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Microstructural changes during the martensitic transformation from face-centred cubic (FCC) to body-centred cubic (BCC) in an Fe-31Ni alloy were observed by scanning electron microscopy (SEM) with a newly developed Peltier stage available at temperatures to  −75°C. Electron channelling contrast imaging (ECCI) was utilized for the in situ observation during cooling. Electron backscatter diffraction analysis at ambient temperature (20°C) after the transformation was performed for the crystallographic characterization. A uniform dislocation slip in the FCC matrix associated with the transformation was detected at −57°C. Gradual growth of a BCC martensite was recognized upon cooling from −57°C to −63°C. [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]

An in situ straining holder capable of tensile deformation and high-angle tilt for electron tomography was developed for polymeric materials. The holder has a dedicated sample cartridge, on which a variety of polymeric materials, such as microtomed thin sections of bulk specimens and solvent-cast thin films, can be mounted. Fine, stable control of the deformation process with nanoscale magnification was achieved. The holder allows large tensile deformation (≃ 800 μm) with a large field of view (800 × 200 μm before the deformation), and a high tilt angle (±75°) during in situ observations. With the large tensile deformation, the strain on the specimen can be as large as 26, at least one order of magnitude larger than the holder's predecessor. We expect that meso- and microscopic insights into the dynamic mechanical deformation and fracture processes of polymeric materials can be obtained by combining the holder with a transmission electron microscope equipped with an energy filter. The filter allows zero-loss imaging to improve the resolution and image contrast for thick specimens. We used this technique to study the deformation process in a silica nanoparticle-filled isoprene rubber. [ABSTRACT FROM AUTHOR]

In conventional transmission electron microscopy, specimens to be observed are placed in between the objective lens pole piece and therefore exposed to a strong magnetic field about 2 T. For a ferromagnetic specimen, magnetization of the specimen causes isotropic and anisotropic defocusing, deflection of the electron beam as well as deformation of the specimen, which all become more severe when the specimen tilted. Therefore electron tomography on a ferromagnetic crystalline specimen is highly challenging because tilt-series data sets must be acquired without changing the excitation condition of a specific diffraction spot. In this study, a scanning transmission electron microscopy (STEM) tomography method without magnetizing a ferromagnetic specimen has been developed for three-dimensional (3D) visualization of dislocations in α-Fe, which is a typical ferromagnetic material. Magnetic-field-free environment down to 0.38 ± 0.07 mT at the specimen position is realized by demagnetizing the objective lens pole piece of a commercial STEM instrument. By using a spherical aberration corrector with the magnetic-field-free environment, an “aberration corrected Low-Mag STEM mode” with no objective lens field reaches a convergence semi angle ∼1 mrad and a spatial resolution ∼5 nm, and shows an adequate performance of imaging dislocations under a two-beam excitation condition for a low-index diffracted beam. The illumination condition for the aberration corrected Low-Mag STEM mode gives no overlap between the direct beam disk (spot) and neighboring diffraction disks. An electron channeling contrast imaging technique, in which an annular detector was located at a doughnut area between the direct beam and the neighboring diffracted beams, was effectively employed with the aberration corrected Low-Mag STEM mode to keep image intensity high enough even at large specimen-tilt angles. The resultant tomographic observation visualized 3D dislocation arrangements and active slip planes in a deformed α-Fe specimen. [ABSTRACT FROM AUTHOR]

The nanoscale characterization of thermally activated solid reactions plays a pivotal role in products manufactured by nanotechnology. Recently, in situ observation in transmission electron microscopy combined with electron tomography, namely four-dimensional observation for heat treatment of nanomaterials, has attracted great interest. However, because most nanomaterials are highly reactive, i.e. , oxidation during transfer and electron beam irradiation would likely cause fatal artefacts; it is challenging to perform the artifact-free four-dimensional observation. Herein, we demonstrate our development of a novel in situ three-dimensional electron microscopy technique for thermally activated solid-state reaction processes in nanoparticles (NPs). The sintering behaviour of Cu NPs was successfully visualized and analyzed in four-dimensional space-time. An advanced image processing protocol and a newly designed state-of-the-art MEMS-based heating holder enable the implementation of considerably low electron dose imaging and prevent air exposure, which is of central importance in this type of observation. The total amount of electron dose for a single set of tilt-series images was reduced to 250 e - nm -2 , which is the lowest level for inorganic materials electron tomography experiments. This study evaluated the sintering behaviour of Cu NPs in terms of variations in neck growth and particle distance. A negative correlation between the two parameters is shown, except for the particle pair bound by neighbouring NPs. The nanoscale characteristic sintering behavior of neck growth was also captured in this study.

Microstructural changes during the martensitic transformation from face-centred cubic (FCC) to body-centred cubic (BCC) in an Fe-31Ni alloy were observed by scanning electron microscopy (SEM) with a newly developed Peltier stage available at temperatures to  -75°C. Electron channelling contrast imaging (ECCI) was utilized for the in situ observation during cooling. Electron backscatter diffraction analysis at ambient temperature (20°C) after the transformation was performed for the crystallographic characterization. A uniform dislocation slip in the FCC matrix associated with the transformation was detected at -57°C. Gradual growth of a BCC martensite was recognized upon cooling from -57°C to -63°C., (© The Author(s) 2020. Published by Oxford University Press on behalf of The Japanese Society of Microscopy.)