Capturing the non-equilibrium state in light–matter–free-electron interactions through ultrafast transmission electron microscopy

Ultrafast transmission electron microscope(UTEM) with the multimodality of time-resolved diffraction, imaging,and spectroscopy provides a unique platform to reveal the fundamental features associated with the interaction between free electrons and matter. In this review, we summarize the principles, instrumentation, and recent developments of the UTEM and its applications in capturing dynamic processes and non-equilibrium transient states. The combination of the transmission electron microscope with a femtosecond laser via the pump–probe method guarantees the high spatiotemporal resolution, allowing the investigation of the transient process in real, reciprocal and energy spaces. Ultrafast structural dynamics can be studied by diffraction and imaging methods, revealing the coherent acoustic phonon generation and photoinduced phase transition process. In the energy dimension, time-resolved electron energy-loss spectroscopy enables the examination of the intrinsic electronic dynamics of materials, while the photon-induced near-field electron microscopy extends the application of the UTEM to the imaging of optical near fields with high real-space resolution. It is noted that light–free-electron interactions have the ability to shape electron wave packets in both longitudinal and transverse directions, showing the potential application in the generation of attosecond electron pulses and vortex electron beams.

Ultrafast photoemission electron microscopy:A multidimensional probe of nonequilibrium physics

Exploring the realms of physics that extend beyond thermal equilibrium has emerged as a crucial branch of condensed matter physics research.It aims to unravel the intricate processes involving the excitations,interactions,and annihilations of quasi-and many-body particles,and ultimately to achieve the manipulation and engineering of exotic non-equilibrium quantum phases on the ultrasmall and ultrafast spatiotemporal scales.Given the inherent complexities arising from many-body dynamics,it therefore seeks a technique that has efficient and diverse detection degrees of freedom to study the underlying physics.By combining high-power femtosecond lasers with real-or momentum-space photoemission electron microscopy(PEEM),imaging excited state phenomena from multiple perspectives,including time,real space,energy,momentum,and spin,can be conveniently achieved,making it a unique technique in studying physics out of equilibrium.In this context,we overview the working principle and technical advances of the PEEM apparatus and the related laser systems,and survey key excited-state phenomena probed through this surface-sensitive methodology,including the ultrafast dynamics of electrons,excitons,plasmons,spins,etc.,in materials ranging from bulk and nano-structured metals and semiconductors to low-dimensional quantum materials.Through this review,one can further envision that time-resolved PEEM will open new avenues for investigating a variety of classical and quantum phenomena in a multidimensional parameter space,offering unprecedented and comprehensive insights into important questions in the field of condensed matter physics.

Recent progress on advanced transmission electron microscopy characterization for halide perovskite semiconductors

Halide perovskites are strategically important in the field of energy materials. Along with the rapid development of the materials and related devices, there is an urgent need to understand the structure–property relationship from nanoscale to atomic scale. Much effort has been made in the past few years to overcome the difficulty of imaging limited by electron dose,and to further extend the investigation towards operando conditions. This review is dedicated to recent studies of advanced transmission electron microscopy(TEM) characterizations for halide perovskites. The irradiation damage caused by the interaction of electron beams and perovskites under conventional imaging conditions are first summarized and discussed. Low-dose TEM is then discussed, including electron diffraction and emerging techniques for high-resolution TEM(HRTEM) imaging. Atomic-resolution imaging, defects identification and chemical mapping on halide perovskites are reviewed. Cryo-TEM for halide perovskites is discussed, since it can readily suppress irradiation damage and has been rapidly developed in the past few years. Finally, the applications of in-situ TEM in the degradation study of perovskites under environmental conditions such as heating,biasing, light illumination and humidity are reviewed. More applications of emerging TEM characterizations are foreseen in the coming future, unveiling the structural origin of halide perovskite’s unique properties and degradation mechanism under operando conditions, so to assist the design of a more efficient and robust energy material.

