• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.109-110
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• 2014

주사전자현미경(Scanning Electron Microscopy: SEM)은 고체상태에서 미세조직과 형상을 관찰하는 데에 가장 다양하게 쓰이는 분석기기로서 최근에 판매되고 있는 고분해능 SEM은 수 나노미터의 분해능을 가지고 있다. 그리고 SEM의 초점심도가 크기 때문에 3차원적인 영상의 관찰이 용이해서 곡면 혹은 울퉁불퉁한 표면의 영상을 육안으로 관찰하는 것처럼 보여준다. 활용도도 매우 다양해서 금속파면, 광물과 화석, 반도체 소자와 회로망의 품질검사, 고분자 및 유기물, 생체시료 nnnnnnnnn와 유가공 제품 등 모든 산업영역에 걸쳐 있다(Fig. 1). 입사된 전자빔이 시료의 원자와 탄성, 비탄성 충돌을 할 때 2차 전자(secondary electron)외에 후방산란전자(back scattered electron), X선, 음극형광 등이 발생하게 되는 이것을 통하여 topography (시료의 표면 형상), morphology(시료의 구성입자의 형상), composition(시료의 구성원소), crystallography (시료의 원자배열상태)등의 정보를 얻을 수 있다. SEM은 2차 전자를 이용하여 시료의 표면형상을 측정하고 그 외에는 SEM을 플랫폼으로 하여 EDS (Energy Dispersive X-ray Spectroscopy), WDS (Wave Dispersive X-ray Spectroscope), EPMA (Electron Probe X-ray Micro Analyzer), FIB (Focus Ion Beam), EBIC (Electron Beam Induced Current), EBSD (Electron Backscatter Diffraction), PBMS (Particle Beam Mass Spectrometer) 등의 많은 분석장치들이 SEM에 부가적으로 장착되어 다양한 시료의 측정이 이루어진다. 이 중 결정구조, 조성분석을 쉽고 효과적으로 할 수 있게 하는 X선 분석장치인 EDS를 SEM에 일체화시킨 장비와 EDS 및 PBMS를 SEM에 장착하여 반도체 공정 중 발생하는 나노입자의 형상, 성분, 크기분포를 측정하는 PCDS(Particle Characteristic Diagnosis System)에 대해 소개하고자 한다. - EDS와 통합된 SEM 시스템 기본적으로 SEM과 EDS는 상호보완적인 기능을 통하여 매우 밀접하게 사용되고 있으나 제조사와 기술적 근간의 차이로 인해 전혀 다른 방식으로 운영되고 있다. 일반적으로 SEM과 EDS는 별개의 시스템으로 스캔회로와 이미지 프로세싱 회로가 개별적으로 구현되어 있지만 로렌츠힘에 의해 발생하는 전자빔의 왜곡을 보정을 위해 EDS 시스템은 SEM 시스템과 연동되어 운영될 수 밖에 없다. 따라서, 각각의 시스템에서는 필요하지만 전체 시스템에서 보면 중복된 기능을 가지는 전자회로들이 존재하게 되고 이로 인해 SEM과 EDS에서 보는 시료의 이미지의 차이로 인한 측정오차가 발생한다(Fig. 2). EDS와 통합된 SEM 시스템은 중복된 기능인 스캔을 담당하는 scanning generation circuit과 이미지 프로세싱을 담당하는 FPGA circuit 및 응용프로그램을 SEM의 회로와 프로그램을 사용하게 함으로 SEM과 EDS가 보는 시료의 이미지가 정확히 일치함으로 이미지 캘리브레이션이 필요없고 측정오차가 제거된 EDS 측정이 가능하다. - PCDS 공정 중 발생하는 입자는 반도체 생산 수율에 가장 큰 영향을 끼치는 원인으로 파악되고 있으며, 생산수율을 저하시키는 원인 중 70% 가량이 이와 관련된 것으로 알려져 있다. 현재 반도체 공정 중이나 반도체 공정 장비에서 발생하는 입자는 제어가 되고 있지 않은 실정이며 대부분의 반도체 공정은 저압환경에서 이루어지기에 이 때 발생하는 입자를 제어하기 위해서는 저압환경에서 측정할 수 있는 측정시스템이 필요하다. 최근 국내에서는 CVD (Chemical Vapor Deposition) 시스템 내 파이프내벽에서의 오염입자 침착은 심각한 문제점으로 인식되고 있다(Fig. 3). PCDS (Particle Characteristic Diagnosis System)는 오염입자의 형상을 측정할 수 있는 SEM, 오염입자의 성분을 측정할 수 있는 EDS, 저압환경에서 기체에 포함된 입자를 빔 형태로 집속, 가속, 포화상태에 이르게 대전시켜 오염입자의 크기분포를 측정할 수 있는 PBMS가 일체화 되어 반도체 공정 중 발생하는 나노입자 대해 실시간으로 대처와 조치가 가능하게 한다.

