• Applied Microscopy
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• 제50권
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• pp.21.1-21.3
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• 2020

Sample preparation is significantly important to the high-resolution transmission electron microscopy (HRTEM) characterization of nanomaterials. However, many general organic solvents can dissolve the necessary organic polymer support layer in TEM grid, which causes it difficult to obtain high-quality samples of oil-soluble nanomaterials. In this study, a new sample preparation method for oil-soluble nanomaterials has been developed by using the sublimable material as a transition layer. Experiments also show that there is no damage to TEM grids and high-quality HRTEM images can be obtained via this method. This approach paves the way to applicable HRTEM sample preparation of oil-soluble nanomaterials.

• Applied Microscopy
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• 제51권
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• pp.19.1-19.7
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• 2021

The main purpose of this paper is the preparation of transmission electron microscopy (TEM) samples from the microsized powders of lithium-ion secondary batteries. To avoid artefacts during TEM sample preparation, the use of ion slicer milling for thinning and maintaining the intrinsic structure is described. Argon-ion milling techniques have been widely examined to make optimal specimens, thereby making TEM analysis more reliable. In the past few years, the correction of spherical aberration (Cs) in scanning transmission electron microscopy (STEM) has been developing rapidly, which results in direct observation at an atomic level resolution not only at a high acceleration voltage but also at a deaccelerated voltage. In particular, low-kV application has markedly increased, which requires a sufficiently transparent specimen without structural distortion during the sample preparation process. In this study, sample preparation for high-resolution STEM observation is accomplished, and investigations on the crystal integrity are carried out by Cs-corrected STEM.

• Applied Microscopy
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• 제46권2호
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• pp.110-115
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• 2016

Transmission electron microscopy (TEM) is a powerful tool for analyzing a broad range of materials and provides localized information about the microstructure. However, the analysis results are strongly influenced by the quality of the thin foil specimen. Sample preparation for TEM analysis requires considerable skill, especially when the area of interest is small or the material of interest is difficult to thin because of its high hardness and its mechanical instability when thinned. This article selectively reviews recent advances in TEM sample preparation techniques using a tripod polisher. In particular, it introduces two typical types (fl at type and wedge type) of TEM sample preparation and the benefits and drawbacks of each method; finally, a method of making better samples for TEM analysis is suggested.

• 한국재료학회지
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• 제13권9호
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• pp.598-605
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• 2003

The optimized conditions for the cross-sectional TEM sample preparation using tripod polisher and ion-beam miller was confirmed by AFM and TEM. For the TEM observation of interfaces including InGaN layers like InGaN/GaN MQW structures, the sample preparation by the only tripod polishing was useful due to the reduction of artifacts. On the other hand, in case of the thick nitride films like ELO, PE, and superlattice, both tripod polishing and controlled ion-beam milling were required to improve the reproducibility. As a result, the ion-beam milling with the $60^{\circ}$modulation showed the minimum height difference between film and sapphire interface and the ion-beam milling of the $80^{\circ}$modulation showed the broad observable width.

• Applied Microscopy
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• 제45권4호
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• pp.199-202
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• 2015

A simple and novel transmission electron microscopy (TEM) sample preparation method for phase change nanowire is investigated. A $Ge_2Sb_2Te_5$ (GST) nanowire TEM sample was meticulously prepared using nanomanipulator and gas injection system in a field emission scanning electron microscopy for efficient and accurate TEM analysis. The process can minimize the damage during the TEM sample preparation of the nanowires, thus enabling the crystallographic analysis of as-grown GST nanowires without unexpected phase transition caused by e-beam heating.

• Applied Microscopy
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• 제42권1호
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• pp.49-52
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• 2012

For TEM study of biological samples or polymers that are contained in organic structure, it is often required that the sample is prepared by using ultramicrotome and stained with proper agents to increase the contrast of organic structure. In this study, we investigated an efficient TEM sample preparation method for ductile heterogeneity material by using ultramicrotomy. Cryo-ultramicrotomy is a suitable method that is capable of rendering sample hardness for various ductile materials. However, it has several factors to consider, such as experimental cost, working time and finding the optimal staining conditions. To satisfy these considerations, we prepared TEM sample by using ultramicrotome without cryofunction, and secured the sample hardness by applying the staining process prior to ultrathin sectioning. The cross-linked polyethylene structure in the sample was stained with the 2% $RuO_4$ solution in a sealed test tube for 24 hours at $4^{\circ}C$. After the sample staining, ultrathin sections of sample were prepared using ultramicrotome. As a result, it was revealed that the difficulties associated with staining of ultrathin sections prepared by low-temperature conditions were improved. In addition, appropriate staining depth of sample could be selected for sectioning process. The quality of TEM sample obtained by using this method was better than that of cryo-ultramicroscopy. Finally, it is expected that our method could be effectively applied in TEM sample preparation for a variety of nano-bio convergence materials.

• Applied Microscopy
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• 제46권3호
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• pp.167-169
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• 2016

Solder/electroless nickel immersion gold (ENIG) joint sample which is comprised of dissimilar materials with different mechanical properties has limited the level of success in preparing thin samples for transmission electron microscopy (TEM). This short technical note reports the operation parameters for ultramicrotomy of solder joint sample and TEM analysis results. The solder joint sample was successfully sliced to 50~70 nm thick lamellae at slicing speed of 0.8~1.2 mm/s using a boat-type $45^{\circ}$ diamond knife. Ultramicrotomy can be applied as a routine sample preparation technique for TEM analysis of solder joints.

• 한국전자현미경학회:학술대회논문집
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• 한국현미경학회 2001년도 제32차 추계학술대회
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• pp.18-22
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• 2001

A technique to characterize specific site of materials using a combination of a dedicated focused ion beam system(FIB), and Intermediate-voltage scanning transmission electron microscope(STEM) or transmission electron microscope(TEM) equipped with a scanning electron microscope(SEM) unit has been developed. The FIB system is used for preparation of electron transparent thin samples, while STEM or TEM is used for localization of a specific site to be milled in the FIB system. An FIB-STEM(TEM) compatible sample holder has been developed to facilitate thin sample preparation with high positional accuracy Positional accuracy of $0.1{\mu}m$ or better can be achieved by the technique. In addition, an FIB micro-sampling technique has been developed to extract a small sample directly from a bulk sample in a FIB system These newly developed techniques were applied for the analysis of specific failure in Si devices and also for characterization of a specific precipitate In a metal sample.

• 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.

• 한국재료학회:학술대회논문집
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• 한국재료학회 1993년도 추계 학술발표 강연 및 논문 개요집
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• pp.59-59
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• 1993