• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.135-135
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• 2018

천이금속 질화물 코팅은 우수한 기계적 특성들로 인해 공구 코팅으로 많이 사용 되어왔다. 그 중에서도 특히 Cr계 경질 코팅은 높은 경도와 낮은 표면조도, 우수한 마찰특성 등 뛰어난 기계적 특성을 나타내므로 공구 코팅으로의 적용 가능성이 크다. 그러나 최근 공구산업의 발전으로 인해 공구가 더욱 가혹한 환경에서 사용됨에 따라, 공구의 수명을 향상시키고 보호하기 위해 코팅의 높은 밀착력이 요구되고 있으며, 모재와 코팅 사이에 중간층을 합성함으로써 공구의 밀착력을 향상시키는 연구가 활발히 진행되고 있다. 이전 연구에서 모재/중간층/코팅간의 경도와 탄성계수 비율(H/E ratio)의 구배가 코팅의 밀착력에 큰 영향을 미치는 것으로 확인되었다. 그러므로, WC 모재와 Cr계 코팅의 중간값의 H/E ratio를 갖는 중간층의 합성을 통해 코팅의 밀착력을 향상시킬 수 있을 것으로 판단된다. 본 연구에서는, 코팅의 밀착력을 향상시키기 위해 다양한 중간층을 증착한 CrZrN, CrAlN 코팅을 비대칭 마그네트론 스퍼터링 장비를 이용하여 합성하였다. 모재로는 디스크 형상의 WC-6wt.%Co 시편을 사용하였고 Cr, Zr, Si, Al single 타겟을 이용하여 Cr, CrN, CrZrN, CrZrSiN 등의 중간층이 증착된 코팅을 합성했다. 코팅의 합금상, 경도 및 탄성계수, 미세조직 및 조성, 표면 조도을 확인하기 위해 X-ray diffractometer (XRD), Fischer scope, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), atomic force microscopy를 사용하였고, 코팅의 밀착 특성을 분석하기 위해 scratch tester와 optical microscopy (OM)를 이용하였다. 코팅의 내열성을 확인하기 위해 코팅을 furnace에 넣어 공기중에서 500, 600, 700, 800, 900, $1,000^{\circ}C$로 30분 동안 annealing 한 후에 nano-indentation을 사용하여 경도를 측정하였다. CrZrN 및 CrAlN 코팅을 나노 인덴테이션으로 분석한 결과, 모든 코팅의 경도(33.4-35.8 GPa)와 탄성계수(384.1-391.4 GPa)는 중간층의 종류에 상관없이 비슷한 값을 보인 것으로 확인됐다. 그러나, 코팅의 마찰계수는 중간층의 종류에 따라 다른 값을 보였다. CrZrN 코팅의 경우 CrN 합금상 중간층을 갖을 때 가장 낮은 값을 보였으며, CrAlN 코팅의 경우 CrN/CrZrSiN 중간층을 증착하였을때 마찰계수는 0.34로 CrZrN 중간층을 증착하였을 때(0.41)에 비해 낮은 값을 보였다. 또한, 코팅의 마모율 및 마모폭도 비슷한 경향을 보인 것으로 보아, CrN/CrZrSiN 중간층을 합성한 CrAlN 코팅의 내마모성이 상대적으로 우수한 것으로 판단된다. 코팅의 밀착력의 경우도 마찰계수와 비슷한 경향을 보였다. 이것은 중간층의 H/E ratio가 코팅의 내마모성에 미치는 영향에 의한 결과로 사료된다. H/E ratio는 파단시의 최대 탄성 변형율로써, 모재/중간층/코팅의 H/E ratio 구배에 따라 코팅 내의 응력의 완화 정도가 변하게 된다. WC 모재 (H/E=0.040)와 CrAlN 코팅(H/E=0.089) 사이에서 CrN, CrZrSiN 중간층의 H/E ratio는 각각 0.076, 0.083으로 모재/중간층/코팅의 H/E ratio 구배가 점차 증가함을 확인 할 수 있었고, 일정 응력이 지속적으로 가해지면서 진행되는 마모시험중에 CrN과 CrZrSiN 중간층이 WC와 CrAlN 코팅 사이에서 코팅 내부의 응력구배를 완화시키는 역할을 함으로써 CrAlN 코팅의 내마모성이 향상된 것으로 판단된다. 모든 코팅을 열처리 후 경도 분석 결과, CrN/CrZrSiN 중간층을 증착한 CrAlN 코팅은 $1,000^{\circ}C$까지 약 28GPa의 높은 경도를 유지한 것으로 확인 되었고, 이는 CrZrSiN 중간층 내에 존재하는 SiNx 비정질상의 우수한 내산화성에 의한 결과로 판단된다.

