• Applied Microscopy
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• 제46권1호
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• pp.14-19
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• 2016

Currently, focused ion beams (FIB) are widely used for specimen preparation in atom probe tomography (APT), which is a three-dimensional and atomic-scale compositional analysis tool. Specimen preparation, in which a specific region of interest is identified and a sharp needle shape created, is the first step towards successful APT analysis. The FIB technique is a powerful tool for site-specific specimen preparation because it provides a lift-out technique and a controllable manipulation function. In this paper, we demonstrate a general procedure containing the crucial points of FIB-based specimen preparation. We introduce aluminum holders with moveable pin and an axial rotation manipulator for specimen handling, which are useful for flipping and rotating the specimen to present the backside and the perpendicular direction. We also describe specimen preparation methods for nanowires and nanopowders, using a pick-up method and an embedding method by epoxy resin, respectively.

• 한국표면공학회지
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• 제53권1호
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• pp.29-35
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• 2020

In this study, five different specimen preparation methods were introduced and their advantages and disadvantages were presented. One of them, an epoxy mounting method has advantages of constant exposure area, ease of surface preparation without touching the specimen surface during polishing or cleaning, use of small amount of material and ease of specimen reuse by polishing or etching. However, in order to eliminate unexpected errors resulting from preferable reaction at the specimen/epoxy interface and contact resistance between the specimen and copper conducting line for electrical connection, it is recommended to cover the wall side of the specimen with porous anodic oxide films and to remain the contact resistance lower than 1 ohm. The increased contact resistance between the specimen and Cu conducting line appeared to result in increases of anodizing voltage and solution temperature during anodizing by which thickness and hardness of anodizing film on Al2024 alloy were drastically decreased and color of the films became more brightened.

• Applied Microscopy
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• 제48권2호
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• pp.49-53
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• 2018

A successful transmission electron microscope (TEM) analysis is closely related to the preparation of the TEM specimen and should be followed by the suitable TEM specimen preparation depending on the purpose of analysis and the subject materials. In the case of the Si-based anode material, lithium atoms of formed Li silicide were removed due to ion beam and electron beam during TEM specimen preparation and TEM observation. To overcome the problem, we proposed a new technique to make a TEM specimen without the ion beam damage. In this study, two types of test specimens from the Si-based anode material of Li-ion battery were prepared by respectively adopting the only focused ion beam (FIB) method and the new FIB-ultramicrotome method. TEM analyses of two samples were conducted to compare the Ga ion damage of the test specimen.

• Applied Microscopy
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• 제44권4호
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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.

• 과학기술학연구
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• 제11권2호
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• pp.67-96
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• 2011

그동안 시각 이미지 연구들은 풍부한 세부 사항을 담은 사진으로부터 특정한 과학자의 주장을 담은 다이어그램까지 이어지는 시각적 연쇄(visual chain)에 주목해왔다. 이 때 시각적 연쇄의 양 끝에 위치한 사진과 다이어그램은 서로 다른 종류의, 다른 성격을 지닌 시각 이미지로 여겨졌다. 그러나 이 글에서 소개할 현미경 사진은 제작 과정에서 불필요한 세부 사항이 제거되고, 특정한 정보를 담은 다이어그램과 같은 성격을 띠게 된다. 사례로 다룬 현미경 사진은 풍부한 세부사항을 담기 때문에 객관적이라 여겨지는 시각적 연쇄의 사진에 대입되지 않는 것이다. 그렇다면 이 현미경 사진이 사진으로서 객관성을 유지할 수 있는 원동력은 무엇일까? 이 글은 국내의 한 실험실이 겪었던 현미경 사진의 변화를 추적한다. 후발 그룹인 실험실이 경험한 현미경 사진 향상은 선도 그룹과의 직접 접촉을 통해 전달받은 표본 제작법 때문이었다. 표본 제작법은 암묵지로서 논문에서 상당 부분 감추어지며, 이 때문에 현미경 사진은 자신에게 특정한 의미를 부여했던 탄생 배경으로부터 분리되어 객관성을 유지할 수 있게 된다. 사례로 다룬 현미경 사진이 다이어그램과 같은 성격을 지니며 동시에 사진으로서 객관성을 유지할 수 있었던 원동력을 표본 제작법에서 찾을 수 있다. 이 글은 표본 제작법에 주목하여 기존 연구에서는 강조되지 못했던 현미경 사진의 새로운 측면을 드러내고 있다.

• 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.

