• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.8 no.2
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• pp.254-263
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• 1998

A worker employed in a serpentine mine was found developed mesothelioma as the first case of Korea in 1997. Asbestos was known as a causative agent for mesothelioma. Thus, asbestos contamination in mines could be a big health threat to those workers who were unknowingly exposed. However, there was no report that any minerals found in Korea contained asbestos. This study was carried out to find the presence of any asbestiform fibers in minerals which could be obtained in Korean mines. We examined fifteen minerals from 44 mines which were suspected contaminated with asbestiform fibers. Asbestiform analysis was done with high resolution transmission electron microscope(TEM), with energy dispersive X-ray spectroscope(EDX) and X-ray diffraction(XRD) analyses. Among asbestiform fibers, chrysotile was found in chrysotile, serpentine, talc and pyrophylite specimens from 11 mines. Tremolite was found in tremolite and talc specimens from three mines. Mordenite was found in zeolite specimens from two mines. Wallastonite and sepiolite were found in wallastonite and sepiolite specimens respectively. Crocidolite, antigorite and actinolite were found from talc specimens. But no asbestiform fiber contaminants were found in doromite, vermiculite, limestone, marble, gypsum, kaolin, and clary specimens. Thus, these asbestiform fibers such as such as chrysotile, tremolite, mordenite, crocidolite, antigorite and actinolite could be the responsible agents for the health hazards such as mesothelioma and other cancers.

• Journal of Conservation Science
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• v.35 no.2
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• pp.145-152
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• 2019

The metal-manufacturing method and smelting temperature of ancient metal-production processes have been studied by analyzing the principal elements and microstructures of slag. However, the microstructure of slag varies according to the solidification cooling rate and types and relative amounts of various oxides contained within the smelting materials. Hence, there is a need for accurate analysis methods that allow slag to be distinguished by more than its composition or microstructure. In this study, the microstructures of slag discharged as a result of smelting iron sands collected from Pohang and Gyeongju, as well as the slag excavated from the Ungyo site in Wanju, were analyzed by using metalloscopy, scanning election microscopy-energy dispersine X-ray spectroscopy(SEM-EDS) and wavelength dispersive X-ray fluorenscence(WD-XRF). Furthermore, the microcrystals were accurately characterized by performing Raman micro-spectroscopy, which is a technique that can be used to identify the microcrystals of slags. SEM-EDS analysis of Pohang slag indicated that its white polygonal crystals could be Magnetite; however, Raman micro-spectroscopy revealed that these crystals were actually $ulv{\ddot{o}}spinel$. Raman micro-spectroscopy and SEM-EDS were also used to verify that the coarse white dendritic structures observed in the Gyeongju-slag were $W{\ddot{u}}stites$. Additionally, the Wanju slag was observed to have a glassy matrix, which was confirmed by Raman micro-spectroscopy to be Augite. Thus, we have demonstrated that Raman micro-spectroscopy can accurately identify slag microcrystals, which are otherwise difficult to distinguish as solely based on their chemical composition and crystal morphology. Therefore, we conclude that it has excellent potential as a slag analysis technique.

• 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.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.25 no.3
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• pp.294-300
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• 2015

Objectives: The aim of this study is to identify physicochemical properties such as chemical composition, size, shape and crystal structure of powder byproducts generated from a metallization process and its 1st scrubber in the semiconductor industry. Methods: Powder samples were collected from inner chambers during maintenance of the W-plug process equipment (using tungsten hexafluoride as a precursor material) and its 1st scrubber. The chemical composition, size and shape of the powder particles were determined by field emission scanning electron microscopy (SEM) and transmission electron microscopy (TEM) equipped with an energy dispersive spectroscope (EDS). The crystal structure of the powders was analyzed by X-ray diffraction (XRD). Results: From the SEM-EDS and TEM-EDS analyses, O and W were mainly detected, which indicates the powder byproducts are tungsten trioxide ($WO_3$), whereas Al, F and Ti were detected as low peaks. The powder particles were spherical and nearly spherical, and the particle size collected from the process equipment and its 1st scrubber showed 10-20 nm (agglomerates: 55-90 nm) and 16-20 nm (agglomerates: 80-120 nm) as primary particles, respectively. The XRD patterns of the yellow powder byproducts exhibit five peaks at $23.8^{\circ}$ $33.9^{\circ}$ $41.74^{\circ}$ $48.86^{\circ}$ and $54.78^{\circ}$ which correspond to the (200), (220), (222), (400), and (420) planes of cubic $WO_3$. Conclusions: We elucidated the physicochemical characteristics of the powder byproducts collected from W-plug process equipment and its 1st scrubber. This study should provide useful information for the development of alternative strategies to improve the working environment and workers' health.