Application of electron microscopy in gastroenterology

Electron microscopy has long been used in research in the fields of life sciences and materials sciences.Transmission and scanning electron microscopy and energy-dispersive X-ray spectroscopy(EDX)analyses have also been performed in the field of gastroenterology.Electron microscopy and EDX enable(1)Observation of ultrastructural differences in esophageal epithelial cells in patients with gastroesophageal reflux and eosinophilic esophagitis;(2)Detection of lanthanum deposition in the stomach and duodenum;(3)Ultrastructural and elemental analyses of enteroliths and bezoars;(4)Detection and characterization of microorganisms in the gastrointestinal tract;(5)Diagnosis of gastrointestinal tumors with neuroendocrine differentiation;and(6)Analysis of gold nanoparticles potentially used in endoscopic photodynamic therapy.This review aims to foster a better understanding of electron microscopy applications by reviewing relevant clinical studies,basic research findings,and the state of current research carried out in gastroenterology science.

Fixation methods for electron microscopy of human and other liver

For an electron microscopic study of the liver,expertise and complicated,time-consuming processing of hepatic tissues and cells is needed.The interpretation of electron microscopy(EM) images requires knowledge of the liver fine structure and experience with the numerous artifacts in fixation,embedding,sectioning,contrast staining and microscopic imaging.Hence,the aim of this paper is to present a detailed summary of different methods for the preparation of hepatic cells and tissue,for the purpose of preserving long-standing expertise and to encourage new investigators and clinicians to include EM studies of liver cells and tissue in their projects.

A review of in situ transmission electron microscopy study on the switching mechanism and packaging reliability in non-volatile memory

Non-volatile memory(NVM)devices with non-volatility and low power consumption properties are important in the data storage field.The switching mechanism and packaging reliability issues in NVMs are of great research interest.The switching process in NVM devices accompanied by the evolution of microstructure and composition is fast and subtle.Transmission electron microscopy(TEM)with high spatial resolution and versatile external fields is widely used in analyzing the evolution of morphology,structures and chemical compositions at atomic scale.The various external stimuli,such as thermal,electrical,mechanical,optical and magnetic fields,provide a platform to probe and engineer NVM devices inside TEM in real-time.Such advanced technologies make it possible for an in situ and interactive manipulation of NVM devices without sacrificing the resolution.This technology facilitates the exploration of the intrinsic structure-switching mechanism of NVMs and the reliability issues in the memory package.In this review,the evolution of the functional layers in NVM devices characterized by the advanced in situ TEM technology is introduced,with intermetallic compounds forming and degradation process investigated.The principles and challenges of TEM technology on NVM device study are also discussed.

Scanning transmission electron microscopy: A review of high angle annular dark field and annular bright field imaging and applications in lithium-ion batteries

Scanning transmission electron microscopy(STEM) has been shown as powerful tools for material characterization,especially after the appearance of aberration-corrector which greatly enhances the resolution of STEM. High angle annular dark field(HAADF) and annular bright field(ABF) imaging of the aberration-corrected STEM are widely used due to their high-resolution capabilities and easily interpretable image contrasts. However, HAADF mode of the STEM is still limited in detecting light elements due to the weak electron-scattering power. ABF mode of the STEM could detect light and heavy elements simultaneously, providing unprecedented opportunities for probing unknown structures of materials. Atomiclevel structure investigation of materials has been achieved by means of these imaging modes, which is invaluable in many fields for either improving properties of materials or developing new materials. This paper aims to provide a introduction of HAADF and ABF imaging techniques and reviews their applications in characterization of cathode materials, study of electrochemical reaction mechanisms, and exploring the effective design of lithium-ion batteries(LIBs). The future prospects of the STEM are also discussed.

