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불활성 가스의 O<sub>2</sub>와 CO 불순물 제거를 위한 Ni 촉매의 물성 평가
김광배,진새라,김은석,임예솔,이현준,김성훈,노윤영,송오성,Kim, Kwangbae,Jin, Saera,Kim, Eunseok,Lim, Yesol,Lee, Hyunjun,Kim, Seonghoon,Noh, Yunyoung,Song, Ohsung 한국산학기술학회 2020 한국산학기술학회논문지 Vol.21 No.4
반도체 산업용 9N 이상의 초고순도 N<sub>2</sub>, Ar 등 불활성 가스 제조를 위해 가스 정제공정에 사용되고 있는 Ni 촉매의 물성 평가 및 촉매적 특성을 확인하였다. 조성이 다른 원기둥 형태의 C1, 츄러스 형태의 C2의 두 가지 Ni 촉매에 대해 비교 평가를 진행하였다. Ni 촉매의 형상과 미세구조를 분석하기 위해 광학현미경과 FE-SEM을 이용하였으며, 조성 확인 및 물성을 분석하기 위해 EDS, XRD, 그리고 micro-Raman 분석을 이용하였다. 또한 Ni 촉매의 비표면적 및 촉매적 특성을 확인하기 위해 BET, Pulse Titration 분석을 진행하였다. 조성 분석결과, C1의 경우, 상대적으로 graphite가 불순물로 다량 포함되어 있는 것을 확인하였으며, C2는 C1에 비해 Ni의 함량이 높은 것을 확인하였다. 비표면적 분석 결과, C2의 비표면적이 C1보다 약 1.69배 정도 큰 것을 확인할 수 있었다. 촉매적 특성분석 결과, 상온에서 O<sub>2</sub>와 CO 불순물 제거 정도가 C2가 우수함을 확인하였다. 따라서 반도체 산업용 초고순도 불활성 기체 제조를 위한 Ni 촉매로는 불순물이 적고, 비표면적이 크며, 상온에서 O<sub>2</sub>와 CO 제거 성능이 우수한 C2가 적합함을 확인하였다. This study examined the catalytic property of Ni-catalyst used in the gas purifying process to manufacture inert gases of N2 and Ar with high-purity over 9N for semiconductor industrial applications. Two types of Ni-catalysts with a cylindrical shape (C1) and churros shape structure (C2) were compared for the assessment. Optical microscopy and FESEM were used to analyze the shape and microstructure of the Ni-catalyst. EDS, XRD, and micro-Raman characterization were performed to examine the composition and properties. BET and Pulse Titration analyses were conducted to check the surface area and catalytic property of the Ni-catalyst. From the composition analysis results, C1 contained a relatively large amount of graphite as an impurity, and C2 contained higher Ni contents than C1. From specific surface area analysis, the specific surface area of C2 was approximately 1.69 times larger than that of C1. From catalytic property analysis, outstanding performance in O<sub>2</sub> and CO impurity removal was observed at room temperature. Therefore, C2, having low-impurity and large specific surface area, is a suitable catalyst for the high-purity inert gas process in the semiconductor industry because of its outstanding performance in O<sub>2</sub> and CO impurity removal at room temperature.
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질소 5N 가스 분위기에서 다공질 ZrFe 합금의 산화 안정화
김광배,진새라,임예솔,이현준,김성훈,노윤영,송오성 대한금속·재료학회 2021 대한금속·재료학회지 Vol.59 No.10
A porous ZrFe alloy specimen was prepared as a 6 × 3 mm (diameter × thickness) disk. The reaction of the ZrFe alloy was confirmed while the whole system was maintained at a target temperature, which was increased from 150 oC to 950 oC in a 99.999% low purity nitrogen atmosphere, consisting of 10 ppm of impurity gas. Surface color, pore size, stabilized layer, and phase change were confirmed with optical microscopy, scanning electron microscopy-energy dispersive X-ray spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and Micro-Raman, according to temperature. The surface color of the ZrFe alloy changed from metallic silver to dark gray as the temperature increased. In the EDS and XPS results, nitrogen component was not observed, and oxygen content increased on each surface at the elevated temperatures. In this way, the ZrFe alloy was stabilized in a low purity nitrogen atmosphere, preventing rapid nitride reactions.