• Korean Journal of Materials Research
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• v.24 no.10
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• pp.520-525
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• 2014

Effects of Cu and B on effective grain size and low-temperature toughness of thermo-mechanically processed high-strength bainitic steels were investigated in this study. The microstructure of the steel specimens was analyzed using optical, scanning, and transmission electron microscopy; their effective grain size was also characterized by electron back-scattered diffraction. To evaluate the strength and low-temperature toughness, tensile and Charpy impact tests were carried out. The specimens were composed of various low-temperature transformation products such as granular bainite (GB), degenerated upper bainite (DUB), lower bainite (LB), and lath marteniste (LM), dependent on the addition of Cu and B. The addition of Cu slightly increased the yield and tensile strength, but substantially deteriorated the low-temperature toughness because of the higher volume fraction of DUB with a large effective grain size. The specimen containing both Cu and B had the highest strength, but showed worse low-temperature toughness of higher ductile-brittle transition temperature (DBTT) and lower absorbed energy because it mostly consisted of LB and LM. In the B-added specimen, on the other hand, it was possible to obtain the best combination of high strength and good low-temperature toughness by decreasing the overall effective grain size via the appropriate formation of different low-temperature transformation products containing GB, DUB, and LB/LM.

• Journal of People, Plants, and Environment
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• v.24 no.6
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• pp.585-593
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• 2021

Background and objective: Illegal open-air incineration, which is criticized as a leading source of air pollutants among agricultural activities, currently requires constant effort and attention. Countries around the world have been undertaking studies on the emission of heavy metal substances in fine dust discharged during the incineration process. A precise analytical method is required to examine the harmful effects of particulate pollutants on the human body. Methods: In order to simulate open-air incineration, the infrastructure needed for incineration tests complying with the United States Environmental Protection Agency (EPA) Method 5G was built, and a large-area analysis was conducted on particulate pollutants through automated scanning electron microscopy (SEM)-energy-dispersive X-ray spectroscopy (EDS). For the test specimen, high-density polyethylene (HDPE) waste collected by the DangJin Office located in Choongcheongnam-do was used. To increase the identifiability of the analyzed particles, the incineration experiment was conducted in an incinerator three times after dividing the film waste into 200 g specimens. Results: Among the metal particulate matters detected in the HDPE waste incineration test, transition metals included C (20.8-37.1 wt%) and O (33.7-37.9 wt%). As for other chemical matters, the analysis showed that metal particulate matters such as metalloids, alkali metals, alkaline earth metals, and transition metals reacted to C and C-O. Si, a representative metalloid, was detected at 14.8-20.8 wt%, showing the highest weight ratio except for C and O. Conclusion: In this study, the detection of metal chemicals in incinerated particulate matters was effectively confirmed through SEM-EDS. The results of this study verified that HDPE waste adsorbs metal chemicals originating from soil due to its own properties and deterioration, and that when incinerated, it emits particulate matters containing transition metals and other metals that contribute to the excessive production and reduction of reactive oxygen species.