Transmission Electron Microscopy as a Powerful Tool for Investigating Lithium-ion Battery Materials

Transmission electron microscopy(TEM) stands out as one of the most powerful tools for characterizing materials at multiple scales and dimensions. This unique technique has nowadays been widely employed in investigating the lithium-ion battery(LIB) materials. The present perspective paper focuses on several LIB related aspects that are recently revealed by using TEM. Finally, we present outlook on the future directions of TEM for LIB research and development.

Imaging Ultrafast Plasmon Dynamics within a Complex Dolmen Nanostructure Using Photoemission Electron Microscopy

We report direct nanoscale imaging of ultrafast plasmon in a gold dolmen nanostructure excited with the 7fs laser pulses by combining the interferometric time-resolved technology with the three-photon photoemission electron microscopy(PEEM).The interferometric time-resolved traces show that the plasmon mode beating pattern appears at the ends of the dimer slabs in the dolmen nanostructure as a result of coherent superposition of multiple localized surface plasmon modes induced by broad bandwidth of the ultrafast laser pulses.The PEEM measurement further discloses that in-phase of the oscillation field of two neighbor defects are surprisingly observed,which is attributed to the plasmon coupling between them.Furthermore,the control of the temporal delay between the pump and probe laser pluses could be utilized for manipulation of the near-field distribution.These findings deepen our understanding of ultrafast plasmon dynamics in a complex nanosystem.

Visualization of atomic scale reaction dynamics of supported nanocatalysts during oxidation and ammonia synthesis using in-situ environmental(scanning) transmission electron microscopy

Reaction dynamics in gases at operating temperatures at the atomic level are the basis of heterogeneous gas-solid catalyst reactions and are crucial to the catalyst function.Supported noble metal nanocatalysts such as platinum are of interest in fuel cells and as diesel oxidation catalysts for pollution control,and practical ruthenium nanocatalysts are explored for ammonia synthesis.Graphite and graphitic carbons are of interest as supports for the nanocatalysts.Despite considerable literature on the catalytic processes on graphite and graphitic supports,reaction dynamics of the nanocatalysts on the supports in different reactive gas environments and operating temperatures at the single atom level are not well understood.Here we present real time in-situ observations and analyses of reaction dynamics of Pt in oxidation,and practical Ru nanocatalysts in ammonia synthesis,on graphite and related supports under controlled reaction environments using a novel in-situ environmental(scanning) transmission electron microscope with single atom resolution.By recording snapshots of the reaction dynamics,the behaviour of the catalysts is imaged.The images reveal single metal atoms,clusters of a few atoms on the graphitic supports and the support function.These all play key roles in the mobility,sintering and growth of the catalysts.The experimental findings provide new structural insights into atomic scale reaction dynamics,morphology and stability of the nanocatalysts.

Characterization of swift heavy ion tracks in MoS2 by transmission electron microscopy

The various morphologies of tracks in MoS2 irradiated by swift heavy ions at normal and 30° incidence with 9.5–25.0 MeV/u 86Kr, 129Xe, 181Ta, and 209Bi ions were investigated by transmission electron microscopy. The diameter of ion tracks increases from 1.9 nm to 4.5 nm with increasing electronic energy loss. The energy loss threshold of the track formation in MoS2 is predicted as about 9.7 keV/nm based on the thermal spike model and it seems consistent with the experimental results. It is shown that the morphology of ion tracks is related to the penetration length of ions in MoS2. The formation process of ion tracks is discussed based on the cooperative process of outflow and recrystallization of the molten phase during rapid quenching.

