• Applied Microscopy
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• 제34권2호
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• pp.95-102
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• 2004

본 실험에서는 tripod polishing 방법을 이용하여 Pd/GaN/Sapphire 박막, PZT/MgO/Si 박막, 304 stainless steel 분말, $Mo_5Si_3/Mo_2B$ diffusion couple의 매우 다양한 물성이 포함된 불균질 재료의 TEM 시편을 제작하고 분석하였다. Tripod polishing을 사용하여 시편을 준비하면 시편의 종류에 관계없이 시편의 선단부에 매우 광범위한 전자빔 투과 영역을 지닌 TEM 시편을 얻을 수 있었으며, Pd/GaN/Sapphire 박막, PZT/MgO/Si 박막과 같이 기판이 경한 반도체 재료의 경우에는 연마 정도가 균일하며 연마과정 동안 오염이 심하지 않기 때문에 ion milling으로 cleaning 없이 TEM 관찰이 가능하다. 한편 304 stainless steel 분말과 같은 금속재료의 경우 짧은 시간의 ion milling 은 시편의 오염 제거에 도움된다. $Mo_5Si_3/Mo_2B$ diffusion couple에 형성된 실리사이드는 큰 취성 때문에 polishing 동안 시편이 깨지는 현상으로 전자가 투과할 수 있을 정도의 연마가 불가능하여 1시간 정도 ion milling 연마가 필요하다. Tripod polishing으로 TEM 시편을 준비하면 분석하고자 하는 지역을 정확하고도 넓게 연마할 수 있다. 또한 비교적 짧은 시간 내에 ion milling 없이 TEM 시편을 제작할 수 있기 때문에 ion milling에서 유발되는 여러 가지 문제점들을 해결할 수 있는 장점이 있었다. 그러나 tripod polishing은 전부 수작업으로 시편을 준비하기 때문에 시편을 제작하는 과정 동안 매우 세심한 주의가 요구되며 제작자의 숙련도와 경험을 필요로 하는 단점이 있다.

• 한국초전도ㆍ저온공학회논문지
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• 제8권1호
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• pp.9-14
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• 2006

Sample preparation plays a critical role in microstructure analysis using TEM. Although TEM specimen has been usually prepared by jet-polishing or Ar-ion beam milling technique. these methods could not be applied to YBCO CC which is composed of IBAD or RABiTS substrates, several buffet layers, and YBCO superconducting layer because of big difference in mechanical strengths between the metallic phase and oxide phases. To obtain useful cross-sectional information such as interface between the phases or second phases in YBCO CC, it is prerequisite to secure the large area of thin section in the cross-sectional direction. The superconducting layer or the buffer layers are relatively weak and fragile compared to the metallic substrate such as Ni-5wt%W RABiTS of Hastelloy-based IBAD, and preferential removal of weak ceramic phases during polishing steps makes specimen preparation almost impossible. Tripod polisher and small jig were home-made and employed to sample preparation. The polishing angle was maintained <$1^{\circ}$ throughout the polishing steps using 2 micrometers attached to the tripod plate. TEM specimens with large and thin area could be secured and used for RABiTS/IBAD substrate analyses. In some cases, additional Ar-beam ion milling with low beam current and impinging angle was used for less than 30 sec. to remove debris or polishing media attacked to the specimens.

• Applied Microscopy
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• 제45권4호
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• pp.203-207
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• 2015

Sample preparation is very important for crystal structure analysis of novel nanostructured materials in electron microscopy. Generally, a grid dispersion method has been used as transmission electron microscope (TEM) sampling method of nano-powder samples. However, it is difficult to obtain the cross-sectional information for the tabular-structured materials. In order to solve this problem, we have attempted a new sample preparation method using focused ion beam. Base on this approach, it was possible to successfully obtain the electron diffraction patterns and high-resolution TEM images of the cross-section of tabular structure. Finally, we were able to obtain three-dimensional crystallographic information of novel zeolite nano-crystal of the tabular morphology by applying the new sample preparation technique.

• 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.

• Corrosion Science and Technology
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• 제7권3호
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• pp.139-144
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• 2008

The results of microstructure observations of the $Al_2O_3$ scale formed on a Fe-Cr-Al steel during high temperature oxidation in the $SO_2$ atmosphere are presented. Morphology of the scale has been studied by SEM and TEM techniques. Phase and chemical compositions have been studied by EDX and XRD techniques. The alumina oxide is a primary component of the scale. TEM observations showed that the scale was multilayer. The entire surface of the scale is covered with "whiskers", which look like very thin platelets and have random orientation. The cross section of a sample shows, that the "whiskers" are approximately $2{\mu}m$ high, however the compact scale layer on which they reside is $0.2{\mu}m$ thick. The scale layer was composed mainly of small equiaxial grains and a residual amount of small columnar grains. EDX analysis of the scale surface showed that the any sulfides were found in the formed outer and thin inner scale layer. A phase analysis of the scale formed revealed that it is composed mainly of the $\theta-Al_2O_3$ phase and a residual amount of $\alpha-Al_2O_3$.

• Journal of Korean Vacuum Science & Technology
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• 제6권2호
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• pp.92-96
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• 2002

In this paper, we treated the Ni$_3$Al based alloy samples with intense pulsed ion beams (IPIB) at the beam parameters of 250KV acceleration voltage, 100 - 200 A/cm$^2$ current density and 60 u pulse duration. We simulated the thermal-mechanical process near the surface of Ni$_3$Al based alloy with our STEIPIB codes. The surface morphology and the cross-section microstructures of samples were observed with SEM, the composition of the sample surface layer was determined by X-ray Energy Dispersive Spectrometry (XEDS) and the microstructure on the surface was observed by Transmission Electron Microscope (TEM). The results show that heating rate increases with the current density of IPIB and cooling rate reached highest value less than 150 A/cm$^2$. The irradiation of IPIB induced the segregation of Mo and adequate beam parameter can improve anti-oxidation properly of IC6 alloy. Some craters come from extraneous debris and liquid droplets, and some maybe due to the melting of the intersection region of interphase. Increasing the pulse number enlarges average size of craters and decreases number density of craters.