Search

Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) enable the visualization of three-dimensional (3D) microstructures ranging from atomic to micrometer scales using 3D reconstruction techniques based on computed tomography algorithms. This 3D microscopy method is called electron tomography (ET) and has been utilized in the fields of materials science and engineering for more than two decades. Although atomic resolution is one of the current topics in ET research, the development and deployment of intermediate-resolution (non-atomic-resolution) ET imaging methods have garnered considerable attention from researchers. This research trend is probably not irrelevant due to the fact that the spatial resolution and functionality of 3D imaging methods of scanning electron microscopy (SEM) and X-ray microscopy have come to overlap with those of ET. In other words, there may be multiple ways to carry out 3D visualization using different microscopy methods for nanometer-scale objects in materials. From the above standpoint, this review paper aims to (i) describe the current status and issues of intermediate-resolution ET with regard to enhancing the effectiveness of TEM/STEM imaging and (ii) discuss promising applications of state-of-the-art intermediate-resolution ET for materials research with a particular focus on diffraction contrast ET for crystalline microstructures (superlattice domains and dislocations) including a demonstration of in situ dislocation tomography. [ABSTRACT FROM AUTHOR]

Highlights • A magnetizing specimen holder that can apply a 0.5-T in-plane field has been developed. • The holder consists of three miniaturized electromagnets with 180-µm gap lengths. • Magnetization reversal of a Nd-Fe-B magnet from saturated state was observed in-situ. Abstract A side-entry specimen holder capable of applying a 0.5-tesla in-plane magnetic-induction field for in-situ transmission electron microscopy was developed. Three miniaturized electromagnets with 300 × 300-µm pole area and 180-µm pole gap are stacked along the electron-beam path in the holder. The middle magnet is used for magnetizing the specimen, which is inserted into the pole gap by using a 40-µm-width cantilever for atomic-force microscopy. The upper and lower magnets are used to keep the electron beam parallel to the optical axis. Magnetic-field magnitude was determined on the basis of experimentally measured electron-deflection angles and induction-field profiles along the electron-beam path calculated by finite element electromagnetic simulation. Magnetization reversal in 300-nm-thick Nd-Fe-B magnets from the saturated state was in-situ observed by using the holder and a 1-MeV cold-field-emission transmission electron microscope. The observation revealed that domain-wall pinning occurred in different manners at the c-plane and non-c-plane grain boundaries. The holder was thereby shown to be useful for analysis of magnetization-reversal behaviors of hard magnetic materials. [ABSTRACT FROM AUTHOR]

The charging effect due to electron irradiation in an electron microscope has been studied so far with incident electrons. Here we report on a new specimen holder to control the charging effect by using electrons emitted from an irradiation port in the holder while maintaining a constant intensity of the incident electron beam. Details of the charging effect, such as electric field variation, are expected to be investigated by electron holography. The new specimen holder was developed by modifying a double-probe piezodriving specimen holder to introduce an electron irradiation port in one of its two arms. As a result, the new modified specimen holder consists of a piezodriving probe and an electron irradiation port, both of which can be controlled in three dimensions, using piezoelectric elements and micrometers. We demonstrate that variations in the charging effect for epoxy resin and surface contamination can be observed by electron holography. [ABSTRACT FROM PUBLISHER]

Abstract: Electron tomography requires a wide angular range of specimen-tilt for a reliable three-dimensional (3D) reconstruction. Although specimen holders are commercially available for tomography, they have several limitations, including tilting capability in only one or two axes at most, e.g. tilt–rotate. For amorphous specimens, the image contrast depends on mass and thickness only and the single-tilt holder is adequate for most tomographic image acquisitions. On the other hand, for crystalline materials where image contrast is strongly dependent on diffraction conditions, current commercially available tomography holders are inadequate, because they lack tilt capability in all three orthogonal axes needed to maintain a constant diffraction condition over the whole tilt range. We have developed a high-angle triple-axis (HATA) tomography specimen holder capable of high-angle tilting for the primary horizontal axis with tilting capability in the other (orthogonal) horizontal and vertical axes. This allows the user to trim the specimen tilt to obtain the desired diffraction condition over the whole tilt range of the tomography series. To demonstrate its capabilities, we have used this triple-axis tomography holder with a dual-axis tilt series (the specimen was rotated by 90° ex-situ between series) to obtain tomographic reconstructions of dislocation arrangements in plastically deformed austenitic steel foils. [Copyright &y& Elsevier]

As the development of quantised storage media progresses, detailed knowledge is required about the magnetisation reversal behaviour of sub-micron sized magnetic structures in external magnetic fields. Using the Lorentz mode of transmission electron microscopy (LTEM) the magnetic microstructure of thin film samples can be imaged with high spatial resolution. A novel approach for in situ magnetising experiments is described which combines the development of a custom-made sample holder which generates two orthogonal in-plane components of magnetic field in the specimen plane with the benefit of computer-controlled variation of the field. We present a specimen stage suitable for a Philips CM30 Twin/LTEM, which allows the generation of well-defined magnetic in-plane fields in the TEM. [Copyright &y& Elsevier]

• Development of a cartridge based turning holder. • Increase the reliability of magnetic induction mapping in TEM. • Cartridge system for wide range of samples. • Measurements of materials with low and high magnetic coercivity. • Precise holder tilt measurement using an inclinometer. Magnetic induction mapping in the transmission electron microscope using phase contrast techniques such as off-axis electron holography and differential phase contrast imaging often requires the separation of the magnetic contribution to the recorded signal from the electrostatic contribution. When using off-axis electron holography, one of the experimental approaches that can be used to achieve this separation is to evaluate half of the difference between phase shift images that have been recorded before and after turning the sample over. Here, we introduce a cartridge-based sample mounting system, which is based on an existing on-axis tomography specimen holder and can be used to turn a sample over inside the electron microscope, thereby avoiding the need to remove the holder from the microscope to turn the sample over manually. We present three cartridge designs, which are compatible with all pole piece designs and can be used to support conventional 3-mm-diameter sample grids, Si 3 N 4 -based membrane chips and needle-shaped specimens. We make use of a wireless inclinometer that has a precision of 0.1° to monitor the sample holder tilt angle independently of the microscope goniometer readout. We also highlight the need to remove geometrical image distortions when aligning pairs of phase shift images that have been recorded before and after turning the sample over. The capabilities of the cartridge-based specimen holder and the turning approach are demonstrated by using off-axis electron holography to record magnetic induction maps of lithographically-patterned soft magnetic Co elements, a focused ion beam milled hard magnetic Nd-Fe-B lamella and an array of four Fe 3 O 4 nanocrystals. [ABSTRACT FROM AUTHOR]