• Analytical Science and Technology
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• v.6 no.3
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• pp.275-282
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• 1993

A direct and simultaneous method to determine the $SiO_2$ and $ZrO_2$ in zircon sand of raw mineral and its treated one were studied by optical emission spectrometer using DC arc source. The synthetic standard was prepared by mixing with pure metal oxide, and it was diluted with buffer(graphite) and flux($Li_2B_4O_7$). The mixing ratio of buffer and flux and its dilution ratio to sample was investigated in order to choose the best excitation conditions. The optimum mixing and dilution ratios were 0.22:1 and 40, and the standard deviations of analytical results were 1.9% for $SiO_2$ and 4.7% for $ZrO_2$.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.10a
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• pp.16.2-16.2
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• 2011

Graphene has attracted significant attention due to its unique characteristics and promising nanoelectronic device applications. For practical device applications, it is essential to synthesize high-quality and large-area graphene films. Graphene has been synthesized by eloborated mechanical exfoliation of highly oriented pyrolytic graphite, chemical reduction of exfoliated grahene oxide, thermal decomposition of silicon carbide, and chemical vapor deposition (CVD) on metal substrates such as Ni, Cu, Ru etc. The CVD has advantages over some of other methods in terms of mass production on large-areas substrates and it can be easily separated from the metal substrate and transferred to other desired substrates. Especially, plasma-enhanced CVD (PECVD) can be very efficient to synthesize high-quality graphene. Little information is available on the synthesis of graphene by PECVD even though PECVD has been demonstrated to be successful in synthesizing various carbon nanostructures such as carbon nanotubes and nanosheets. In this study, we synthesized graphene on $Ni/SiO_2/Si$ and Cu plate substrates with CH4 diluted in $Ar/H_2$ (10%) by using an inductively-coupled PECVD (ICPCVD). High-quality graphene was synthesized at as low as $700^{\circ}C$ with 600 W of plasma power while graphene layer was not formed without plasma. The growth rate of graphene was so fast that graphene films fully covered on substrate surface just for few seconds $CH_4$ gas supply. The transferred graphene films on glass substrates has a transmittance at 550 nm is higher 94%, indicating 1~3 monolayers of graphene were formed. FETs based on the grapheme films transferred to $Si/SiO_2$ substrates revealed a p-type. We will further discuss the synthesis of graphene and doped graphene by ICPVCD and their characteristics.

• Journal of the Korean Electrochemical Society
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• v.12 no.1
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• pp.34-39
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• 2009

In this study, a needle coke was oxidized in a mixture of dilute nitric acid and sodium chlorate ($NaClO_3$) solutions and followed by heat treatment. The samples were analyzed with using XRD, FESEM, elemental analyzer, BET, and Raman spectroscopy. Double layer capacitance was measured with the charge and discharge measurements. The consisting layers of the needle coke were expanded to single phase showing only (001) diffraction peak by the acid treatment for 24 hours. The oxidized coke returned to a graphite structure appearing (002) peak after heat treatment above $200^{\circ}C$. The structure returned could be more easily accessible to the ions by the first charge, and improve the double layer capacitance at the second charge. The two-electorde cell from acid treated coke and $300^{\circ}C$ heat treatment exhibited the maximum capacitances of 32.1 F/g and 29.5 F/ml at the potential of $0{\sim}2.5\;V$.

• Proceedings of the Materials Research Society of Korea Conference
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• 2012.05a
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• pp.80.2-80.2
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• 2012

그라핀(graphene)은 탄소 원자의 2차원 육각형 $sp^2$ 결합체로서 탄소 나노구조체가 가지는 여러 가지 우수한 특성을 보유하면서 대면적 기판 위에서 소자구현 및 투명전극 등으로의 우수한 응용성 때문에 고품질 그라핀 제조와 물리적 특성, 소자응용에 관한 연구가 활발히 진행되고 있다. 최근 그라핀 제조를 위한 여러 가지 방법이 개발되고 있으나 화학적 박리법이 저비용으로 대량생산을 위해 가장 유리한 방법으로 주목을 받고 있다. 화학적 박리법은 벌크 그라파이트를 강한 산을 이용하여 산화시켜 형성된 산화 그라파이트(graphite oxide)을 열적으로 팽창시켜 박리하고 환원하여 그라핀으로 제조하는 것이다. 보통 열적팽창을 위해서 열처리 로를 사용하게 되는데, 본 연구에서는 박리를 보다 효율적으로 진행시키고 고품질의 그라핀을 얻기 위해 마이크로웨이브를 이용한 박리법을 적용하였다. 마이크로웨이브는 설비가 간단하고 매우 균일하게 열팽창을 시킬 수 있을 뿐만 아니라 대량생산에서도 유리할 것으로 기대하였다. 천연 그라파이트(99.9%, 평균입도 $200{\mu}m$)를 Hummer 방법에 따라 $H_2SO_4$와 $KMnO_4$를 사용하여 산화시키고 필터링 후 마이크로웨이브를 조사하였다. 이후 환원 처리를 거쳐 그라핀을 제조하였다. 라만스펙트럼 및 투과전자현미경으로 분석한 결과 우수한 품질의 그라핀이 형성되었음을 알 수 있었다. 그라핀의 두께 및 품질은 마이크로웨이브의 인가시간 및 반복 횟수가 증가함에 따라 크게 영향받는 것을 확인하였다. 본 발표에서는 마이크로웨이브를 사용한 산화 그라파이트 박리 및 그라핀 제조라는 새로운 시도와 주요변수에 따른 그라핀 특성에 관한 결과를 논의할 것이다.

