• Applied Microscopy
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• v.46 no.3
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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.

• Applied Microscopy
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• v.42 no.1
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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.

• Journal of the Korean Ceramic Society
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• v.36 no.10
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• pp.1132-1138
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• 1999

• Applied Microscopy
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• v.26 no.2
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• pp.105-121
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• 1996

투과전자현미경을 이용한 최근의 재료 분석기술에 대해 일본 토호쿠대학의 ASMA (Atomic Scale Morphology Analysis) 연구실에서 얻은 실험결과를 중심으로 설명하였다. 현재 토호쿠대학에서 가동 중에 있는 가속전압 1250 kV의 초고압 투과전자현미경은 분해능이 약 0.1nm이며, 이 전자현미경으로부터 얻은 고분해능상은 대형컴퓨터를 이용한 시뮤레이션에 의해 해석 할 수 있음을 나타내었다. 또한, 이러한 뛰어난 고분해능 특성을 가진 초고압 투과전자현미경과 최근 재료 분야의 전자현미경 시료 제작기술의 하나로서 크게 주목받고 있는 초박절편법 (Ultramicrotomy)을 이용한 헤마타이트 미립자의 내부구조 해석 결과를 나타내었다. 새로운 전자현미경 분석기법을 위한 주변장비의 눈에 띄는 발달중의 하나로서 전자현미경상을 디지탈 형태로 기록하고, 이를 효과적인 화상처리 기법으로 해석할 수 있는 Imaging Plate (IP)를 주목할 수 있다. 본 논문에서는 IP의 응용 예로서 IP를 이용하여 기록한 고분해능 전자현미경상과 전자 회절패턴의 정량해석 결과에 대해 나타내었다. 에너지분산 X-선 검출기를 이용한 새로운 분석기법의 예로서 전자 채널링 효과를 이용한 ALCHEMI법을 Ni-Al-Mn계 화합물에 대한 실험결과와 함께 나타내었다. 또한, 전자에너지 손실 분광 분석법을 이용한 최근 분석 결과로서 여러 구리 화합물의 전자구조 차이에 따른 구리의 $L_{23}$ 가장자리 피이크 변화를 나타내었다. 새로운 전자현미경법인 에너지 필터를 사용하여 $Al_{0.5}In_{0.5}As$의 전자회절 패턴의 백그라운드를 제거한 결과를 에너지 필터를 사용하지 않은 $Al_{0.5}In_{0.5}As$의 전자회절 패턴과 비교하여 나타내었다.

• Journal of the Korean institute of surface engineering
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• v.25 no.2
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• pp.97-102
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• 1992

Transimission electron microscope(TEM)/ultramicrotomy were used to characterize the detailed surface morphology of 2024-T3 Al alloy surfaces prepared by various pretreatment process. It was found that, for good and superior initial adhesive strength and durability, chemically pretreated substrates appeared essential. The film morphology developed after CSA etching treatment, ass revealed by TEM, suggested the present of irregular cell pattern with finely separated whisker-like protrusion with was responsible for increase of bond strength.

• Korean Journal of Materials Research
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• v.12 no.7
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• pp.533-539
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• 2002

Porous anodic aluminum oxide layer for nano templates was prepared in acidic solutions. In order to investigate effects of 2nd anodization on ordered formation behaviors of the porous oxide layers, electrochemical and microstructural studies were performed, primarily using TEM, FE- SEM, AFM, and Ultramicrotomy. The pore diameter of the anodic oxide layer increased approximately linearly with increasing voltages, and to the contrary, the pore density decreased. It was shown that 2nd anodizing on the cell base after dissolving 1st anodic oxide layer was remarkably effective for forming ordered array of the pores, comparing with the case for 1st anodization only. And for controlling the diameter of pores, widening method by chemical dissolution seemed more practical than by electrochemical methods.

• Korean Journal of Materials Research
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• v.12 no.7
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• pp.540-544
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• 2002

Hydration treatments were performed on the pure aluminum substrate at $100^{\circ}C$ followed by anodizing and heat treatments on the layers. The transformation behaviors of the oxide layers according to the hydration treatment were studied using TEM, XRD, RBS etc. Above $90^{\circ}C$ the hydrous oxide film could be formed, which were turned out to be hydrous oxides(AlOOH $nH_2$O). The anodization on the hydrous oxide film was more effective for the transition of amorphous anodic oxides to the crystalline $\Upsilon-Al_2$ $O_3$ comparing with the case for anodizing on the aluminum substrate without hydration treatment And additional heat treatments were also helpful for the acceleration of the transformation of the hydrous oxide to $\Upsilon-Al_2$ $O_3$. During the heat treatment the interface between $\Upsilon-Al_2$ $O_3$and the hydrous oxide layers migrated to the outer side of hydrous layer.