• Applied Microscopy
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• 제45권2호
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• pp.101-105
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• 2015

Numerous digital image analysis techniques have been developed with regard to transmission electron microscopy (TEM) with the help of programming. DigitalMicrograph (DM, Gatan Inc., USA), which is installed on most TEMs as operational software, includes a script language to develop customized software for image analysis. Based on the DM script language, this work provides a script source listing for quantitative strain measurements based on a geometric phase analysis.

• Applied Microscopy
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• 제26권4호
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• pp.447-456
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• 1996

Fracture surfaces of materials contain useful information ranging from crack path to the mechanism of fracture. Since limitation of electron transparency requires a sample in the form of thin foil for TEM observations, it is impossible to extract such information directly from the fracture surfaces. In this study, the method of surface replication from the ceramic fracture surface is employed to characterize the process of crack propagation in ceramic matrix composites using TEM analysis. The surface replica from the fracture surface in ceramic materials provides detailed surface morphology and more importantly, loosened particles on the fracture surface are collected. Electron diffraction and chemical composition analyses of these particles reveal crack path in the specimen. Furthermore, one can determine the mode of fracture by observing the fracture surface morphology from the image of replica. Two examples are given to illustrate the potential of the surface replication technique. In the first example, apparent toughness increase in $B_{4}C-Al$ composites at high strain rate is investigated by surface replication to elucidate the mechanism of fracture at different strain rates. The polytypes of SiC formed during the sintering of SiC-AlN composite and their effect on the fracture behavior of SiC-AlN composite are analyzed in the second example.

• 대한금속재료학회지
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• 제50권7호
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• pp.511-516
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• 2012

Low temperature ${\delta}$-precipitation phenomenon below 2-step aging ($718^{\circ}C$, $8hr+621^{\circ}C$, 8 hr) temperature of cold drawn Inconel 718 alloy wire was investigated. The investigation was carried out on wires with a cold drawn ratio of 0, 20, 50 and 70% using OM, SEM, XRD, TEM, and DSC. In microstructures of 50 and 70% drawn wire, many precipitates were found along the grain boundaries and the twin boundaries in deformation band. From the results of the XRD and TEM analysis, the precipitates were identified as plate-like ${\delta}$-phase. From the results of the DSC analysis, it was also found that a temperature of ${\delta}$-precipitation decreases with an increase of the cold drawn ratio. We concluded that cold drawing of inconel 718 wire promotes the ${\delta}$-precipitation, and under the condition of a high drawing ratio, the ${\delta}$-phase could be precipitated at a temperature below the aging temperature ($718^{\circ}C$).

• Korean Chemical Engineering Research
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• 제46권6호
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• pp.1113-1118
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• 2008

$CuFe_2O_4$와 $Fe_3O_4$의 탄소 침적 및 환원 특성을 $900^{\circ}C$에서 TGA, XRD, SEM, TEM 등의 분석 및 반응 후 가스조성분석을 통하여 연구하였다. XRD 분석결과 환원된 $Fe_3O_4$는 Fe(iron)와 graphite(C) 그리고 $Fe_3C$으로 구성되어 있는 것으로 나타났다. 반면에, 환원된 $CuFe_2O_4$에서는 graphite나 $Fe_3C$가 나타나지 않았다. SEM을 이용하여 표면 구조를 관찰한 결과 환원된 $Fe_3O_4$의 표면이 탄소로 뒤덮여 있는 것을 확인할 수 있었다. 이와 달리 $CuFe_2O_4$에서는 $CH_4$ 전환율 및 환원속도가 높았고, 환원반응 후 탄소량 추정결과 $Fe_3O_4$에서보다 훨씬 낮게 나타났다. TEM 분석결과 $Fe_3O_4$ 입자로부터 탄소가 판상구조의 형태로 성장한 것을 확인할 수 있었다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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• pp.187-187
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• 2012

In this report, the plasmonic nanopores of less than 5 nm diameter were fabricated on the apex of the pyramidal cavity array. The metallic pyramidal pit cavity can also utilized as the plasmonic bioreactor, and the fabricated Au or Al metallic nanopore can provide the controllable translocation speed down using the plasmonic optical force. Initially, the SiO2 nanopore on the pyramidal pit cavity were fabricated using conventional microfabrication techniques. Then, the metallic thin film was sputter-deposited, followed by surface modification of the nanometer thick membrane using FESEM, TEM and EPMA. The huge electron intensity of FESEM with ~microsecond scan speed can provide the rapid solid phase surface transformation. However, the moderate electron beam intensity from the normal TEM without high speed scanning can only provide the liquid phase surface modification. After metal deposition, the 100 nm diameter aperture using FIB beam drilling was obtained in order to obtain the uniform nano-aperture. Then, the nanometer size aperture was reduced down to ~50 nm using electron beam surface modification using high speed scanning FESEM. The followed EPMA electron beam exposure without high speed scanning presents the reduction of the nanosize aperture down to 10 nm. During these processes, the widening or the shrinking of the nanometer pore was observed depending upon the electron beam intensity. Finally, using 200 keV TEM, the diameter of the nanopore was successively down from 10 nm down to 1.5 nm.

