Ultra-high voltage electron microscopy: Past,present, and future

High voltage electron microscopy has shown numerous advantages for the study of natural science, including biology, but it is especially useful in materials science. The most important advantage for materials science is in-situ experiments on detailed processes of the same phenomena that occur in bulk materials. For such in-situ experiments, the specimens should be thicker than a few microns to observe the behavior of lattice effect. The maximum observable thickness of the specimens and other advantages markedly increase with increasing accelerating voltage, and since 1965, two 3 MV instruments have been installed. The present paper is mainly concerned with these 3 MV electron microscopes and their applications to new research fields.     

The research center for ultra-high voltage electron microscopy at Osaka University

High-voltage electron microscopy has shown itself advantageous for the study of natural science, including biology, but especially for materials science. The most important advantage for materials science is for in situ experiments about the detailed processes of the phenomena that occur in bulk materials. The present paper is mainly concerned with several types of in situ experiments that have been carried out in the Research Center for Ultra-High Voltage Electron Microscopy, Osaka University. The following subjects have been studied: (a) fundamental problems, such as the conditions necessary for in situ experiments, functional features of specimen treatment devices, and the effects of electron irradiation; (b) the dislocation behavior of crystals under various conditions; (c) high-temperature behavior of refractory materials, mainly ceramic composites; (d) new applications of electron irradiation effects, such as amorphization of crystalline materials and electron-irradiation-induced foreign-atom implantation; (e) environment-matter interaction, mainly chemical amorphization of alloys; and (f) future trends of the in situ experiment, such as combinations with Auger valency electron spectroscopy and high-resolution electron microscopy.     

The initial stages of ordering in alloys studied by electron diffraction and high resolution microscopy

The combined use of selected area electron diffraction and high resolution electron microscopy can provide important information about the microstructure of materials. Both techniques have been applied to study the ordering behaviour in a number of alloys. The ordering process is not always straightforward and mostly intermediate long period modulated structures are formed. Using dark field high resolution electron microscopy the ordering sequence as well as the structure of the intermediate phases have been established for Au₄Mn and Au₅Mn₂. For Ni₄Mo the high resolution observations provide new information about the ordering mechanism in its very earliest stages.     

扫描离子电导显微镜技术及其在纳米生物学研究中的应用

扫描探针显微镜技术的出现开辟生命科学研究的新纪元并逐步发展成为在纳米尺度研究细胞结构与功能的一类新型的显微镜技术。扫描离子电导显微镜技术就是新近发展起来的这一扫描探针显微镜技术家族中的一员,可被用来在生理条件下、高分辨率及非接触地研究活细胞的表面形貌,从而帮助人们深入研究细胞微观结构与功能的关系。本文简要介绍扫描离子电导显微镜技术的基本原理,并结合国外研究现状综述该技术在纳米生物学研究中的应用。     

Lorentz phase microscopy of magnetic materials

We propose a method of Lorentz phase microscopy for in situ studies and imaging magnetic materials in transmission electron microscopy (TEM) based on the solution of the magnetic transport-of-intensity equation. We also describe the appropriate way of solving this equation that may be useful for understanding and practical use of non-holographic methods for phase retrieval in electron microscopy, especially in imaging magnetic materials. The method is simple, since it is primarily based on classical Fresnel imaging. On the other hand, it is quantitative and can be applied in any TEM without changing the basic hardware. Therefore, it may well find important practical applications in ultramicroscopy and modern magnetic materials research.     

Correlative microscopy of detergent granules

The microstructure of detergent products for textile cleaning determines to a large extent the physical properties of these products. Correlative microscopy was used to reveal the microstructure by reconciling images obtained by scanning electron microscopy with energy dispersive X-ray analysis, X-ray microtomography and Fourier transform infrared microscopy. These techniques were applied on the same location of a subsample of a spray-dried detergent base powder embedded in polyacrylate. In this way, the three-dimensional internal and external structure of detergent granules could be investigated from milli to nano scale with detailed spatial information about the components present. This will generate knowledge how to design optimal microstructures for laundry products to obtain product properties demanded by the market. This method is also very useful for other powder systems used in a large variety of industries (e.g. for pharmaceutical, food, ceramic and metal industries).     