• Journal of the korean academy of Pediatric Dentistry
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• v.32 no.2
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• pp.321-331
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• 2005

The purpose of this study was to compare the effectiveness of mechanical and acid treatment on enamel surfaces for the retention of pit and fissure sealants and evaluate the presence of a prismless layer. The etch pattern produced on enamel from immature and mature premolar teeth extracted with varying period of acid etching using 37% phosphoric acid was examined using a scanning electron microscope(SEM). The composition of each groups was evaluated using an energy dispersive x-ray(EDX) spectroscopy. The result of present study can be summarized as follows: 1. Prismless layer was commonly observed on the fissure enamel in young and mature premolar. 2. There were no differences in micro-structure and etching pattern on fissure enamel between the young and the mature premolar. 3. The most effective etching pattern for retention of pit and fissure sealant was observed in 60 seconds of etching time and no apparent difference of etching pattern was found among 15, 30, and 45 seconds of etching time which showed non-retentive etching patterns. 4. The etching pattern obtained by grinding enamel surface with bur followed by 60 seconds of etching was similar to that of 60 seconds of etching without any pretreatment of fissure surface. 5. Type 2 etching pattern was commonly found on fissure enamel in both young and mature premolar. 6. The calcium content and P/Ca ratio in fissure enamel between the young and the mature premolar were significantly different(P<0.05). But content of calcium, phosphate and P/Ca ratio on various regions of fissure enamel in both young and mature premolar did not showed any difference. Based on these results, prismless layer may negatively influence the retention of pit and fissure sealants. Therefore, the mechanical removal of the prismless layer by grinding prior to etching or by prolonged etching time of enamel within the fissure system should result in an improved bonding of a pit and fissure sealant.

• Journal of Conservation Science
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• v.32 no.4
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• pp.579-588
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• 2016

This study analyzed nonmetallic inclusions in iron swords with a ring pommel excavated in the Ipbuk-dong, Suwon. Scanning electron microscopy with energy dispersive spectroscopy(SEM-EDS) was used to estimate the iron-making temperature, and we compared the oxide with $SiO_2$ to investigate the heat-treatment technology in the production of iron swords with a ring pommel by investigating the artificial insertion of a slag former and the metallurgical structure. From the wustite observed in most of the specimens, it is judged that these swords were produced by heating and forging iron smelted at a low temperature using the solid reduction method. In addition, judging from the partial presence of $P_2O_5$, it is assumed that they were smelted directly with natural ore, not calcined. From the ratios of $CaO/SiO_2$ and $TiO_2/SiO_2$, it is judged that the raw material for iron-making was iron ore and that a calcareous slag former was not artificially inserted. The structure of the blade part on the front end was pure iron. From the high carbon content of the blade part on the ring pommel and the formation of a martensitic structure and pearlite colony, it is judged that they were tempered after carburizing and that the back, handle part, and ring pommel were unintentionally carburized. Judging from the structure of these specimens, it was noted that they were produced by applying artificial partial heat-treatment technology. This study attempted to present a more scientific analysis by using the method of interpretation through component analysis of nonmetallic inclusions appearing in one relic by the ratio of the oxide divided by $SiO_2$. It is judged that reinterpreting the arguments by the results of the existing analysis and research in this way can obtain different interpretations.

• Journal of the Mineralogical Society of Korea
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• v.6 no.1
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• pp.1-16
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• 1993

The chemical and optical absorption spectroscopic characters of pink and colorless tourmalines from San Diego mine in California, U.S.A., blue/green tourmalines from anonymous mine, Brazil, and brownis black tourmalines from Uncheon and Haksan mines in Korea have been studied using X-ray diffractometer, electron microprobe, optical absorption spectroscopy, and heat treatment. Least-squares refinements give unit cell diminsions : a = 15.96-16.01 ${\AA}$, c = 7.15-7.16 ${\AA}$ for the brownish black tourmalines, a = 15.82 - 15.87 ${\AA}$, c = 7.09 - 7.10 ${\AA}$ for pink tourmalines, and a = 15.88 - 15.94 ${\AA}$, c = 7.12 - 7.15 ${\AA}$ for blue green tourmalines. The colors of tourmalines are responsible for the transition elements. The pink color is attributed to the $Mn^{3+}$ ions, the blue-green to $Fe^{2+}$ and $Mn^{2+}$, bluish green to $Cu^{2+}$, and the brownish black to $Fe^{2+}$, $Fe^{2+}$ - $Fe^{3+}$, and $Fe^{2+}$ - $Ti^{4+}$. The $Mn^{3+}$ ions of pink color tourmalines are stabilized in the Y sites compressed along the O(1)H-O(3)H axis by Jahn-Teller distortion. Heating removes the pink or red component from tourmalines, producing the colorless stones from the pink and red ones. The bluish green samples change into the greenish blue ones and a certain yellowish green samples change into the light green ones by heat treatment. In the elbaite-schorl series, the concentration of Fe and Mn are variable depending on the color zones. The green zone is characterrized by the high content of Fe and Mn are variable depending on the color zones. The green zone is characterized by the high content of Fe, whereas the pink zone by the high content of Mn. Mn increases in deep yellow zone compared with yellow or colorless zones.