• Journal of Microbiology and Biotechnology
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• 제24권10호
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• pp.1354-1367
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• 2014

In the present work, we describe a simple, cheap, and unexplored method for "green" synthesis of silver nanoparticles using cell extracts of the cyanobacterium Anabaena doliolum. An attempt was also made to test the antimicrobial and antitumor activities of the synthesized nanoparticles. Analytical techniques, namely UV-vis spectroscopy, X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), and TEM-selected area electron diffraction, were used to elucidate the formation and characterization of silver-cyanobacterial nanoparticles (Ag-CNPs). Results showed that the original color of the cell extract changed from reddish blue to dark brown after addition of silver nitrate solution (1 mM) within 1 h, suggesting the synthesis of Ag-CNPs. That the formation Ag-CNPs indeed occurred was also evident from the spectroscopic analysis of the reaction mixture, wherein a prominent peak at 420 nm was noted. TEM images revealed well-dispersed, spherical Ag-CNPs with a particle size in the range of 10-50 nm. The X-ray diffraction spectrum suggested a crystalline nature of the Ag-CNPs. FTIR analysis indicated the utilization of a hydroxyl (-OH) group in the formation of Ag-CNPs. Ag-CNPs exhibited strong antibacterial activity against three multidrug-resistant bacteria. Additionally, Ag-CNPs strongly affected the survival of Dalton's lymphoma and human carcinoma colo205 cells at a very low concentration. The Ag-CNPs-induced loss of survival of both cell types may be due to the induction of reactive oxygen species generation and DNA fragmentation, resulting in apoptosis. Properties exhibited by the Ag-CNP suggest that it may be used as a potential antibacterial and antitumor agent.

• 전기화학회지
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• 제14권3호
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• pp.157-162
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• 2011

투과형 전자 현미경과 전기화학 임피던스 분광법을 이용하여 리튬 이차전지의 흑연 음극에 생성되는 표면피막의 고온 안정성을 고찰하였다. 투과형 전자 현미경을 이용한 분석에 의해 $60^{\circ}C$에서 저장되는 동안 표면피막의 일부가 전해질 용액 중에 용해되는 것이 확인되었으며, 이 과정에서 피막의 두께 감소 및 피막의 형상이 다공성 구조로 변하였다. 한편, 이 과정에서 피막의 조성 변화에 기인하는 것으로 추측되는 표면피막의 저항 증가가 전기화학 임피던스 분광법에 의하여 확인되었다. 표면피막의 고온 안정성은 vinylene carbonate, 1,3-propane sultone, etylene sulfite와 같은 첨가제에 의해 제한적으로 개선되었다.

• 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 $\alpha-Al_2O_3$.

• Corrosion Science and Technology
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• 제11권1호
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• pp.9-14
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• 2012

The formation of the Fe-Al inhibition layer in hot-dip galvanizing is a confusing issue for a long time. This study presents a characterization result on the inhibition layer formed on C-Mn-Cr and C-Mn-Si dual-phase steels after a short time galvanizing. The samples were annealed at $800^{\circ}C$ for 60 s in $N_{2}$-10% $H_{2}$ atmosphere with a dew point of $-30^{\circ}C$, and were then galvanized in a bath containing 0.2 %Al. X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) was employed for characterization. The TEM electron diffraction shows that only $Fe_{2}Al_{5}$ intermetallic phase was formed. No orientation relationship between the $Fe_{2}Al_{5}$ phase and the steel substrate could be identified. Two peaks of Al 2p photoelectrons, one from metallic aluminum and the other from $Al^{3+}$ ions, were detected in the inhibition layer, indicating that the layer is in fact a mixture of $Fe_{2}Al_{5}$ and $Al_{2}O_{3}$. TEM/EDS analysis verifies the existence of $Al_{2}O_{3}$ in the boundaries of $Fe_{2}Al_{5}$ grains. The nucleation of $Fe_{2}Al_{5}$ and the reduction of the surface oxide probably proceeded concurrently on galvanizing, and the residual oxides prohibited the heteroepitaxial growth of $Fe_{2}Al_{5}$.

• 한국재료학회지
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• 제17권4호
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• pp.207-214
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• 2007

We fabricated thermally-evaporated 10 -Ni/(poly)Si and 10 -Ni/1 -Ir/(poly)Si structures to investigate the microstructure of nickel monosilicide at the elevated temperatures required for annealing. Silicides underwent rapid at the temperatures of 300-1200 for 40 seconds. Silicides suitable for the salicide process formed on top of both the single crystal silicon actives and the polycrystalline silicon gates. A four-point tester was used to investigate the sheet resistances. A transmission electron microscope(TEM) and an Auger depth profile scope were employed for the determination of vertical section structure and thickness. Nickel silicides with iridium on single crystal silicon actives and polycrystalline silicon gates shoed low resistance up to 1000 and 800, respectively, while the conventional nickle monosilicide showed low resistance below 700. Through TEM analysis, we confirmed that a uniform, 20 -thick silicide layer formed on the single-crystal silicon substrate for the Ir-inserted case while a non-uniform, agglomerated layer was observed for the conventional nickel silicide. On the polycrystalline silicon substrate, we confirmed that the conventional nickel silicide showed a unique silicon-silicide mixing at the high silicidation temperature of 1000. Auger depth profile analysis also supports the presence of thismixed microstructure. Our result implies that our newly proposed iridium-added NiSi process may widen the thermal process window for the salicide process and be suitable for nano-thick silicides.