• Korean Journal of Materials Research
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• v.23 no.2
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• pp.123-127
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• 2013

The electrolytic reduction of a spent oxide fuel involves liberation of the oxygen in a molten LiCl electrolyte, which is a chemically aggressive environment that is too crosive for typical structural materials. Therefore, it is essential to choose the optimum material for the process equipment for handling a molten salt. In this study, the corrosion behavior of pyro-carbon made by CVD was investigated in a molten LiCl-$Li_2O$ salt under an oxidation atmosphere at $650^{\circ}C$ and $750^{\circ}C$ for 72 hours. Pyro-carbon showed no chemical reactions with the molten salt because of its low wettability between pyro-carbon and the molten salt. As a result of XRD analysis, pyro-carbon exposed to the molten salt showed pure graphite after corrosion tests. As a result of TGA, whereas the coated layer by CVD showed high anti-oxidation, the non-coated layer showed relatively low anti-oxidation. The stable phases in the reactions were $C_{(S)}$, $Li_2CO_{3(S)}$, $LiCl_{(l)}$, $Li_2O$ at $650^{\circ}C$ and $C_{(S)}$, $LiCl_{(l)}$, $Li_2O_{(S)}$ at $750^{\circ}C$. $Li_2CO_{(S)}$ was decomposed at $750^{\circ}C$ into $Li_2O_{(S)}$ and $CO_{2(g)}$.

• Korean Journal of Materials Research
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• v.30 no.11
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• pp.581-588
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• 2020

Reducing CO₂ into high value fuels and chemicals is considered a great challenge in the 21st century. Efficiently activating CO₂ will lead to an important way to utilize it as a resource. This article reviews the latest progress of g-C₃N₄ based catalysts for CO₂ reduction. The different synthetic methods of g-C₃N₄ are briefly discussed. Article mainly introduces methods of g-C₃N₄ shape control, element doping, and use of oxide compounds to modify g-C₃N₄. Modified g-C₃N₄ has more reactive sites, which can significantly reduce the probability of photogenerated electron hole recombination and improve the performance of photocatalytic CO₂ reduction. Considering the literature, the hydrothermal method is widely used because of its simple equipment and process and easy control of reaction conditions. It is foreseeable that hydrothermal technology will continue to innovate and usher in a new period of development. Finally, the prospect of a future reduction of CO₂ by g-C₃N₄-based catalysts is predicted.

• Ceramist
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• v.21 no.4
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• pp.388-405
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• 2018

In this paper, we review about current development of electrode materials for Li-ion batteries and catalysts for fuel cells. We scrutinized various electrode materials for cathode and anode in Li-ion batteries, which include the materials currently being used in the industry and candidates with high energy density. While layered, spinel, olivine, and rock-salt type inorganic electrode materials were introduced as the cathode materials, the Li metal, graphite, Li-alloying metal, and oxide compound have been discussed for the application to the anode materials. In the development of fuel cell catalysts, the catalyst structures classified according to the catalyst composition and surface structure, such as Pt-based metal nanoparticles, non-Pt catalysts, and carbon-based materials, were discussed in detail. Moreover, various support materials used to maximize the active surface area of fuel cell catalysts were explained. New electrode materials and catalysts with both high electrochemical performance and stability can be developed based on the thorough understanding of earlier studied electrode materials and catalysts.

• Journal of the Korean institute of surface engineering
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• v.56 no.1
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• pp.62-68
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• 2023

Silicon (Si) is considered as a promising substitute for the conventional graphite due to its high theoretical specific capacity (3579 mAh/g, Li₁₅Si₄) and proper working voltage (~0.3V vs Li⁺/Li). However, the large volume change of Si during (de)lithiation brings about severe degradation of battery performances, rendering it difficult to be applied in the practical battery directly. As a one feasible candidate of industrial Si anode, silicon monoxide (SiO_x) demonstrates great electrochemical stability with its specialized strategy, downsized Si nanocrystallites surrounded by Li⁺ inactive buffer phase (Li₂O and Li₄SiO₄). Nevertheless, SiO_x inherently has the initial irreversible capacity and poor electrical conductivity. To overcome those issues, conformal carbon coating has been performed on SiO_x utilizing ethylbenzene as the carbon precursor of chemical vapor deposition (CVD). Through various characterizations, it is confirmed that the carbon is homogeneously coated on the surface of SiO_x. Accordingly, the carbon-coated SiOx from CVD using ethylbenzene demonstrates 73% of the first cycle efficiency and great cycle life (88.1% capacity retention at 50th cycle). This work provides a promising synthetic route of the uniform and scalable carbon coating on Si anode for high-energy density.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.08a
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• pp.351-352
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• 2011

