• Title/Summary/Keyword: TEM grid

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그래핀 합성 및 TEM grid막으로의 응용

  • Lee, Byeong-Ju;Jeong, Gu-Hwan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.461-461
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    • 2011
  • 최근의 나노기술의 발전과 함께 나노미터크기의 물질들의 물성과 미세구조 등을 분석하기 위한 노력들이 활발히 이루어지고 있다. 투과전자현미경(transmission electron microscope; TEM)은 나노물질의 미세구조 관찰, 화학성분 분석, 전자기적 특성평가가 가능한 초정밀 분석장비이다. TEM 관찰을 위한 시편의 제작방법중 TEM 그리드(grid)를 사용하는 방법은, 분석하고자 하는 물질을 망(mesh) 형태의 그리드에 도포하여 샘플을 준비하는 방법으로 다른 방법에 비해 아주 빠르고 간편한 장점이 있다. 그러나 TEM 그리드에 나노물질을 분산/도포하여 공중에 떠있는 형태로 샘플을 제작하려면, 나노물질이 mesh 사이로 빠져나오지 않도록 그리드 mesh의 간격이 아주 미세하여야 하는데, 일반적으로 mesh의 크기가 미세할수록 그리드의 가격은 높아진다. 또한 기존에 사용되고 있는 비정질 탄소박막으로 덮여진 그리드는 극미세 크기의 나노물질 및 탄소나노물질을 분석할 경우, 고해상도의 TEM상을 얻는데 한계가 있다. 한편 그래핀은 2차원의 육각판상의 구조로 탄소원자가 빼곡히 채워진 흑연 한 층의 나노재료이다. 이는 원자단위 두께로 가장 얇은 물질로서 기계적 강도가 우수하여 지지막으로의 응용이 가능하다고 알려져 있다. 따라서 TEM grid막으로 사용할 경우 기존의 고가의 미세한 mesh가 형성된 그리드를 사용하지 않아도 나노물질을 효과적으로 분석할 수 있을 것으로 예상 된다. 본 연구에서는 열화학증기증착법(thermal chemical vapor deposition; TCVD)을 이용하여 300 nm 두께의 니켈박막이 증착된 기판위에 대면적으로 합성한 그래핀을 TEM 관찰용 그리드 위에 전사(transfer)함으로써 나노물질이 그리드 mesh사이로 빠져나오지 않는 저가의 TEM 그리드 제작 방법 및 응용 가능성에 대하여 보고한다.

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Synthesis of Graphene Using Thermal Chemical Vapor Deposition and Application as a Grid Membrane for Transmission Electron Microscope Observation (열화학증기증착법을 이용한 그래핀의 합성 및 투과전자현미경 관찰용 그리드 멤브레인으로의 응용)

  • Lee, Byeong-Joo;Jeong, Goo-Hwan
    • Korean Journal of Materials Research
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    • v.22 no.3
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    • pp.130-135
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    • 2012
  • We present a method of graphene synthesis with high thickness uniformity using the thermal chemical vapor deposition (TCVD) technique; we demonstrate its application to a grid supporting membrane using transmission electron microscope (TEM) observation, particularly for nanomaterials that have smaller dimensions than the pitch of commercial grid mesh. Graphene was synthesized on electron-beam-evaporated Ni catalytic thin films. Methane and hydrogen gases were used as carbon feedstock and dilution gas, respectively. The effects of synthesis temperature and flow rate of feedstock on graphene structures have been investigated. The most effective condition for large area growth synthesis and high thickness uniformity was found to be $1000^{\circ}C$ and 5 sccm of methane. Among the various applications of the synthesized graphenes, their use as a supporting membrane of a TEM grid has been demonstrated; such a grid is useful for high resolution TEM imaging of nanoscale materials because it preserves the same focal plane over the whole grid mesh. After the graphene synthesis, we were able successfully to transfer the graphenes from the Ni substrates to the TEM grid without a polymeric mediator, so that we were able to preserve the clean surface of the as-synthesized graphene. Then, a drop of carbon nanotube (CNT) suspension was deposited onto the graphene-covered TEM grid. Finally, we performed high resolution TEM observation and obtained clear image of the carbon nanotubes, which were deposited on the graphene supporting membrane.

