intrinsic structural information turns out to be a compelling pushing the spatial resolution limits of but challenging need. This article provides a comprehensive review on the electron microscopy, advanced aberration revolutionary strategies toward the electron microscopic imaging of beam- correction techniques[1] or ptychographic sensitive materials and associated materials science discoveries, based on diffractive imaging methods[2] nowadays the principles of electron–matter interaction and mechanisms of electron allow the imaging of nanoscale objects down to atomic- or even deep sub-Ång- beam damage. Finally, perspectives and future trends in this field are put strom resolution. In addition, modern forward. TEM instruments unite various spectro- scopic and in situ (operando) techniques and provide multidimensional correlated 1. Introduction structural, chemical and electronic information spanning the spatial,[3] time,[4–8] energy,[9] and momentum dimensions.[10] Developments in transmission electron microscopy (TEM) Such high-resolution and correlated information is important in are largely motivated by the quest for essential information in providing a solid basis for the determination of structure–prop- erty relationships in materials. Notwithstanding this, electrons interact very strongly with materials, which might inevitably Prof. Q. Chen, C. Zhu, Prof. X. Li, Prof. Y. Zhu Center for Electron Microscopy introduce temporary or permanent structural changes, typically State Key Laboratory Breeding Base of Green Chemistry Synthesis through atomic displacements or electronic excitations. Thus, Technology and College of Chemical Engineering the development of TEM techniques and methods for imaging Zhejiang University of Technology materials that are highly vulnerable to electron beam irradia- Hangzhou 310014, China tion becomes crucial. In fact, while successful applications of E-mail: [email protected] low-dose cryogenic-TEM techniques[11–14] and single-particle Prof. C. Dwyer [15,16] Department of Physics tomography (SPT) methods have boosted developments Arizona State University in structural biology in the past decades,[17] knowledge of elec- Tempe, AZ 85287-1504, USA tron beam damage in a wider range of materials science speci- G. Sheng mens remains fragmentary by comparison, and corresponding Advanced Membranes and Porous Materials Center TEM imaging technologies and methodologies are much less Physical Science and Engineering King Abdullah University of Science and Technology explored until recently. Thuwal 23955-6900, Kingdom of Saudi Arabia Actually, many aspects of the latest advances in materials Prof. C. Zheng science research are exactly pioneered by the synthesis and State Key Laboratory of Surface Physics and Department of Physics application of materials which happen to be beam-sensitive. Fudan University Such materials include i) inorganic materials containing light Shanghai 200438, China metals,[18,19] zeolites,[20–24] and low-dimensional materials (e.g., E-mail: [email protected] graphene, carbon nanotubes, and molybdenum disulfide);[25–27] The ORCID identification number(s) for the author(s) of this article can be found under https://doi.org/10.1002/adma.201907619. ii) organic materials like covalent–organic frameworks (COFs),[28,29] macromolecules,[30–32] and polymers;[33] and DOI: 10.1002/adma.201907619 iii) organic–inorganic hybrid materials like metal–organic Adv. Mater. 2020, 32, 1907619 1907619 (1 of 42) © 2020 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.advancedsciencenews.com www.advmat.de frameworks (MOFs)[34–36] and organic–inorganic hybrid perov- skites.[34,37] These materials have intriguing physicochemical Qiaoli Chen is an associate properties and promising applications,[38–44] and direct imaging professor in the College in the TEM provides a powerful tool to correlate, not only bulk of Chemical Engineering structure, but also local structure with their properties at the at Zhejiang University of atomic scale. This is, however, constrained by the fact that their Technology (China). She structures degrade rapidly during TEM imaging upon the expo- received her Ph.D. degree sure to electrons above a certain kinetic energy, dose rate or in physical chemistry from accumulated dose.[24,45] For example, MOFs comprise a large Xiamen University (China) family of porous crystalline materials featuring highly design- in 2018 and was a visiting able and flexible pore architectures, framework topologies and scholar at Emory University structural functionalities, and they hold great promise for a during 2016–2017. Her wide range of applications, such as gas separation and storage, research interests include sensing, and catalysis.[46–48] However, an unambiguous struc- chemical synthesis and structural elucidation of nanostruc- ture determination of MOFs through TEM imaging is unfor- tured materials using combined electron microscopy and tunately very challenging because most MOFs typically collapse diffraction techniques. after exposure to only a few electrons Å–2.[34,35,49] As another example, graphene, well known for its 2D structure, unprece- Changlin Zheng is a pro- dented mechanical strength and high charge carrier mobility, is fessor in the Department of susceptible to degradation for electron beam energies exceeding [45] Physics at Fudan University 80 keV. As yet another example, a major barrier to the next- (China). He received his generation lithium-ion batteries (LIB) involves the growth of Ph.D. degree in physics from dendrites on the anodes (e.g., lithium-metal anode), which also the Humboldt University of falls beyond the capability of conventional TEM characteriza- Berlin (Germany) in 2009 tion due to the high electron vulnerability of lithium and its [50] and worked as a research related phases. Such examples highlight the severe restric- fellow at Monash Centre for tions that must be imposed on TEM imaging of beam-sensitive Electron Microscopy, Monash materials. These restrictions largely limit the accessible image University (Australia) from resolution and signal-to-noise ratio (SNR) for the reasonable 2010–2017. His research identification and interpretation of the intrinsic materials struc- interests focus on the development of advanced electron tures. To this end, the development of revolutionary TEM tech- microscopy techniques (diffraction, imaging, and spectros- nologies and methodologies for imaging irradiation-vulnerable copy) and their applications in condensed matter physics materials is at the cutting edge of many emerging fields in and materials science. materials science, and will dramatically accelerate the pace of groundbreaking discoveries in these fields. In this review, we systematically summarize the recently Yihan Zhu works as a developed strategies to overcome electron beam damage in professor in the Center for TEM imaging, including both instrumental and methodolog- Electron Microscopy and ical innovations, with an emphasis on the basic principles of the College of Chemical electron–matter interactions and mechanisms of electron beam Engineering at Zhejiang damage. Applications of these strategies and associated funda- University of Technology mental discoveries in materials science are presented. Finally, a (China). He received his short discussion on the perspectives and future trends is given. Ph.D. degree in chemistry at Zhejiang University (China) in 2010. During 2010–2017, 2. Physical Origin and Behavior of Electron he worked as a postdoctoral Beam Damage fellow and research scientist at King Abdullah University of Science and Technology. 2.1. Basic Principles of Electron–Matter Interaction His research interests now focus on low-dose electron microscopy and structural elucidation of beam-sensitive As probing particles, electrons interact much more strongly with materials for applications such as catalysis, gas separation, condensed matter compared to X-ray photons and neutrons. and energy conversion/storage. Owing to Coulomb interactions, the cross-section for electrons to scatter from atoms
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