Characterization of the near-surface layers of carbon steels modified by interaction with intense pulsed plasma beams: scanning electron microscopy investigations

Modification of materials is a wide area in materials science, especially surface modification. To investigate the results of the modification process, treated and nontreated samples were compared. Intense plasma pulses of argon or nitrogen were used to irradiate the carbon steels. In all samples, the near‐surface layer was melted. Results of scanning electron microscopy investigations of the surface morphology and cross‐sections, as well as the results of tribological tests, are presented. The obtained results allowed us to draw conclusions about changes in material properties and to propose subsequent studies using other investigation techniques.     

Electron microscopy of quantum dots

This brief review describes the different types of semiconductor quantum dot systems, their main applications and which types of microscopy methods are used to characterize them. Emphasis is put on the need for a comprehensive investigation of their size distribution, microstructure, chemical composition, strain state and electronic properties, all of which influence the optical properties and can be measured by different types of imaging, diffraction and spectroscopy methods in an electron microscope.     

Transmission electron microscopy of interfaces in structural ceramic composites

Ceramic composites based either on a particulate, fibre or a lamellar architecture are potentially useful as damage-tolerant high-temperature engineering materials. The ability of the interfaces in such systems to deflect cracks is vital to the damage tolerance of these materials. Transmission electron microscopy techniques enable the chemical and physical characterization of these interfaces, providing information on interlayer thicknesses, chemical species, local bonding and the microstructural features which give rise to the interfacial properties, thereby enabling a full understanding not only of composites after processing, but also after exposure to aggressive environments such as air at high temperature. Examples of the application of transmission electron microscopy to all three composite architectures are described.     

The importance of microscopy in studying the wear behaviour of ceramic surfaces

This paper demonstrates how careful microscopy of worn ceramic surfaces can be used to provide information on the mechanisms of material removal. This information is necessary as a critical complement to wear-rate data obtainable from simple wear tests alone (e.g. lapping with diamond grits). Scanning electron microscopy has been extensively used to investigate the changing appearance of worn surfaces as plasticity and fracture processes compete as materials removal and redistribution mechanisms. Examples of the use of secondary electron imaging at different surface tilts, back-scattered electron imaging and stereo imaging are shown. Further, transmission electron microscopy of samples specially prepared to contain the worn surface layer can reveal the presence of phase changes accompanying wear. Furthermore, observations have been made of instances whereby brittle fracture has unexpectedly occurred as a result of repeated plastic deformation of surfaces at low contact severities. Some conclusions are drawn regarding the influence of specimen microstructure, abrasive grit size and environment of the wear of glass-bonded (debased) alumina and titania materials.     

Scanning electron microscopy and transmission electron microscopy study of hot-deformed γ-TiAl-based alloy microstructure

The aim of this work was to assess the changes in the microstructure of hot‐deformed specimens made of alloys containing 46–50 at.% Al, 2 at.% Cr and 2 at.% Nb (and alloying additions such as carbon and boron) with the aid of scanning electron microscopy and transmission electron microscopy techniques. After homogenization and heat treatment performed in order to make diverse lamellae thickness, the specimens were compressed at 1000 °C. Transmission electron microscopy examinations of specimens after the compression test revealed the presence of heavily deformed areas with a high density of dislocation. Deformation twins were also observed. Dynamically recrystallized grains were revealed. For alloys no. 2 and no. 3, the recovery and recrystallization processes were more extensive than for alloy no. 1.     

Low-voltage scanning electron microscopy of low-density materials

Delicate microstructures in low-density polymer foams and silica aerogel are susceptible to coating damage, artifact structures induced by coating, and electron-beam damage when they are examined by conventional scanning electron microscopy (SEM) techniques. These problems can be reduced significantly and even eliminated when these materials are examined directly with no coating using low-voltage scanning electron microscopy (LVSEM). Much of the fine structure in these materials also can be resolved at low voltage in a SEM equipped with a field-emission gun (FESEM).     

Imaging tissue engineering scaffolds using multiphoton microscopy

In this study, we combined two-photon autofluorescence and second harmonic generation imaging to investigate the three-dimensional microstructure and nonlinear optical properties of tissue engineering scaffolds. We focused on five different types of scaffold materials commonly used in tissue engineering, including: open-cell polylactic acid, polyglycolic acid, collagen composite scaffold, collagraft bone graft matrix strip, and nylon. By the use of multiphoton microscopy and a motorized stage, we obtained high resolution, spectrally resolved structural information of the scaffolds over large areas or in three-dimensions. Our results show that the nonlinear optical properties of the scaffolds will enable us to spectrally and morphologically distinguish the different types of scaffold materials investigated. We envision multiphoton microscopy to be a useful technique in tissue engineering applications in understanding the interplay between cultured cells and the scaffold materials.     

