• Applied Microscopy
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• 제36권spc1호
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• pp.9-17
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• 2006

An interface and a grain boundary in the solid state can be quite unstable and vibrate violently under special circumstances. Two examples of such a vibration, as observed by in-situ transmission electron microscopy, were presented.

• 소성∙가공
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• 제33권2호
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• pp.118-122
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• 2024

Micro-electromechanical systems (MEMS) based in-situ heating holders have been developed to enable high resolution imaging of heat treatment analysis. However, unlike the standard 3 mm metal disk specimens used in the furnace-based heating holder and general transmission electron microscopy holder, the MEMS-based in-situ heating holder requires thin specimens that can be penetrated by electrons to be transferred onto the MEMS chip. Previously, focused ion beam milling was used to transfer metal specimens, but it has the disadvantage of being expensive and the risk of specimen damage due to gallium ions. Therefore, in this study, we devised a method of transferring metallic materials by ultrasonic treatment using a transmission electron microscopy specimen made by electro jet polishing. A 3mm electropolished metal disk was placed in an appropriate solution, ultrasonicated, and then drop casted. The transfer of the specimen was successful, but it was confirmed that dislocations were formed inside the specimen due to ultrasonic treatment. This study provides a novel method for transferring metallic materials onto MEMS chips, which is cost-effective and less gallium ion damaging to the specimen. The results of this study can be used to improve the efficiency of heat treatment analysis using MEMS-based in-situ heating holders.

• Applied Microscopy
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• 제51권
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• pp.8.1-8.7
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• 2021

Growing demands for comprehending complicated nano-scale phenomena in atomic resolution has attracted in-situ transmission electron microscopy (TEM) techniques for understanding their dynamics. However, simple to safe TEM sample preparation for in-situ observation has been limited. Here, we suggested the optical microscopy based micro-manipulating system for transferring TEM samples. By adopting our manipulator system, several types of samples from nano-wires to plate-like thin samples were transferred on micro-electro mechanical systems (MEMS) chip in a single step. Furthermore, the control of electrostatic force between the sample and the probe tip is found to be a key role in transferring process.

• Applied Microscopy
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• 제38권4호
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• pp.383-386
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• 2008

In performing in situ heating transmission electron microscopy (TEM) for materials characterizations, arising concerns such as specimen drifts and unintentional Cu contamination are discussed. In particular, we analysed the thermal and mechanical characteristics of in situ heating holders to estimate thermal drift phenomena. From the experimental results, we suggest an empirical model to describe the thermal drift behavior so that we can design an effective plan for in situ heating experiment. Practical approaches to minimize several hindrances arisen from the experiment are proposed. We believe that our experimental recommendations will be useful for a microscopist fascinated with the powerful potential of in situ heating TEM.

• Applied Microscopy
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• 제45권2호
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• pp.95-100
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• 2015

The in-situ heating transmission electron microscopy experiment allows us to observe the time- and temperature-dependent dynamic processes in nanoscale materials by examining the same specimen. The temperature, which is a major experimental parameter, must be measured accurately during in-situ heating experiments. Therefore, calibrating the thermocouple readout of the heating holder prior to the experiment is essential. The calibration can be performed using reference materials whose phase-transformation (melting, oxidation, reduction, etc.) temperatures are well-established. In this study, the calibration experiment was performed with four reference materials, i.e., pure Sn, Al-95 wt%Zn eutectic alloy, NiO/carbon nanotube composite, and pure Al, and the calibration curve and formula were obtained. The thermocouple readout of the holder used in this study provided a reliable temperature value with a relative error of <4%.