• Journal of the Mineralogical Society of Korea
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• v.16 no.3
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• pp.255-263
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• 2003

Margarite, occurring in an Unkyori Formation of Miwon area, Chungcheongbukdo, South Korea, was investigated using a high-resolution transmission electron microscope (HRTEM) to reveal the microstructural intergrowth textures of margarite. HRTEM images of margarite, which was previously confirmed to have intergrowth textures by petrographic microscope and back-scattered electron images, show that chlorite occurs as thin packets of layers interlayered within margarite crystals, and intercalated chlorite layers are intergrown irregularly in areas as a few hundred angstroms thick slabs or isolated chlorite unit layers. Margarite crystals observed by HRTEM consist of a well-ordered 2M polytype, and electron diffraction pattern shows no prominent streaking along the 001 (or $c^{*}$) direction, indicating that there is no significant stacking disorder in margarite. Intercalated extra brucite-like layers, which are approximately 5 $\AA$ thick, are observed locally within margarite crystals. Insertion of such extra brucite-like layer at the interlayer of margarite would result in a chlorite-like structure unit. (001) margarite layers are parallel to (001) of chlorite, and margarite layers are not extended from (001) of chlorite, indicating that margarite was apparently produced through a dissolution-precipitation mechanism.m.

• Journal of the Korean Recycled Construction Resources Institute
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• v.5 no.4
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• pp.435-441
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• 2017

Studies on self-healing have currently been diversified and the methods to evaluate the studies have become more diversified as well. Among them, the back-scattered electron (BSE) image acquired through the scanning electron microscope (SEM) is attempted as the means to evaluate the self-healing effect on cracks. In order evaluate by the BSE image, sophisticated pre-processing of specimen is critical and this injected inside the particle, pore and artificial crack of the hardener to stabilize the structure of the newly generated self-healing product and it enables to endure the stress on polishing without deformation. The impregnated specimen smoothen the surface to obtain the BSE image of high resolution that polishing is made for diamond suspension for wet polishing after dry polishing. As a result of evaluating the self-healing product on the impregnated and polished self-healing specimen, the generated product is formed from the surface of the artificial crack and the self-healing substances are confirmed as $Ca(OH)_2$ and C-S-H.

• Korean Journal of Materials Research
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• v.21 no.5
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• pp.263-267
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• 2011

The present study was carried out to evaluate the microstructural and mechanical properties of cross-roll rolled pure copper sheets, and the results were compared with those obtained for conventionally rolled sheets. For this work, pure copper (99.99 mass%) sheets with thickness of 5 mm were prepared as the starting material. The sheets were cold rolled to 90% thickness reduction and subsequently annealed at $400^{\circ}C$ for 30 min. Also, to analyze the grain boundary character distributions (GBCDs) on the materials, the electron back-scattered diffraction (EBSD) technique was introduced. The resulting cold-rolled and annealed sheets had considerably finer grains than the initial sheets with an average size of 100 ${\mu}M$. In particular, the average grain size became smaller by cross-roll rolling (6.5 ${\mu}M$) than by conventional rolling (9.8 ${\mu}M$). These grain refinements directly led to enhanced mechanical properties such as Vickers micro-hardness and tensile strength, and thus the values showed greater increases upon cross-roll rolling process than after conventional rolling. Furthermore, the texture development of <112>//ND in the cross-roll rolling processed material provided greater enhancement of mechanical properties relative to the case of the conventional rolling processed material. In the present study, we systematically discuss the enhancement of mechanical properties in terms of grain refinement and texture distribution developed by the different rolling processes.

• Economic and Environmental Geology
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• v.53 no.2
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• pp.183-196
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• 2020

This study aimed to recover native gold from the concentrate using microwave-nitric acid leaching and magnetic/hydro separation experiments. The insoluble-residue was filtered from leaching solution through microwave-nitric acid leaching experiment. As a result of the atomic absorption spectrometer(AAS) analysis of the filtered leaching solution, it was discovered that Au content was not eluted at all and it was observed from the back scattered electron(BSE) image that native gold was liberated in the insoluble-residue. When magnetic/hydro separation experiments were applied for the insoluble-residue, magnetic and non magnetic minerals were separtated from insoluble-residue. Magnetite was recovered from the magnetic minerals and as a result of applying the hydro separation experiment again for the non-magnetic mineral, native gold was recovered. The native gold was identified through the X-ray diffraction(XRD) analysis and BSE image.