Time-resolved cryotransmission electron microscopy

We describe a new technique, time-resolved cryotransmission electron microscopy (TRC-TEM), that can be used to study changes in microstructure occurring during dynamic processes such as phase transitions and chemical reactions. The sample is prepared on an electron microscope grid maintained at a fixed temperature in a controlled atmosphere. The dynamic process is induced on the grid by a change in pH, salt, or reactant concentration by rapid mixing with appropriate solutions. Alternatively, induction is by rapid change of specimen temperature, or by controlled evaporation of a volatile component. We call such procedures on-the-grid processing. The dynamic process is permitted to run for a defined time and then the thin-film specimen is thermally fixed by plunging into liquid ethane at its freezing point, producing a cryotransmission electron microscopy specimen. By repeating this procedure with varying delays between induction and sample fixation, we can observe transient microstructures. We demonstrate the use of TRC-TEM to study the intermediate structures that form during the transitions between Lα, I_II, and H_II liquid crystalline phases in phospholipid systems. We also identify several other possible applications of the technique.     

Scanning probe microscopy for industrial applications: Selected examples

Some examples are selected to demonstrate the variety of possible scanning probe microscopy application in industry. Magnetic and magneto-optical storage media can be investigated by magnetic force microscopy, whereas a conventional scanning force microscope is used to examine surface features of many different materials, such as technical glasses, photosensitive materials, new superconductors, and biomolecules. Some other examples include the modification as well as the observation of liquid crystal devices, and the impact that scanning probe microscopy has on other techniques such as high precision stepping motors and high quality electron beam sources.     

Scanning and transmission electron microscopy microstructure characterization of mechanically alloyed Nb–Ti–Al alloys

Results are presented of an investigation of the microstructure development during mechanical alloying and following consolidation of an Nb15Ti15Al alloy. The alloy was synthesized from elemental as well as pre‐alloyed powders. The microstructure of this material was examined by transmission electron microscopy, scanning electron microscopy and X‐ray diffraction. The use of pre‐alloyed TiAl powder for synthesis of the Nb15Ti15Al alloy meant that a much shorter time was required to complete the mechanical alloying process compared with the synthesis of elemental powders. The investigation indicates that three phases were present in the consolidated materials: the Nb solid solution, the Nb₃Al intermetallic phase and the dispersoid.     

Electron microscopy and diffraction of radiation-sensitive nanostructured materials

Soft matter research of natural organic and synthetic nanomaterials is an area in nanoscience and technology that has been growing particularly quickly in recent years. The materials under investigation are sensitive to high‐energy electrons. Any structure characterization using electron microscopy thus requires special care. First, we illustrated this on naturally grown nanotubes observed by normal and cryogenic scanning electron microscopy. Second, we studied the ordering and orientation of the mesophase in template‐grown nanotubes and nanorods containing discotic liquid crystals without and with doping, as desired. For these studies, we mainly used transmission electron diffraction and microscopy at low‐dose conditions, high‐efficiency image acquisition, and cryoprotection of the structures at liquid helium temperature. Additional analytical information was obtained by electron energy filtering observations.     

Problem oriented transmission electron microscopy

The relative advantages and disadvantages of the variety of transmission electron microscopical techniques which can be applied to materials science problems are argued by the examination of problems from a range of different fields. The further developments which will be needed before the full potential of some of the more modern approaches can be achieved are also discussed, as are the increasing uses of ‘edge-on’ specimen preparation methods.     

激光共焦扫描显微镜及其应用

介绍了共焦激光显微镜的基本光路、成像原理、关键技术及应用。     

Comparative light microscopy,scanning electron microscopy and transmission electron microscopy of selected organic walled microfossils

Two simple techniques are described and illustrated. The first is for the study of one specimen by both light microscopy (LM) and scanning electron microscopy (SEM). The second is for the study of one selected specimen by LM, SEM and in ultrathin section by transmission electron microscopy (TEM). Although these techniques were developed for the comparative study of Precambrian organic walled microfossils (OWMs), they could be used for a wide range of other specimens.