A review of sample thickness effects on high-resolution transmission electron microscopy imaging

Li, Shouqing; Chang, Yifan; Wang, Yumei; Xu, Qiang; Ge, Binghui

doi:10.1016/j.micron.2019.102813

Cited by 16 publications

(8 citation statements)

References 37 publications

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“…Transmission electron microscopy (TEM) is based on electron–matter interactions to probe the structural and chemical information of a specimen. The TEM specimens must be very thin to avoid multiple scattering of electrons. , Although the acceptable thickness varies with the electron energy and atomic numbers of the sample, specimens thinner than 100 nm are generally required, and “thinner is better” is nearly an invariable axiom in TEM research. Therefore, specimen preparation is crucial for achieving high-resolution imaging and quantitative analysis when the sample is a bulk material.…”

Section: Introductionmentioning

confidence: 99%

Cryogenic Focused Ion Beam Enables Atomic-Resolution Imaging of Local Structures in Highly Sensitive Bulk Crystals and Devices

et al. 2022

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With the development of ultralow-dose (scanning) transmission electron microscopy ((S)TEM) techniques, atomic-resolution imaging of highly sensitive nanomaterials has recently become possible. However, applying these techniques to the study of sensitive bulk materials remains challenging due to the lack of suitable specimen preparation methods. We report that cryogenic focused ion beam (cryo-FIB) can provide a solution to this challenge. We successfully extracted thin specimens from metal–organic framework (MOF) crystals and a hybrid halide perovskite single-crystal film solar cell using cryo-FIB without damaging the inherent structures. The high quality of the specimens enabled the subsequent (S)TEM and electron diffraction studies to reveal complex unknown local structures at an atomic resolution. The obtained structural information allowed us to resolve planar defects in MOF HKUST-1, three-dimensionally reconstruct a concomitant phase in MOF UiO-66, and discover a new CH 3 NH 3 PbI 3 structure and locate its distribution in a single-crystal film perovskite solar cell. This proof-of-concept study demonstrates that cryo-FIB has a unique ability to handle highly sensitive materials, which can substantially expand the range of applications for electron microscopy.

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Section: Introductionmentioning

confidence: 99%

Cryogenic Focused Ion Beam Enables Atomic-Resolution Imaging of Local Structures in Highly Sensitive Bulk Crystals and Devices

et al. 2022

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“…The solid Zn deposition particle starts to present a uniformly porous structure in the fifth cycle, which could be confirmed by the black and white contrast in the transmission electron microscopy (TEM) image in Figure d. (Note that the white contrast zones in the high-resolution TEM (HRTEM) image indicate the lower Zn atom density compared with the black contrast zones Figure e.…”

Section: Resultsmentioning

confidence: 67%

“…Oppositely, it is found that a hybrid aqueous electrolyte (3 M Zn(TfO) 2 /H 2 O/triethyl phosphate (TEP) = 4:1, by weight ratio) could promote the formation of regulated porous Zn anodes. The solid Zn deposition particle 41 ) The regularly microporous Zn in the deposition layer continues to evolve and spreads across the whole Zn layer during continuous cycling, and uniformly distributed "pores" between the deposited Zn nanoparticles could be observed in Figure 2e. Interestingly, the solid Zn deposition particle presents sustainable self-regulation of "pore" structure during repeated Zn deposition−dissolution in the hybrid aqueous electrolyte and finally in situ forms a three-dimensional interconnecting microporous topological Zn electrode (3D-Topo-Zn) (Figure 2f).…”

Section: ■ Results and Discussionmentioning

confidence: 98%

Constructing Three-Dimensional Topological Zn Deposition for Long-Life Aqueous Zn-Ion Batteries

Yan

Huang

Zhao

et al. 2022

ACS Appl. Mater. Interfaces

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Uniform and compact Zn deposition–dissolution is essential to achieve high Coulombic efficiency and long lifespan for Zn anodes. More attention has been commonly focused on the suppression of macroscopic Zn dendrites in the previous reports. The rational control of the microstructure of Zn deposition to prevent the intrinsic volume expansion and pulverization of Zn metal so as to stabilize Zn anodes is less discussed. Herein, we construct a three-dimensional topological Zn deposition at the nanoscale through an in situ electrochemical process in the optimal hybrid aqueous electrolyte. The topological electrode structure can efficiently accommodate microscopic strain and volume variation and thus largely preserve the macroscopic integrity and electrical contact of Zn anodes, leading to enhanced reversibility and stability. With the unique topological structure of Zn deposition, the Coulombic efficiency of Zn anodes could reach >99.9% with excellent cycling over 1182 h at 2 mA cm–2 and 2 mA h cm–2 (Zn utilization: 11.4%). The evolution of “dead” Zn during repeated cycling is first investigated using a homemade semiquantitative analysis method to determine the critical “short slab” for aqueous Zn batteries under the practical application. This work provides an insightful method to regulate the microscopic morphology of Zn deposition for high-performance Zn batteries.

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“…After, the framework is plunge-frozen into a mixture of ethane and propane, in which liquid ethane is also used as a joint cryogenic agent but requires temperature control by the freezing devices . Meanwhile, failure to fully embed the specimen in cryogenic agent can result in radiation damage to the nanomaterials and poor resolution in image; , therefore, optimizing sample distribution and ice thickness in plunge-freezing are required. Finally, the grid is exposed to liquid nitrogen and preserved to be analyzed by the EM.…”

Section: Sample Preparations and Em Setups For Different Nanobio Asse...mentioning

confidence: 99%

Engineered Nanomaterials’ Fate Assessment in Biological Matrices: Recent Milestones in Electron Microscopy

Cota-Ruíz

Cantu

et al. 2021

ACS Sustainable Chem. Eng.

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Engineered nanomaterials undergo a dynamic interaction with matrices such as soil, water, and biological tissues in their lifetime. The investigation and assessment of these interactions is the key to understand the implications that nanotechnology has on different aspects, including biotoxicity, therapeutic efficacy, and overall environmental sustainability. Electron microscopy (EM) is a high-resolution imaging technique that has been rapidly developed to achieve in situ, in vitro, and realtime imaging of nanomaterials in biological matrices. This perspective is the first to review the recent progress on assessing nanobio interaction at different biological levels using EM. We provide a clear picture of different EM configurations with their overall properties and a systematic summary of three main sample preparation methods, such as nanomaterials in dehydrated, frozen, and hydrated matrices. This perspective also provides a thorough discussion on the findings of the past five years on nanobio assessments using EM, such as the identification of nanocorona formation inside seeds during nanoagricultural studies; near-native structural analysis of lipid nanoparticles in nanomedicine studies; and the real-time observation of tumor cell internalization of gold nanoparticle in cancer research. Solving how engineered nanomaterials behave in a biological matrix has made a qualitative leap in nanoresearch. By summarizing recent studies, this perspective discusses the benefits and overall pitfalls of EM in aspects such as the resolution, sampling, and cost.

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A review of sample thickness effects on high-resolution transmission electron microscopy imaging

Cited by 16 publications

References 37 publications

Cryogenic Focused Ion Beam Enables Atomic-Resolution Imaging of Local Structures in Highly Sensitive Bulk Crystals and Devices

Cryogenic Focused Ion Beam Enables Atomic-Resolution Imaging of Local Structures in Highly Sensitive Bulk Crystals and Devices

Constructing Three-Dimensional Topological Zn Deposition for Long-Life Aqueous Zn-Ion Batteries

Engineered Nanomaterials’ Fate Assessment in Biological Matrices: Recent Milestones in Electron Microscopy

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