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불활성 가스의 O₂와 CO 불순물 제거를 위한 Ni 촉매의 물성 평가
김광배(Kwangbae Kim),진새라(Saera Jin),김은석(Eunseok Kim),임예솔(Yesol Lim),이현준(Hyunjun Lee),김성훈(Seonghoon Kim),노윤영(Yunyoung Noh),송오성(Ohsung Song) 한국산학기술학회 2020 한국산학기술학회논문지 Vol.21 No.4
반도체 산업용 9N 이상의 초고순도 N₂, Ar 등 불활성 가스 제조를 위해 가스 정제공정에 사용되고 있는 Ni 촉매의 물성 평가 및 촉매적 특성을 확인하였다. 조성이 다른 원기둥 형태의 C1, 츄러스 형태의 C2의 두 가지 Ni 촉매에 대해 비교 평가를 진행하였다. Ni 촉매의 형상과 미세구조를 분석하기 위해 광학현미경과 FE-SEM을 이용하였으며, 조성 확인 및 물성을 분석하기 위해 EDS, XRD, 그리고 micro-Raman 분석을 이용하였다. 또한 Ni 촉매의 비표면적 및 촉매적 특성을 확인하기 위해 BET, Pulse Titration 분석을 진행하였다. 조성 분석결과, C1의 경우, 상대적으로 graphite가 불순물로 다량 포함되어 있는 것을 확인하였으며, C2는 C1에 비해 Ni의 함량이 높은 것을 확인하였다. 비표면적 분석 결과, C2의 비표면적이 C1보다 약 1.69배 정도 큰 것을 확인할 수 있었다. 촉매적 특성분석 결과, 상온에서 O₂와 CO 불순물 제거 정도가 C2가 우수함을 확인하였다. 따라서 반도체 산업용 초고순도 불활성 기체 제조를 위한 Ni 촉매로는 불순물이 적고, 비표면적이 크며, 상온에서 O₂와 CO 제거 성능이 우수한 C2가 적합함을 확인하였다. This study examined the catalytic property of Ni-catalyst used in the gas purifying process to manufacture inert gases of N2 and Ar with high-purity over 9N for semiconductor industrial applications. Two types of Ni-catalysts with a cylindrical shape (C1) and churros shape structure (C2) were compared for the assessment. Optical microscopy and FESEM were used to analyze the shape and microstructure of the Ni-catalyst. EDS, XRD, and micro-Raman characterization were performed to examine the composition and properties. BET and Pulse Titration analyses were conducted to check the surface area and catalytic property of the Ni-catalyst. From the composition analysis results, C1 contained a relatively large amount of graphite as an impurity, and C2 contained higher Ni contents than C1. From specific surface area analysis, the specific surface area of C2 was approximately 1.69 times larger than that of C1. From catalytic property analysis, outstanding performance in O₂ and CO impurity removal was observed at room temperature. Therefore, C2, having low-impurity and large specific surface area, is a suitable catalyst for the high-purity inert gas process in the semiconductor industry because of its outstanding performance in O₂ and CO impurity removal at room temperature.
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김광배,임예솔,김은석,진새라,이현준,김성훈,노윤영,송오성 대한금속·재료학회 2020 대한금속·재료학회지 Vol.58 No.7
The properties and H2O adsorption characteristics of two types of zeolites (3A and 13X) with the same shape but different element composition were identified. These zeolites are used in gas purification processes to manufacture 9N ultra-pure inert gases for semiconductor process applications. To analyze the shape and microstructure of the zeolites, an optical microscope and FE-SEM were used. EDS, micro-Raman, and XRD analysis were conducted to analyze their compositions and properties. BET analysis was performed to identify their specific surface areas. Finally, a breakthrough analysis was conducted at room temperature. Based on the results of the optical and microstructure analyses, the cylindrical shaped 3A and 13X were determined to be composed of 2.5-um polyhedrons and 1.4-um massive shapes, respectively. The results of the compositional analysis showed that the main components of both zeolites were Si and Al, whereas K and Na existed in 3A and 13X, respectively. The results of the specific surface area analysis demonstrated that the surface area of 13X was 32 times larger than that of 3A. Specifically, the total specific surface areas were 22.42 and 720.33 m2/g for 3A and 13X, respectively. The results of the H2O adsorption characteristic analysis showed that the H2O concentration of 13X was 1.33 times higher than that of 3A. Therefore, with respect to using zeolite for gas purification process applications, 13X might be more suitable to achieve excellent specific surface area and remarkable H2O adsorption.
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