Improvement of femtosecond SPPs imaging by two-color laser photoemission electron microscopy

Clear imaging of surface plasmon polaritons(SPPs)is a prerequisite for SPPs-based applications.In this work,we demonstrate an improvement of near-field imaging of SPPs via directly comparing the visibility of the photoemission electron microscopy(PEEM)image of SPPs under one-and two-color laser excitation(also known as one-or two-color laser PEEM).By measuring the photoelectron yield and the contrast of the interference fringes of SPPs,we demonstrate that in addition to enhancing the photoemission yield,two-color laser PEEM can significantly improve the contrast between bright and dark fringes(nearly 4 times higher than that of one-color laser case).By recording the nonlinear order of the photoelectrons ejected from the bright and dark fringes,respectively,the underlying mechanism for the improved visibility is revealed.In addition,the influences of the polarization direction of 400-nm laser on the PEEM images of the SPPs with different wave vector directions are shown.These results can provide technical support for the development of SPPs-based communication devices and catalysis.

High Resolution Electron Microscopy Observations of Structural Changes in Iron Nitride Films Annealed in Vacuum

Iron-nitride films were prepared by reactive sputtering, and the effect of annealing treatment on the structures was investigated by means of in-situ electron microscopy and high resolution electron microscopy (HREM). As-deposited films were observed to be a mixed structure of a few ultrafine ε-Fe2-3N particles existing in the amorphous matrix. lt was found that the structurerelaxation in the amorphous occurred at 473 K, and the ultrafine grains began to grow at the higher annealing temperatures. The transition of the amorphous to ε-Fe2-3N was almost completed at 673 K. It is considered that the formation of the ideal ε-Fe3N is originated from the ordering of the nitrogen atoms during the annealing in vacuum. On the other hand, γ’-phase (Fe4N) was seen to precipitation of ε-phase at 723 K. Two possible modes are proposed in the precipitation of γ’-phase, depending on the heating rate and crystallographic orientation relationships. i.e. [121]ε [001]γ, (210)ε(110)γ and [100]ε[110]γ, (001)ε(111)γ. In addition,α-Fe particles were observed to form from the γ’-phase at high temperatures. We assumed that these structural changes are due to the diffusion of nitrogen and iron atoms during the annealing,except for the case of the precipitation of the γ’-phase as depicted above. The results obtained in this work are in a good agreement with the assumption.

Nucleation and Growth of Thallium on Thin Film Mercury Electrode: Voltammetric, Scanning Electron Microscopy, Chronoamperometric and Electrochemical Impedance Studies

Thallium is a heavy metal highly toxic to the biosphere. It can be determined by anodic stripping voltammetry after deposition on mercury film. The aim of this work is to study the conditions and mechanisms of deposition of Hg on glassy carbon electrode and Tl on Hg film by cyclic voltammetry, scanning electron microscopy, chronoamperometry and impedance techniques. The results showed a germination and growth of a 3D Hg phase on glassy carbon electrode. Similarly, the electrodeposition of Tl on Hg follows a 3D three-dimensional nucleation with diffusion controlled growth. The impedance measurements reveal an easier charge transfer on the Tl film.

Scanning Electron Microscopy (SEM) of the Bug Eye and Sand Coral

We present a Scanning Electron Microscopy (SEM) technique for the characterisation of biological and non-biological samples at nano-scale level. Scanning Electron Microscopy has been around for a long while especially in material science laboratories in developed countries. The SEM has enabled scientist to have a better understanding of microstructure by providing unsurpassed optical magnifications of samples. In this introductory paper, we introduce the techniques of using SEM to capture highly magnified microstructure of a fly found on an African soybean (Glycine max) seed. We are able to estimate the number of lenses in each eye and zoom into features that could describe its life characteristics. Hexagonal lenses are estimated to have sizes ranging from 14 um to 19 um. This paper also presents a finding of a sea coral “pie like structure” on a single grain of sand used for water filtration.

ELECTRON MICROSCOPY STUDIES OF LENS FROM TWO CASES OF OCULAR SIDEROSIS

Cases report Case 1: A 50-year-old man was injuried by iron filings on his left eye. He was admitted to our hospital on Feb. 3, 1987. On examination, his visual acuity was 20/15 OD and 20/500 OS. Left eye: The cornea was clear, the anterior chamber depth was 3 CT, tyndall(-). Iris pattern is clear, pupil was 3.5×3.5mm. Dilated pupil examination: There were scattered brown-yellow ironrust under anterior capsule and the lens cortex had become totally opaque. Nuclear, posterior capsule and fundus can't be ...