• 대한세포병리학회지
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• 제16권1호
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• pp.10-17
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• 2005

This study was performed to compare manual liquid-based preparation with conventional Papanicolaou tests in view of the cytologic diagnoses and specimen adequacy. The specimens of 5,979 women from 33 local clinics and 1 general hospital were prepared by both manual liquid-based preparation and conventional Papanicolaou test. The cytologic diagnoses and specimen adequacy were evaluated in Department of Fathology in Kyoungpook National University School of Medicine. A conventional Papanicolaou test was always prepared first, after that residual material on the sampling device was rinsed into a liquid preservative, and then thin-layer slides were prepared using manual method of liquid-based cervicovaginal cytology. Conventional and liquid-based slides were read independently, and cytologic diagnoses and specimen adequacy were classified using the Bethesda System. Of the cases, 5,763 (96.3%,) had the same interpretation, and there was no significant diagnostic difference in 5,853 (97.8%) cases. When evaluating cases with more than one diagnostic class difference, the manual liquid-based preparation demonstrated a statistically significant overall improvement (2.1%) in the detection of squamous intraepithelial lesion and invasive cancer. Using manual method of liquid-based preparation, there was 14.1%, reduction in unsatisfactory slides through excellent cellular presentation. In conclusion, the manual liquid-based preparation produces standardized quality, superior sensitivity and improved adequacy as compared to the conventional method.

• Applied Microscopy
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• 제32권4호
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• pp.311-317
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• 2002

입자 크기에 따라 상전이 경로가 달라지며 매우 큰 응집체로 존재하는 gibbsite 분말과 같은 재료의 정량적인 전이 구조 분석의 전제로서 입자 크기가 선택적인 TEM 시편의 준비가 절실히 요구된다. 입자 크기 선택성을 실현한 TEM 시편 준비의 방법론을 확립하기 위한 방안으로서 본 실험이 전개되었다. 약 1 wt%의 gibbsite 원료 분말을 에탄올 용매에 혼합 한 뒤, ball-milling에 의해 조분쇄 처리를 하고 증류수에 1 : 19의 비로 희석된 분산 조제, Darvan C, 0.25 vol%의 첨가와 함께 ultrasonic 처리를 하여 gibbsite suspension을 만들었다. 제조된 gibbsite suspension의 누적 농도 변화 관찰에 의한 침강 시간의 조정 후 정적 침강 분리에 의해 nm 크기별로 분리된 TEM 시편을 만들 수가 있었다. 시편의 전체적인 양상은 SEM으로 관찰하였고 개개 입자들의 morphology 는 TEM으로 분석하였다. 또한, 공정 과정 중의 상변화 가능성을 검토하기 위해 XRD 분석을 실시하였다.

• Applied Microscopy
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• 제39권3호
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• pp.277-281
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• 2009

Practical difficulties for preparing a good crosssectional specimen of GaN-based materials for transmission electron microscopy have arisen due to large difference of mechanical properties between hard ceramic substrate and soft GaN-layered materials. Uneven polishing, sudden cracking, delamination, and selective sputtering during the conventional wedge polishing technique are often encountered as experimental hindrances. The preparation technique based on Strecker's method can be applied to overcome these difficulties, which eventually leads to mechanically stable TEM samples independent of the mechanical properties of materials. The basic idea is to use hard ceramic dummy filler for embedding the sample of interest into the dummy frame. In this study, we applied this technique into preparing cross-sectional TEM specimen of the GaN-based materials with mechanical instability and demonstrated usefulness of this hard dummy filler method in which the possible modifications of the sample of interest during the preparation must be avoidable. In addition, practical precautions during the preparation were discussed.

• 자원리싸이클링
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• 제17권4호
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• pp.30-36
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• 2008

본 연구에서는 하수슬러지 소각재를 원료로 사용한 다공성 경량재료의 제조 및 물성측정 실험을 수행하였다. 경량충진재로써 perlite와 silica sphere의 2종류 경량물질을 각각 사용하였으며, 무기바인더로써 벤토나이트를 첨가하여 $1,000^{\circ}C$에서 소성하는 방법으로 경량재료를 제조하였다. 제조한 시편은 밀도, 압축강도, 열전도도 및 흡음율을 측정하여 원료 조성 및 제조 조건에 따른 각각의 물성변화를 조사하였다. 실험결과 perlite를 경량충진재로 사용한 시편의 밀도는 $1.23{\sim}1.37g/cm^3$, 압축강도는 $242.3{\sim}370.5kg/cm^2$로 나타났으며, silica sphere를 사용한 경우는 perlite에 비해 밀도가 낮고 압축강도가 $100kg/cm^2$ 이하인 것으로 나타났다. 또한, 경량재료의 열전도도는 원료 조성에 따라 $0.3{\sim}0.5W/m^{\circ}K$의 수치를 보여 일반 콘크리트보다 단열효과가 매우 우수한 것으로 나타났다.