Three-dimensional Finite Difference Modeling of Time-domain Electromagnetic Method Using Staggered Grid (엇갈린 격자를 이용한 3차원 유한차분 시간영역 전자탐사 모델링)

  • Jang, Hangilro;Nam, Myung Jin;Cho, Sung Oh;Kim, Hee Joon
    • Geophysics and Geophysical Exploration
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    • v.20 no.3
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    • pp.121-128
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    • 2017
  • Interpretation of time-domain electromagnetic (TEM) data has been made mostly based on one-dimensional (1-D) inversion scheme in Korea. A proper interpretation of TEM data should employ 3-D TEM forward and inverse modeling algorithms. This study developed a 3-D TEM modeling algorithm using a finite difference time-domain (FDTD) method with staggered grid. In numerically solving Maxwell equations, fictitious displacement current is included based on an explicit FDTD method using a central difference approximation scheme. The developed modeling algorithm simulated a small-coil source configuration to be verified against analytic solutions for homogeneous half-space models. Further, TEM responses for a 3-D anomaly are modeled and analyzed. We expect that it will contribute greatly to the precise interpretation of TEM data.

Development of Multi-sample Loading Device for TEM Characterization of Hydroxyapatite Nanopowder

  • Lee, Jong-Moon;Kim, Jung-Kyun;Jeong, Jong-Man;Kim, Jin-Gyu;Lee, Eunji;Kim, Youn-Joong
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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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.

Sublimable materials facilitate the TEM sample preparation of oil-soluble nanomaterials

  • Yu-Hao Deng
    • Applied Microscopy
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    • v.50
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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.

Structural Analysis & Phase Transition of Amorphous Silica Nanoparticles Using Energy-Filtering TEM (EF-TEM을 이용한 비정질 실리카 나노입자의 구조 및 상전이 연구)

  • Park, Jong-Il;Kim, Jin-Gyu;Song, Ji-Ho;Kim, Youn-Joong
    • Applied Microscopy
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    • v.34 no.1
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    • pp.23-29
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    • 2004
  • In this study, we introduce the structural analysis of amorphous silica nanoparticles by EF-TEM electron diffraction and in-situ heating experiments. Three diffused rings were observed on the electron diffraction patterns of initial silica nanoparticles, while crystalline spot patterns were gradually appeared during the insitu heating process at $900^{\circ}C$. These patterns indicate the basic unit of $SiO_4$ tetrahedra consisting amorphous silica and gradual crystallization into the ideal layer structure of tridymite by heating. Under high vacuum condition in TEM, SiO nanoparticles were redeposited on the carbon grid after evaporation of SiO gas from $SiO_2$ above $850^{\circ}C$ and the remaining $SiO_2$ were crystallized into orthorhombic tridymite, consistent with ex-situ heating results in furnace at $900^{\circ}C$.

Deformation Behavior in Compatible Polymer Blends (고분자블렌드에서의 변형거동)

  • 전병철
    • Proceedings of the Materials Research Society of Korea Conference
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    • 1992.05a
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    • pp.121-121
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    • 1992
  • Deformation behavior of compatible polymer blends was studied using scanning electron, optical, and transmission electron microscopies. Four different compatible systems were employed and charaterized in this investigation : polystyrene(PS) and polyphenylene oxide(PPO), polystyrene(PS) and polyvinlmethylether(PVME), polystyrene(PS) and poly $\alpha$-methylstyrene(P$\alpha$MS). Individual craze and shear deformation zone microstructures were examined by transmission microscopy (TEM). For TEM observations, specimens deformed in-situ on a TEM grid were utilized. Quantiative analysis of these crazes and shear deformation zones was obtained from the nicrodensitometry of the TEM negatives in the manner developed by Lauterwasser and Kramer. Microdensitometry resulys showed that the fibril extension ratio decreased as the PPO content increased in the PS/PPO blends, and finally, for 100% PPO, only shear deformation zones were observed. For the PS/PVME blends, the ribril extension ratio also decreased as the VME content increased. For the PS/P$\alpha$MS blends, the fibril extension ratio increased as the P$\alpha$MS content increased, For the PPO/P$\alpha$MS blends, the fibril extension ratio increased as the P$\alpha$MS content increased.

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Transmission Electron Microscopy Specimen Preparation for Layer-area Graphene by a Direct Transfer Method

  • Cho, Youngji;Yang, Jun-Mo;Lam, Do Van;Lee, Seung-Mo;Kim, Jae-Hyun;Han, Kwan-Young;Chang, Jiho
    • Applied Microscopy
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    • v.44 no.4
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    • pp.133-137
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    • 2014
  • We suggest a facile transmission electron microscopy (TEM) specimen preparation method for the direct (polymer-free) transfer of layer-area graphene from Cu substrates to a TEM grid. The standard (polymer-based) method and direct transfer method were by TEM, high-resolution TEM, and energy dispersive X-ray spectroscopy (EDS). The folds and crystalline particles were formed in a graphene specimen by the standard method, while the graphene specimen by the direct method with a new etchant solution exhibited clean and full coverage of the graphene surface, which reduced several wet chemical steps and accompanying mechanical stresses and avoided formation of the oxide metal.