Tracking lithiation with transmission electron microscopy

Li-ion batteries(LIBs)have dominated energy-storage techniques for portable electronic devices and electric cars,and are expanding their territory into the large-scale energy storage.The energy storage of LIBs is realized by the reversible shuttle of lithium ions between electrodes.It is essential to track the lithium diffusion and obtain a profound insight into the lithiation mechanism during the work cycle of LIBs.Transmission electron microscopy(TEM)is a powerful tool for the structural characterization,which can provide the information about the lithiation at the atomic scale.In this review,we summarize the research frontiers of TEM applications on LIBs.We introduce the techniques for the direct observation of Li species in LIB-related materials.Especially,the application of cryo-TEM is highlighted.Moreover,in-situ TEM technique is further discussed since it shows great advantages in studying the dynamical structure changes of LIBs.The perspectives and strategies in this review offer feasible guidance for researchers to further improve the performance of LIBs.

Characterization of local chemical ordering and deformation behavior in high entropy alloys by transmission electron microscopy

Short-range ordering(SRO)is one of the most important structural features of high entropy alloys(HEAs).However,the chemical and structural analyses of SROs are very difficult due to their small size,complexed compositions,and varied locations.Transmission electron microscopy(TEM)as well as its aberration correction techniques are powerful for characterizing SROs in these compositionally complex alloys.In this short communication,we summarized recent progresses regarding characterization of SROs using TEM in the field of HEAs.By using advanced TEM techniques,not only the existence of SROs was confirmed,but also the effect of SROs on the deformation mechanism was clarified.Moreover,the perspective related to application of TEM techniques in HEAs are also discussed.

Revealing structural degradation in layered structure oxides cathode of lithium ion batteries via in-situ transmission electron microscopy

Transition metal oxides with layered structure have been widely used as cathode materials for lithium-ion batteries(LIBs)which have relatively high energy density,large capacity and long life.However,in the long-term electrochemical cycle,the inevitable degradation of performance of LIBs due to structural degradation in cathodes severely restricts their large-scale practical applications.Understanding the underlying mechanism of structural degradation is the most critical scientific problem.Recently,in situ transmission electron microscopy(TEM)has become a useful tool to study the structural and compositional evolutions at atomic scale in electrochemical reactions,which provided a unique and in-depth understanding of the structural degradation.In this review,we discuss the recent advances in the in situ TEM,focusing on its role in revealing the structural degradation mechanisms in the four key places:(1)the interface between the cathodes and electrolyte;(2)the cathode surface;(3)the particle interior and(4)those induced by thermal effect.The insight gained by the in-situ TEM which is still developing at its fast pace is unique and expected to provide guidance for designing better layered cathode materials.

Single Molecule Imaging with Liquid Phase Electron Microscopy

Few single-molecule experiments have enabled the direct imaging of functional biomacromolecules in real-time in their native liquid environments,resolving their conformational adaptations,transient interactions,and intermediate states.Liquid phase electron microscopy(LP-EM),due to its unique combination of spatial and temporal resolution,has shown to be a promising tool.Recent experiments have enabled successful imaging of intact structures of organic molecules and biological systems with an ordinary electron microscope.Adapting image processing methods and quantitative data analysis from single particle experiments based on the optical microscope,quantifying motion and relaxation of these interacting molecules allows the experimental observations of pathways,to test theoretical predictions,and discovery of new mechanisms.Combining LP-EM with tomography,fluorescence,and mass spectroscopy allows for probing multi-dimensional structural and dynamic information.Challenges remain in obtaining high-quality data in large quantities,which can be improved by developing new liquid cell platforms and machine learning-based data analysis.