• Tribology and Lubricants
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• v.36 no.4
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• pp.207-214
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• 2020

In this study, we investigated the effects of copper and copper-alloy on the frictional and wear properties of low-steel friction material. The proportions of copper and copper-alloy in the brake friction materials used in passenger cars are very high (approximately 5-20% weight), and these materials have significant effects on friction and wear characteristics. In this study, the effects of cupric ingredients, such as the copper fiber and brass fiber, are investigated using the friction materials based on commercial formulations. After the copper and brass fibers from the same formulation were removed, the frictional and wear characteristics were evaluated to determine the influence of the copper and copper-alloy. We evaluated the frictional and wear characteristics by simulating various braking conditions using a 1/5 scale dynamometer. The results show that the friction material containing copper and brass fibers have excellent frictional stability and a low wear rate compared to the friction material that does not contain copper and brass fibers. These results are attributed to the excellent ductility, moderate melting point, high strength, and excellent thermal conductivity of copper and copper-alloy. We analyzed the surfaces of the friction materials before and after the performing the friction tests using a scanning electron microscope-energy dispersive X-ray spectroscope, confocal microscope, and roughness tester to verify the frictional behavior of copper and copper-alloy. In future studies, it will be applied to the development of copper-free friction materials based on the results of this study.

• Journal of Korean Dental Science
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• v.11 no.2
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• pp.71-81
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• 2018

Purpose: The purpose of this study was to investigate the corrosion behaviors of dental implant alloy after microsized surface modification in electrolytes containing Mn ion. Materials and Methods: $Mn-TiO_2$ coatings were prepared on the Ti-6Al-4V alloy for dental implants using a plasma electrolytic oxidation (PEO) method carried out in electrolytes containing different concentrations of Mn, namely, 0%, 5%, and 20%. Potentiodynamic method was employed to examine the corrosion behaviors, and the alternatingcurrent (AC) impedance behaviors were examined in 0.9% NaCl solution at $36.5^{\circ}C{\pm}1.0^{\circ}C$ using a potentiostat and an electrochemical impedance spectroscope. The potentiodynamic test was performed with a scanning rate of $1.667mV\;s^{-1}$ from -1,500 to 2,000 mV. A frequency range of $10^{-1}$ to $10^5Hz$ was used for the electrochemical impedance spectroscopy (EIS) measurements. The amplitude of the AC signal was 10 mV, and 5 points per decade were used. The morphology and structure of the samples were examined using field-emission scanning electron microscopy and thin-film X-ray diffraction. The elemental analysis was performed using energy-dispersive X-ray spectroscopy. Result: The PEO-treated surface exhibited an irregular pore shape, and the pore size and number of the pores increased with an increase in the Mn concentration. For the PEO-treated surface, a higher corrosion current density ($I_{corr}$) and a lower corrosion potential ($E_{corr}$) was obtained as compared to that of the bulk surface. However, the current density in the passive regions ($I_{pass}$) was found to be more stable for the PEO-treated surface than that of the bulk surface. As the Mn concentration increased, the capacitance values of the outer porous layer and the barrier layer decreased, and the polarization resistance of the barrier layers increased. In the case of the Mn/Ca-P coatings, the corroded surface was found to be covered with corrosion products. Conclusion: It is confirmed that corrosion resistance and polarization resistance of PEO-treated alloy increased as Mn content increased, and PEO-treated surface showed lower current density in the passive region.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.11a
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• pp.145-145
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• 2008

High-k materials have been paid much more attention for their characteristics with high permittivity to reduce the leakage current through the scaled gate oxide. Among the high-k materials, $ZrO_2$ is one of the most attractive ones combing such favorable properties as a high dielectric constant (k= 20 ~ 25), wide band gap (5 ~ 7 eV) as well as a close thermal expansion coefficient with Si that results in good thermal stability of the $ZrO_2$/Si structure. During the etching process, plasma etching has been widely used to define fine-line patterns, selectively remove materials over topography, planarize surfaces, and trip photoresist. About the high-k materials etching, the relation between the etch characteristics of high-k dielectric materials and plasma properties is required to be studied more to match standard processing procedure with low damaged removal process. Among several etching techniques, we chose the inductively coupled plasma (ICP) for high-density plasma, easy control of ion energy and flux, low ownership and simple structure. And the $BCl_3$ was included in the gas due to the effective extraction of oxygen in the form of $BCl_xO_y$ compounds. During the etching process, the wafer surface temperature is an important parameter, until now, there is less study on temperature parameter. In this study, the etch mechanism of $ZrO_2$ thin film was investigated in function of $Cl_2$ addition to $BCl_3$/Ar gas mixture ratio, RF power and DC-bias power based on substrate temperature increased from $10^{\circ}C$ to $80^{\circ}C$. The variations of relative volume densities for the particles were measured with optical emission spectroscopy (OES). The surface imagination was measured by scanning emission spectroscope (SEM). The chemical state of film was investigated using energy dispersive X-ray (EDX).