그래핀(Graphene)은 2차원 평면구조의 $sp^2$ 탄소 결합으로 이루어진 물질이다. 일반적으로 그래핀은 탄소 원자 한층 정도의 얇은 두께를 가지면서 강철의 100배 이상 높은 강도, 다이아몬드보다 2배 이상 뛰어난 열 전도성, 그리고 규소보다 100배 이상 빠른 전자이동도 등의 매우 우수한 특성을 지닌다. 그래핀을 합성하거나 얻는 방법에는, 기계적 박리법(Micro mechanical exfoliation), 산화흑연(graphite oxide)을 이용한 reduced graphene oxide(RGO)방법과 탄화 규소(SiC)를 이용한 epitaxial growth 방법 등이 있지만, 대 면적화가 어렵거나 구조적 결함이 큰 문제점이 있다. 반면, 탄화수소(hydrocarbon)를 탄소 공급원으로 하는 열화학 기상 증착법(Thermal chemical vapor deposition, TCVD)은 구조적 결함이 상대적으로 적으면서 대 면적화가 가능하다는 이점 때문에 최근 가장 많이 이용되고 있는 방법이다. TCVD를 이용, 니켈, 몰리브덴, 금, 코발트 등의 금속에서 그래핀 합성연구가 보고되었지만, 대부분 수 층(fewlayer)의 그래핀이 합성되었다. 하지만, 구리 촉매를 이용하는 것이 단층 그래핀 합성에 매우 효율적이라는 연구결과가 보고되었다. 구리의 경우, 낮은 탄소융해도(solubility of carbon) 때문에 표면에서 self limiting 과정을 통하여 단층 그래핀이 합성된다. 그러나 단층 그래핀 일지라도 면저항(sheet resistance)이 매우 높고, 이론적 계산값에 비해 전자이동도(electron mobility)가 낮게 측정된다. 이러한 원인은 구조적 결함에서 기인된 것으로써 산업으로의 응용을 어렵게 만들기 때문에 양질의 단층 그래핀 합성연구는 필수적이다[1,2]. 본 연구에서는 TCVD를 이용하여 구리 포일(25 ${\mu}m$, Alfa Aeser) 위에 메탄가스를 탄소공급원으로 하여 수소를 함께 주입하고, 메탄가스의 양과 합성시간, 열처리 시간을 조절하면서 균일한 단층 그래핀을 합성하였다. 합성된 그래핀을 $SiO_2$ (300 nm)기판위에 전사(transfer)후 라만 분광법(raman spectroscopy)과 광학 현미경(optical microscope)을 통하여 분석하였다. 그 결과, 열처리 시간이 증가할수록 촉매로 사용된 구리 포일의 grain size가 커짐을 확인하였으며, 구리 포일 위에 합성된 그래핀의 grain size는, 구리 포일의 grain size에 의존하여 커짐을 확인하였다. 또한 동일한 grain 내의 그래핀은 균일한 층으로 합성되었다. 이는 기계적 박리법, RGO 방법, epitaxial growth 방법으로 얻은 그래핀과 비교하여 매우 뛰어난 결정성을 지님이 확인되었다. 본 연구를 통하여 면적이 넓으면서도 결정성이 매우 뛰어난 양질의 단층 그래핀 합성 방법을 확립하였다.

• Applied Chemistry for Engineering
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• v.18 no.5
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• pp.522-526
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• 2007

Structural features and electrochemical performances of cokes pyrolized from oxidized cokes were examined, and compared with KOH-activated coke. Needle cokes ($d_{002}=3.5{\AA} $), having a graphene layer structure, were changed to a single phase of graphite oxide after oxidation treatment with an acidic solution having an $NaCLO_3$/needle coke composition ratio of above 7.5, and the inter-layer distance of the oxidized coke was expanded to $6.9{\AA} $ with increasing oxygen content. After heating at $200^{\circ}C$, the oxidized coke was pyrolized to the graphene layer structure with inter-layer distance of $3.6{\AA} $. However, the change of the inter-layer distance of the needle coke was not observed in the KOH activation process. On the other hand, an intercalation of electrolyte ions into the pyrolized coke, observed at first charge, occurred at 1.0 V, in which the value was lower than that of KOH-activation coke. The cell capacitor using pyrolized coke exhibited a lower internal resistance of $0.57{\Omega}$ in 1 kHz, and a larger capacitance per weight and volume of 30.3 F/g and 26.9 F/ml at the two-electrode system in the potential range 0~2.5 V than those of the cell capacitor using KOH-activation of coke. This better electrochemical performance may be associated with structure defects in the graphene layer derived from the process of the inter-layer expansion and shrinkage.