• Applied Microscopy
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• v.46 no.1
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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.

• Journal of the Korean institute of surface engineering
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• v.53 no.1
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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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• v.48 no.2
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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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• 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.

• Journal of Science and Technology Studies
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• v.11 no.2
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• pp.67-96
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• 2011

Studies in scientific visualization have disclosed a visual chain among many scientific visualizations, which starts from the photographs that have many details to diagrams that enable scientists to make specific claims due to their abstract characters. Located at both ends of the visual chain, photographs and diagrams are regarded as being different kinds and having different characteristics. The photographs - or microphotographs to be precise - that this paper discusses, however, had been removed of unnecessary details and were prepared with carful attention to illustrative functions that diagrams usually perform. Following microphotographic changes in a Korean laboratory, this article shows that the knowledge of specimen preparation was transmitted from an American leading group to the Korean laboratory through a direct contact, and that with this, the technique of taking microphotographs of the laboratory was much improved. The specimen preparation method is, however, a tacit knowledge that is invisible in both group's papers. This article argues that the method of specimen preparation is the driving force that made the microphotographs act like carefully prepared diagrams and acquire objectivity.

• Applied Microscopy
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• v.46 no.2
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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.

• The Korean Journal of Cytopathology
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• v.16 no.1
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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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• v.32 no.4
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• pp.311-317
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• 2002

There is great requirement on the TEM specimen preparation method with particle size selectivity as a prerequisite for the quantitative structure analysis on the materials such as gibbsite powder, which generally forms a large agglomerate and shows a variation of transition process depending on their sizes. In this experiment, we made an attempt to give a methodology for the TEM specimen preparation of powder with the size selectivity. After mixing 1 wt% gibbsite powder with ethanol solvent, gibbsite suspension was prepared by application of ball-milling and ultrasonification with addition of 0.25 vol% dispersion agent, Darvan C, which was diluted into distilled water by the ratio 1:19. Appling the static sedimentation method to gibbsite suspension after estimation of the sedimentation time by the measurement of accumulative concentration variation, we acquired TEM specimens with well-dispersed and size selected gibbsite particles in nm scale. Overall picture of each sample was taken by SEM and morphology of each dispersed particle was imaged by TEM. Raw and processed gibbsite powders were also examined by XRD to investigate whether they were suffered from phase change during the process or not.

• Applied Microscopy
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• v.39 no.3
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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.

• Resources Recycling
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• v.17 no.4
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• pp.30-36
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• 2008

The preparation of porous lightweight materials as well as the measurement of physical properties has been performed by using SSA(sewage sludge ash) as the raw material. For this aim, two types of lightweight filler, that is, perlite and silica sphere were employed respectively and bentonite was also used as an inorganic binder. The properties of lightweight specimen calcined at 1,000 were measured in terms of density, compressive strength, thermal conductivity and sound absorption to examine the effect of material composition as well as the preparation condition on the properties of lightweight material. As a result, the density of specimen prepared with perlite was ranged from 1.23 to $1.37g/cm^3$ and the compressive strength was ranged from 242.3 to $370.5kg/cm^2$. In case of specimen prepared with silica sphere, it was found that the compressive strength was less than $100kg/cm^2$ even though density was lower than that of specimen with perlite. As far as the thermal conductivity of specimen was concerned, it was ranged from 0.3 to $0.5W/m^{\circ}K$ depending on material composition so that the insulation effect was superior to conventional concrete.