• Applied Microscopy
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• 제45권1호
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• pp.16-22
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• 2015

The reaction kinetics of the growth of Ni germanide in the Ni/Zr-interlayer/Ge system was investigated using isothermal in situ annealing at three different temperatures in a transmission electron microscope. The growth rate of Ni germanide in the Ni/Zr-interlayer/Ge system was determined to be diffusion controlled and depended on the square root of the time, with the activation energy of $1.04P{\pm}0.04eV$. For the Ni/Zr-interlayer/Ge system, no intermediate or intermixing layer between the Zr-interlayer and Ge substrate was formed, and thus the Ni germanide was formed and grew uniformly due to Ni diffusion through the diffusion path created in the amorphous Zr-interlayer during the annealing process in the absence of any intermetallic compounds. The reaction kinetics in the Ni/Zr-interlayer/Ge system was affected only by the Zr-interlayer.

• Corrosion Science and Technology
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• 제14권6호
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• pp.301-312
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• 2015

Corrosion of zirconium fuel cladding is known to limit the lifetime and reloading cycles of fuel in nuclear reactors. Oxide layers formed on ZIRLO4^{TM}$ cladding samples, after immersion for 300-hour and 50-day in a simulated primary water chemistry condition ($360^{\circ}C$ and 20 MPa), were analyzed by using the scanning transmission electron microscopy (STEM), in-situ transmission electron microscopy (in-situ TEM) with the focused ion beam (FIB) technique, and X-ray diffraction (XRD). Both samples (immersion for 300 hours and 50 days) revealed the presence of the ZrO sub-oxide phase at the metal/oxide interface and columnar grains developed perpendicularly to the metal/oxide interface. Voids and micro-cracks were also detected near the water/oxide interface, while relatively large lateral cracks were found just above the less advanced metal/oxide interface. Equiaxed grains were mainly observed near the water/oxide interface.

• Applied Microscopy
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• 제50권
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• pp.22.1-22.6
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• 2020

In-situ transmission electron microscopy (TEM) holders that employ a chip-type specimen stage have been widely utilized in recent years. The specimen on the microelectromechanical system (MEMS)-based chip is commonly prepared by focused ion beam (FIB) milling and ex-situ lift-out (EXLO). However, the FIB-milled thin-foil specimens are inevitably contaminated with Ga⁺ ions. When these specimens are heated for real time observation, the Ga⁺ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue by Ar⁺ ion milling within FIB system was explored in this study. However, the Ga residue remained in the thin-foil specimen that was extracted by EXLO from the trench after the conduct of Ar⁺ ion milling. To address this drawback, the thin-foil specimen was attached to an FIB lift-out grid, subjected to Ar⁺ ion milling, and subsequently transferred to an MEMS-based chip by EXLO. The removal of the Ga residue was confirmed by energy dispersive spectroscopy.

• Applied Microscopy
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• 제36권spc1호
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• pp.63-69
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• 2006

By utilizing a field emission gun and a biprism installed on a transmission electron microscope (TEM), electron holography is extensively carried out to visualize the electric and magnetic fields of nanomaterials. In the electric field analysis, the distribution of electric potential in a sharp tip made of W coated with $ZrO_2$ is visualized by applying the voltage to the tip. Denser contour lines due to the electric potential are observed with an increase in the bias voltage. In the magnetic field analysis by producing the strong magnetic field with a sharp magnetic needle made of a permanent magnet, the in situ experiment is carried out to investigate the magnetization of hard magnetic materials. The results of these experiments clearly demonstrate that electron holography is a promising advanced transmission electron microscopy technique to characterize the electric and magnetic properties of nanomaterials.

• 한국정보디스플레이학회:학술대회논문집
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• 한국정보디스플레이학회 2005년도 International Meeting on Information Displayvol.II
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• pp.1081-1086
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• 2005

Dynamic behavior of carbon nanotubes (CNTs) in an electric field is directly observed by in-situ transmission electron microscopy (TEM). The CNT field emitters examined by in-situ TEM are multiwalled, double-walled and single walled CNTs. Threshold fields for electron emission and sustainable emission currents depending on the structure of CNTs are presented, and degradation mechanism of the CNT field emitters is discussed. In addition to the microscopy studies on individual CNTs, our recent development in surface treatment of CNT layers grown by chemical vapor deposition, which brings about high density of emission current and high uniformity, is also presented.