• Transactions of Materials Processing
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• v.33 no.2
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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.

• Journal of Mechanical Science and Technology
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• v.20 no.3
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• pp.310-318
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• 2006

In this study, we investigate the feasibility of in-situ crack propagation by using a double cleavage drilled compression (DCDC) specimen showing a slow crack velocity down to 0.03 mm/s under 0.01 mm/s of displacement control. Finite element analysis predicted that the DCDC specimens would show at least 4.3 fold delayed crack initiation time than conventional tensile fracture specimens under a constant loading speed. Using DCDC specimens, we were able to observe the in-situ crack propagation process in a particle reinforced transparent polymer composite. Our results confirmed that the DCDC specimen would be a good candidate for the in-situ observation of the behavior of particle reinforced composites with slow crack velocity, such as the self-healing process of micro-particle reinforced composites.

• Applied Microscopy
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• v.50
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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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• v.38 no.4
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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.

• Corrosion Science and Technology
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• v.22 no.4
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• pp.265-272
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• 2023

The aim of this study was to develop a new in-situ observation method and instrument in micro-scale to investigate the mechanism of stress corrosion cracking (SCC) initiation of Ni-base alloys in a high temperature water environment of pressurized water reactors (PWRs). A laser confocal microscope (LCM), an autoclave with diamond window view port, and a slow strain-rate tester with primary water circulation loop system were components of the instrument. Diamond window, one of the core components of the instrument, was selected based on its optical, chemical, and mechanical properties. LCM was used to observe the specimen in micro-scale, considering the experimental condition of a high-temperature primary water environment. Using in-situ method and instrument, it is possible to observe oxidation and deformation of specimen surface in micro-scale through the diamond window in a high-temperature primary water in real-time. The in-situ method and instrument developed in this work can be utilized to investigate effects of various factors on SCC initiation in a high-temperature water environment.

• Proceedings of the Korean Geotechical Society Conference
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• 2002.03a
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• pp.619-626
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• 2002

In this study, a correlation among pressure, time and quantity of injection was organized from the laboratory tests, which were executed many times representing in-situ soil conditions carefully and then it would be applied to the in-situ soil injection simulator which will be developed for optimal injection into the ground. The sort of sample soils were both sand(A specimen) and silty sand(B specimen). Injection tests were gone into operation by compaction state, injection velocity and the depth individually. In the ground improved with permeation Infection, the relation among injection pressure of the same depth, the injected quantities and time were systematic by the depth. By defining the limit range of injection pressure and quantity about the variety of a linear equation obtained from lining each of their trend, the application of laboratory injection monitoring program and the data to evaluate its realization were produced. In the ground improved with root type injection, the relation between injection pressure and the injected quantities was irregular because fracture state occurred quickly.

• Proceedings of the KIEE Conference
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• 2008.09a
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• pp.233-234
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• 2008

We observed internal space charge behavior for two types of epoxy composites under dc electric fields to investigate the influence of water at high temperature. In the case of glass/epoxy specimen, homocharge is observed at water-treated specimen, and spatial oscillations become clearer in the water-treated specimens. Electric field in the vicinity of the electrodes shows the injection of homocharge. In aramid/epoxy specimens, heterocharge is observed at water-treated specimens, i.e. negative charge accumulates near the anode, while positive charge accumulates near the cathode. Electric field is enhanced just before each electrode. In order to further examine the mechanism of space charge formation, we have developed a new system that allows in situ space charge observation during ion migration tests at high temperature and high humidity. Using this in situ system.

• Proceedings of the KIEE Conference
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• 2008.07a
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• pp.2307-2308
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• 2008

We observed internal space charge behavior for two types of epoxy composites under dc electric fields to investigate the influence of water at high temperature. In the case of glass/epoxy specimen, homocharge is observed at water-treated specimen, and spatial oscillations become clearer in the water-treated specimens. Electric field in the vicinity of the electrodes shows the injection of homocharge. In aramid/epoxy specimens, heterocharge is observed at water-treated specimens, i.e. negative charge accumulates near the anode, while positive charge accumulates near the cathode. Electric field is enhanced just before each electrode. In order to further examine the mechanism of space charge formation, we have developed a new system that allows in situ space charge observation during ion migration tests at high temperature and high humidity. Using this in situ system.

• Proceedings of the Korean Institute of Building Construction Conference
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• 2020.11a
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• pp.192-193
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• 2020

In reinforced concrete adhesion studies, the demolition of the specimen is inevitably involved, and the studies conducted are limited to the macro load-displacement analysis. In order to establish an elaborate model for concrete bonding reinforced rebars, it is necessary to observe the rebar bonding behavior in the in-situ state. In this study, specially manufactured reinforcing bars, micro-UTM and 𝝁-computer tomography (𝝁CT) are used to observe reinforcing bars in the in-situ state. As a result of the monotonic pullout test of the processed reinforcing bar, maximum bond stress were shown to be 16.7MPa, which is slightly higher than the existing 10 to 12 MPa, and then the empty space inside the specimen in which the pullout test was conducted using 𝝁CT was confirmed. Through additional research, the fracture phenomenon of concrete excluding voids will be studied.

• Applied Microscopy
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• v.47 no.3
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• pp.208-213
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• 2017

The microstructural changes in Co nanoparticles and an Au-10at.%Pd thin film have been investigated using an in situ heating holder with a micro-electro-mechanical system (MEMS). In Co nanoparticles, two phases (face-centered cubic and hexagonal close-packed crystal structures) were found to coexist at room temperature and microstructures at temperatures, higher than $1,000^{\circ}C$, were observed with a quick response time and significant stability. The actual temperature of each specimen was directly estimated from the changes in the lattice spacing (Bragg-peak separation). For the Au-10at.%Pd thin film, at a set temperature of $680^{\circ}C$, the actual temperature of the sample was estimated to be $1,020^{\circ}C{\pm}123^{\circ}C$. Note that the specimen temperature should be carefully evaluated because of the undesired effects, i.e., the temperature non-uniformity due to the sample design of the MEMS chip, and distortion due to thermal expansion.