• Journal of the Mineralogical Society of Korea
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• v.22 no.4
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• pp.359-370
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• 2009

Arsenic and heavy metals leached out as a result of oxidation of tailings exposed to the surface pose a serious environmental contamination of mine areas. This study investigated how arsenic behavior is controlled by a variety of processes, such as oxidation of sulfides and formation or alteration of secondary minerals, based on mineralogical methods. The study was carried out using the tailing samples obtained from Nakdong mine located in Jeongseongun, Gangwondo. After separating magnetic and non-magnetic minerals using pretreated tailing samples, each mineral sample was classified according to their colors and metallic lusters observed by the stereoscopic microscope. Subsequently, the mineralogical properties were determined using various instrumental analyses, such as x-ray diffractometer (XRD), energy dispersive spectroscopy (EDS), and electron probe micro analyzer (EPMA). The literature review confirmed that various ore minerals were identified in the Nakdong ore deposits. In this study, however, there were observed a few original ore minerals as well as secondary and/or tertiary minerals newly formed as a result of weathering including oxidation. In particular, we did not recognize pyrrhotite which has been known to originally exist in a large abundance, but peculiarly colloform-type iron (oxy)hydroxides were identified, which indicates most of pyrrhotite has been altered by rapid weathering due to its large reactivity. In addition, a secondary scorodites filling the fissure of weathered primary arsenopyrites were identified, and it is speculated that arsenic is immobilized through such a alteration reaction. Also, we observed tertiary iron (oxy)hydroxides were formed as a result of re-alteration of secondary jarosites, and it suggests that the environment of tailing has been changed to high pH from low pH condition which was initiated and developed by oxidation reactions of diverse primary ore minerals. The environmental change is mainly attributed to interactions between secondary minerals and parental rocks around the mine. As a result, not only was the stability of secondary minerals declined, but tertiary minerals were newly formed. As such a process goes through, arsenic which was immobilized is likely to re-dissolve and disperse into surrounding environments.

• Journal of the Mineralogical Society of Korea
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• v.23 no.2
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• pp.125-139
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• 2010

Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

• Restorative Dentistry and Endodontics
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• v.35 no.2
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• pp.80-87
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• 2010

The purpose of this study was to compare the different canal irrigation methods to prevent the formation of precipitate between sodium hypochlorite (NaOCl) and chlorhexidine (CHX). Extracted 50 human single-rooted teeth were used. The root canals were instrumented using NiTi rotary file (Profile .04/#40) with 2.5% NaOCl and 17% EDTA as irrigants. Teeth were randomly divided into four experimental groups and one control group as follows; Control group: 2.5% NaOCl only, Group 1: 2.5% NaOCl + 2% CHX, Group 2: 2.5% NaOCl + paper points + 2% CHX, Group 3: 2.5% NaOCl + preparation with one large sized-file + 2% CHX, Group 4: 2.5% NaOCl +95% alcohol+ 2% CHX. The teeth were split in bucco-lingual aspect and the specimens were observed using Field Emission Scanning Electron Microscope. The percentages of remaining debris and patent dentinal tubules were determined. Statistical analysis was performed with one-way analysis of variance (ANOVA). Energy Dispersive x-ray Spectroscopy was used for analyzing the occluded materials in dentinal tubule for elementary analysis. There were no significant differences in percentage of remaining debris and patent tubules between all experimental groups at all levels (p > .05). In elementary analysis, the most occluded materials in dentinal tubule were dentin debris. NaOCl/CHX precipitate was detected in one tooth specimen of Group 1. In conclusion, there were no significant precipitate on root canal, but suspected material was detected on Group 1. The irrigation system used in this study could be prevent the precipitate formation.

