• 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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• 제48권4호
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• pp.132-133
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• 2018

One of the most important factors determining the properties of a material is its grain size. However, unclear grain boundaries in the image hinder an accurate measurement of grain size. We demonstrate that grain boundaries existing in the images obtained by scanning transmission electron microscopy (STEM) can be clearly distinguished by applying a Sobel filter to a tilting series of STEM images of a hydrogenation-disproportionation-desorption-recombination processed Nd2Fe14B magnet sample.

• Journal of Powder Materials
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• 제24권4호
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• pp.285-291
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• 2017

We propose a custom analysis technique for the dark field (DF) image based on transmission electron microscopy (TEM). The custom analysis technique is developed based on the $DigitalMicrograph^{(R)}$ (DM) script language embedded in the Gatan digital microscopy software, which is used as the operational software for most TEM instruments. The developed software automatically scans an electron beam across a TEM sample and records a series of electron diffraction patterns. The recorded electron diffraction patterns provide DF and ADF images based on digital image processing. An experimental electron diffraction pattern is recorded from a IrMn polycrystal consisting of fine nanograins in order to test the proposed software. We demonstrate that the developed image processing technique well resolves nanograins of ~ 5 nm in diameter.

• Applied Microscopy
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• 제52권
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• pp.2.1-2.6
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• 2022

With the lightening of the mobile devices, thinning of electrolytic copper foil, which is mainly used as an anode collection of lithium secondary batteries, is needed. As the copper foil becomes ultrathin, mechanical properties such as deterioration of elongation rate and tear phenomenon are occurring, which is closely related to microstructure. However, there is a problem that it is not easy to prepare and observe specimens in the analysis of the microstructure of ultrathin copper foil. In this study, electron backscatter diffraction (EBSD) specimens were fabricated using only mechanical polishing to analyze the microstructure of 8 ㎛ thick electrolytic copper foil in plane view. In addition, EBSD maps and transmission electron microscopy (TEM) images were compared and analyzed to find the optimal cleanup technique for properly correcting errors in EBSD maps.

• 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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• 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.

• Bulletin of the Korean Chemical Society
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• 제34권3호
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• pp.788-792
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• 2013

A shortcoming of using transmission electron microscopy (TEM) for structural analysis via electron diffraction is the relatively large error of the measurements as compared to X-ray diffraction. To reduce these errors, various internal standard methods from earlier studies have been widely used. We developed a new device to facilitate the application of internal standard methods in preparation of TEM grids used for nanopowder analysis. Through the application of a partial mask on the TEM grid, both the internal standards and the research materials can be loaded on the same grid. Through this process, we conducted a TEM analysis that compared synthetic hydroxyapatite (HAp) nanopowder to bone apatite from a bovine femur. We determined that the accuracy of the d-spacing measurements of the HAp and bone powders could be improved to better than 1% after statistical treatments of the experimental data. By applying a quarter mask, we loaded four different nanoparticles on a single TEM grid, with one section designated for the internal standard.

• Journal of the Institute of Electronics Engineers of Korea SD
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• 제41권1호
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• pp.15-20
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• 2004

The interfacial layer between the oxide film and the metal film according to RTP annealing temperature of metal film has been studied. Two types of oxides, BPSG and PETEOS, were used as a bottom layer under multi-layered metal films. We observed the interface between oxide and metal films using SEM (scanning electron microscopy), TEM (transmission electron microscopy), AES (auger electron spectroscopy). Bonding failure was occurred by interfacial reaction between the BPSG oxide and the multi-layered metal films above $650^{\circ}C$ RTP anneal. The phosphorus accumulation layer was observed at interface between BPSG oxide and metal films by AES and TEM measurements. On the other hand, bonding was always good in the sample using PETEOS oxide as a bottom layer. We have known that adhesion between BPSG and multi-layered metal films was improved when the sample was annealed below $650^{\circ}C$.

• Proceedings of the IEEK Conference
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• 대한전자공학회 2002년도 하계종합학술대회 논문집(2)
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• pp.225-228
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• 2002

The adhesion effect between the oxide layer and the metal layer has been studied by RTP anneal. Two types of oxides, BPSG and P-TEOS, were used as a bottom layer under multi-layered metal film. We observe the interface between oxide and metal layer using SEM (scanning electron microscopy), TEM (transmission electron microscopy), AES (auger electron spectroscopy). Adhesion failure was occurred by interfacial reaction between the BPSG oxide and the multi-layered metal film at 650"C RTP anneal. The phosphorus rich layer was observed at interface between BPSG oxide and metal layer by AES and TEM measurements. On the other hand adhesion was a)ways good in the sample used P-TEOS oxide as a bottom layer. We have known that adhesion between BPSG and multi-layered metal film was improved when the sample was annealed below $650^{\circ}C$.TEX>.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• 제27권11호
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• pp.679-685
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• 2014

For the measurements of surface shape milled using FIB (focused ion beam), the silicon bulk, $Si_3N_4/Si$, and Al/Si samples are used and observed the shapes milled from different sputtering rates, incident angles of $Ga^+$ ions bombardment, beam current, and target material. These conditions also can be influenced the sputtering rate, raster image, and milled shape. The fundamental ion-solid interactions of FIB milling are discussed and explained using TRIM programs (SRIM, TC, and T-dyn). The damaged layers caused by bombarding of $Ga^+$ ions were observed on the surface of target materials. The simulated results were shown a little bit deviation with the experimental data due to relatively small sputtering rate on the sample surface. The simulation results showed about 10.6% tolerance from the measured data at 200 pA. On the other hand, the improved analytical model of damaged layer was matched well with experimental XTEM (cross-sectional transmission electron microscopy) data.