• Korean Journal of Materials Research
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• v.23 no.5
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• pp.293-298
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• 2013

In this study, an HP-mod. type(KHR-45A), which is used as a heater tube material in the pyrolysis process, was evaluated for its carburizing properties. It was confirmed from the microstructural observation of the tubes that the volume fraction of carbide increased and that the coarsening of Cr-carbide generated as a degree of carburization increased. The depth of the hardened layer, which is similar to the thickness of the carburized region of each specimen, due to carburization is confirmed by measurement of the micro-Vickers hardness of the cross section tube, which thickness is similar to that of the carburized region of each specimen. Two types of chromium carbides were identified from the EBSD (electron back-scattered diffraction) image and the EDS (energy-dispersive spectroscopy) analysis: Cr-rich $M_{23}C_6$ in the outer region and Cr-rich $M_7C_3$ in the inner region of tubes. The EDS analysis revealed a correlation between the ferromagnetic behavior of the tubes and the chromium depletion in the matrix. The chromium depletion in the austenite matrix is the main cause of the magnetization of the carburized tube. The method used currently for the measurement of the carburization of the tubes is confirmed; carburizing evaluation is useful for magnetic flux density measurement. The volume fraction of the carbide increased as the measuring point moved into the carburized side; this was determined from the calculation of the volume fraction in the cross-section image of the tubes. These results are similar to the trends of carburization measurement when those trends were evaluated by measurement of the magnetic flux density.

• Korean Journal of Materials Research
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• v.21 no.10
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• pp.556-562
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• 2011

We carried out this study to evaluate the grain refining in and the mechanical properties of alloys that undergo severe plastic deformation (SPD). Conventional rolling (CR) and cross-roll rolling (CRR) as SPD methods were used with Ni-20Cr alloy as the experimental material. The materials were cold rolled to a thickness reduction of 90% and subsequently annealed at $700^{\circ}C$ for 30 min to obtain a fully recrystallized microstructure. For the annealed materials after the cold rolling, electron back-scattered diffraction (EBSD) analysis was carried out to investigate the grain boundary characteristic distributions (GBCDs). The CRR process was more effective when used to develop the grain refinement relative to the CR process; as a result, the grain size was refined from $70{\mu}m$ in the initial material to $4.2{\mu}m$ (CR) and $2.4{\mu}m$ (CRR). These grain refinements have a direct effect on improving the mechanical properties; in this case, the microhardness, yield and tensile strength showed significant increases compared to the initial material. In particular, the CRR-processed material showed more effective values relative to the CR-processed materials. The different texture distributions in the CR (001//ND) and CRR (111//ND) were likely the cause of the increase in the mechanical properties. These findings suggest that CRR can result in materials with a smaller grain size, improved texture development and improved mechanical properties after recrystallization by a subsequent annealing process.

• Korean Journal of Metals and Materials
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• v.49 no.1
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• pp.58-63
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• 2011

The grain size and growth direction of a directionally solidified turbine blade were evaluated by the initial nucleation condition at the start block of directional solidification. The initial nucleation condition was controlled by inserting a Ni foil on the directional solidification plate of the directional solidification furnace. Fine grains with good orientation were obtained in the faster cooling condition at the start block. The nucleus number was compared with the cooling rate of the start block by electron back scattered diffraction (EBSD). DSC (differential scanning calorimeter) analysis was performed to compare the melting point and undercooling for nucleation of the coarse nuclei and fine nuclei of the start block. The faster cooling condition at the start block showed more undercooling for nucleation and smaller size of nuclei which resulted in a fine grain with good orientation in the directional turbine blade.