• Journal of the Korean Vacuum Society
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• v.18 no.4
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• pp.288-295
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• 2009

We report the etch characteristics of GaAs and AlGaAs in the diffusion pump-based capacitively coupled $BCl_3$ plasma. Process variables were chamber pressure ($50{\sim}180$ mTorr), CCP power ($50{\sim}200\;W$) and $BCl_3$ gas flow rate ($2.5{\sim}10$ sccm). Surface profilometry was used for etch rate and surface roughness measurement after etching. Scanning electron microscopy was used to analyze the etched sidewall and surface morphology. Optical emission spectroscopy was used in order to characterize the emission peaks of the $BCl_3$ plasma during etching. We have achieved $0.25{\mu}m$/min of GaAs etch rate with only 5 sccm $BCl_3$ flow rate when the chamber pressure was in the range of 50{\sim}130 mTorr. The etch rates of AlGaAs were a little lower than those of GaAs at the conditions. However, the etch rates of GaAs and AlGaAs decreased significantly when the chamber pressure increased to 180 mTorr. GaAs and AlGaAs were not etched with 50 W CCP power. With $100{\sim}200\;W$ CCP power, etch rates of the materials increased over $0.3{\mu}m$/min. It was found that the etch rates of GaAs and AlGaAs were not always proportional to the increase of CCP power. We also found the interesting result that AlGaAs did not etched at 2.5 sccm $BCl_3$ flow rate at 75 mTorr and 100 W CCP power even though it was etched fast like GaAs with more $BCl_3$ gas flow rates. By contrast, GaAs was etched at ${{\sim}}0.3{\mu}m$/min at the 2.5 sccm $BCl_3$ flow rate condition. A broad molecular peak was noticed in the range of $500{\sim}700\;mm$ wavelength during the $BCl_3$ plasma etching. SEM photos showed that 10 sccm $BCl_3$ plama produced more undercutting on GaAs sidewall than 5 sccm $BCl_3$ plasma.

• Journal of the Korean Electrochemical Society
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• v.24 no.4
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• pp.120-132
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• 2021

Although the development of high-Nickel is being actively carried out to solve the capacity limitation and the high price of raw cobalt due to the limitation of high voltage use of the existing LiCoO₂, the deterioration of the battery characteristics due to the decrease in structural stability and increase of the Ni content. It is an important cause of delaying commercialization. Therefore, in order to increase the high stability of the Ni-rich ternary cathod material LiNi_0.6Co_0.2Mn_0.2O₂, precursor Ni_0.6Co_0.2Mn_0.2-x(OH)₂/xTiO₂ was prepared using a nanosized TiO₂ suspension type source for uniform Ti substitution in the precursor. It was mixed with Li₂CO₃, and after heating, the cathode active material LiNi_0.6Co_0.2Mn_0.2-xTi_xO₂ was synthesized, and the physical properties according to the Ti content were compared. Through FE-SEM and EDS mapping analysis, it was confirmed that a positive electrode active material having a uniform particle size was prepared through Ti-substituted spherical precursor and Particle Size Analyzer and internal density and strength were increased, XRD structure analysis and ICP-MS quantitative analysis confirmed that the capacity was effectively maintained even when the Ti-substituted positive electrode active material was manufactured and charging and discharging were continued at high temperature and high voltage.

• Membrane Journal
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• v.34 no.1
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• pp.50-57
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• 2024

In this experiment, Pd-Ag-Cu membrane was manufactured using electroless plating on an α-Al₂O₃ support. Pd, Ag and Cu were each coated on the surface of the support through electroless plating and heat treatment was performed for 18 h at 500℃ in H₂ in the middle of electroless plating to form Pd alloy. The surface of the Pd-Ag-Cu membrane was observed through Scanning Electron Microscopy (SEM), and the thickness of the Pd membrane was measured to be 7.82 ㎛ and the thickness of the Pd-Ag-Cu membrane was measured to be 3.54 ㎛. Energy dispersive X-ray spectroscopy and X-ray diffraction analysis confirmed the formation of a Pd-Ag-Cu alloy with a composition of Pd-78wt%, Ag-8.81wt% and Cu-13.19wt%. The gas permeation experiment was conducted under the conditions of 350~450℃ and 1~4 bar in H₂ single gas and H₂/N₂ mixed gas. The maximum H₂ flux of the hydrogen separation membrane measured in H₂ single gas is 74.16 ml/cm²·min at 450℃ and 4 bar for the Pd membrane and 113.64 ml/cm²·min at 450℃ and 4 bar for the Pd-Ag-Cu membrane. In the case of the separation factor measured in H₂/N₂ mixed gas, separation factors of 2437 and 11032 were measured at 450℃ and 4 bar.