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• A magnetising holder applied in Lorentz microscope is successfully developed. • The holder can apply a 1.5 T pure in-plane magnetic field. • The field strength is determined by calculation and experimental measurement. • The magnetisation process of hot-pressed Nd-Fe-B magnet is observed. A strong in-plane magnetic field is required for Lorentz transmission electron microscopy (LTEM) to observe the evolution of the magnetic domain structure of materials with high coercivity, particularly for research on rare-earth permanent magnets. However, the maximum field of the present in-situ magnetising holder applied in 200-kV or 300-kV TEM does not exceed 0.1 T. In this study, the reason for the low field was analysed, and the field strength was significantly elevated by reducing the field application area of the field generator. From finite element method calculations and experimental measurements, a 1.5 T in-plane field was achieved by our new holder in a 200-kV TEM, and images with good quality could still be obtained. Using the newly developed holder, the magnetisation process of hot-pressed NdFeB magnets was observed. The in-situ magnetising holder can be used in research on a wide variety of magnetic materials. [ABSTRACT FROM AUTHOR]

SUMMARY: ISO 5660‐1 specifies the cone calorimeter method for characterizing the ignition and surface burning behavior of materials. The specimen is irradiated through a square opening in the frame of the specimen holder. The frame is intended to protect the edges of the specimen from irradiation but covers the edges with only a few mm. In tests with products such as composite laminates and sandwich wall panels, the production of pyrolysis gases from the edges and, in many cases, burning have been observed. Early contribution from the edges in the test is not representative for surface burning. A modified specimen holder was developed with a larger specimen size to allow better protection of the edges. The opening for exposure to irradiance of the retainer frame is circular and of the same area as that of the original frame. The distance between the exposed surface and the specimen edges is larger in order to prevent early exposure of edges. Tests using the standard specimen holder resulted in pyrolysis and burning from edges that took place outside of the specimen holder. Comparative tests using the modified specimen holder showed that it prevented the exposure and pyrolysis from edges for an extended time. However, the influence on ignition time and peak heat release due to the increased size of the modified specimen holder has not been characterized fully, and test results should not be used for direct comparison with those of the standard holder. [ABSTRACT FROM AUTHOR]

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]

The physicochemical properties of heterogeneous catalysts in static or inert environments often deviate greatly from the properties under in‐situ or working conditions. To gain an insightful understanding of realistic catalyst properties and the corresponding catalytic mechanisms, it is essential to identify and rationalize changes in catalysts under reaction conditions. In recent years, in‐situ transmission electron microscope (in‐situ TEM) techniques have been increasingly developed, offering a unique approach to visualize the evolution of heterogeneous catalysis with ultra‐high spatial resolution, good energy resolution and reasonable temporal resolution under controllable or even realistic catalytic conditions. In this review, we have summarized recent advances in the in‐situ TEM analysis of heterogeneous catalysis, which suggests the great potential of this technique in this important field. Furthermore, technical challenges and possible solutions are discussed. [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]

A new generation of bioreactors with integrated six degrees of freedom (6 DOF) aims to mimic more accurately the natural intervertebral disc (IVD) load. We developed and validated in a biological and mechanical study a specimen holder and corresponding ex vivo IVD organ model according to the bioreactor requirements for multiaxial loading and a long-term IVD culture. IVD height changes and cell viability were compared between the 6 DOF model and the standard 1 DOF model throughout the 3 weeks of cyclic compressive loading in the uniaxial bioreactor. Furthermore, the 6 DOF model and holder were loaded for 9 days in the multiaxial bioreactor under development using the same conditions, and the IVDs were evaluated for cell viability. The interface of the IVD model and specimen holder, enhanced with fixation screws onto the bone, was tested in compression, torsion, lateral bending, and tension. Additionally, critical motions such as tension and bending were assessed for a combination of side screws and top screws or side screws and adhesive. The 6 DOF model loaded in the uniaxial bioreactor maintained similar cell viability in the IVD regions as the 1 DOF model. The viability was high after 2 weeks throughout the whole IVD and reduced by more than 30% in the inner annulus fibrous after 3 weeks. Similarly, the IVDs remained highly viabile when cultured in the multiaxial bioreactor. In both models, IVD height changes after loading were in the range of typical physiological conditions. When differently directed motions were applied, the holder-IVD interface remained stable under hyper-physiological loading levels using a side screw approach in compression and torsion and the combination of side and top screws in tension and bending. We thus conclude that the developed holding system is mechanically reliable and biologically compatible for application in a new generation of multiaxial bioreactors.

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]

Abstract: A novel specimen holder that enables in situ observation of crack-tip deformation and/or fracture under a controlled environment is developed for a high-voltage electron microscope (HVEM). A window-type environmental cell (EC) that incorporates a uniaxial straining apparatus is built into a side-entry-type single-tilt specimen holder. The gas control in EC, straining apparatus design, limited field of view for crack-tip observation, and specimen preparation for the specimen holder are presented in detail. Experimental results successfully demonstrate that the developed specimen holder is quite useful for the dynamic observation of crack-tip deformation and/or fracture subjected to a hostile environment, such as hydrogen gas. [ABSTRACT FROM AUTHOR]

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]

A simple, new TEM specimen holder to detect cathodoluminescence (CL) in a transmission electron microscope has been developed. This holder accommodates a flat light‐collecting reflector below the specimen and CL signals are guided to an optical spectrometer outside of the microscope through a quartz optical fibre. The compact system requires no modification of the microscope itself and allows large‐angle specimen tilting and easy combination with other associate analytical tools. Test data are presented to aid the future application of the holder. [ABSTRACT FROM PUBLISHER]