• Applied Chemistry for Engineering
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• v.28 no.5
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• pp.534-538
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• 2017

In this study, the molecular weight controlled pitches derived from pyrolyzed fuel oil (PFO) were prepared using solvent extraction and were carbonized. Electrochemical characteristics of lithium battery anode materials were investigated using these petroleum pitches. Three pitch samples prepared by the thermal reaction were 3903 (at $390^{\circ}C$ for 3 h), 4001 (at $400^{\circ}C$ for 1 h) and 4002 (at $400^{\circ}C$ for 2 h). The prepared hexane insoluble pitches were analysed by XRD, TGA, SEM and Gel permeation Chromatography (GPC). The electrochemical characteristics of the PFO-derived pitch as an anode material were investigated by constant current charge/discharge, cyclic voltammetry and electrochemical impedance tests. The coin cell using pitch (4001) and the electrolyte of $LiPF_6$ in organic solvents (EC : DMC = 1 : 1 vol%, VC 3 wt%) has better initial capacity (310 mAh/g) than that of other pitch coin cells. Also, this carbon anode showd a high initial efficiency of 82%, retention rate capability at 2 C/0.1 C of 90% and cycle retention of 85%. It was found that modified pitches improved the cycling and rate capacity performance.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.99-99
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• 2016

최근 공구산업은 산업 발전으로 공구의 사용 환경이 가혹화 되고, 첨단산업용 특수합금들이 발달하면서 이를 가공할 수 있는 새로운 절삭공구소재들이 개발되어지고 있다. 또한 고성능 절삭공구는 공구소재보다 코팅개발이 상대적으로 더욱 효과적이기 때문에 코팅 기술 개발이 활발히 진행되고 있다. 최근 일본에서는 새로운 코팅층 물질 개발보다는 기존의 코팅물질을 조합하거나 개량하여 성능을 향상시키는 추세이며, 이는 현재 공구산업의 효율적인 개발방향을 제시하고 있다. 기존의 빗각 증착은 기판의 각도를 변경하여 증기가 기판에 비스듬하게 입사하도록 조절하여 코팅하는 기술로 박막의 조직을 다양하게 제어하는 것이 가능하며, 구조 제어를 통한 완전화 박막을 이용한 one-batch 다기능 구현을 위하여 많은 연구가 진행되고 있다. 가공이 까다로운 소재를 가공하기 위한 공구에 적용하기 위해서 Al의 함량이 높은 AlTiN 소재가 개발되어 적용되고 있으며, 이 소재는 공구의 수명향상을 위한 표면처리 소재로 각광을 받고 있다. 본 연구에서는 음극아크 증착 시 거대입자가 박막에 증착되어 결함을 만들기 때문에 그 밀도를 낮추기 위해서 음극 아크 증착을 이용하여 공정 변화에 따른 AlTiN 박막의 표면형상을 관찰하고 특성을 평가하였다. 또한 빗각 증착을 적용하여 제작한 AlTiN 박막의 특성을 평가하였다. 고 함량의 AlTi합금 타겟을 음극 아크 소스에 장착하여 AlTiN 박막을 코팅하였다. 시편은 스테인리스강판(SUS304)과 초경(tungsten carbide; WC)을 사용하였다. 음극 아크 소스에 인가되는 전류가 낮을수록 AlTiN 박막 표면에 거대입자의 밀도가 낮아졌으며, 기판 전압과 공정압력이 높을수록 AlTiN 박막의 표면에 존재하는 거대입자의 밀도가 낮아지는 경향을 보였다. 이를 통하여 거대입자밀도를 낮추는 기초공정을 도출하였다. AlTiN 박막 제작 시 빗각을 적용한 결과 $60^{\circ}$의 빗각을 적용한 다층 박막에서 상대적으로 가장 높은 경도 값을 보였다. 본 연구를 통해 음극 아크 증착을 이용하여 거대입자의 밀도가 낮은 박막을 제작할 수 있는 공정을 도출하였고, 빗각증착을 적용하면 경도가 향상되는 결과를 확인하였다.

• Applied Chemistry for Engineering
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• v.31 no.5
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• pp.514-519
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• 2020

Graphite materials for lithium ion battery anode materials are the most commercially available due to their structural stability and low price. Recently, research efforts have been conducted on carbon coatings by improving side reactions at the edge site of carbon materials. The carbon coating process has classified into a CVD by chemical reaction, wet coating process with solvent and dry coating by mechanical impact. In this paper, the rapid crush/coating process was used to solve the problem of which only few parts of the carbon precursor (pitch) can be used and also environmental problems caused by solvent removal in the wet coating process. When the ratio of needle coke to pitch was 8 : 2 wt%, and the rapid crush/coating process was carried out, it was confirmed that the fracture surface was coated by pitch. The pitch-coated sample was treated at 2400 ℃ and 41.8% improvement in 10C/0.1C rate characteristic was observed. It is considered that the material simply manufactured through the simple crush/coating process can be used as an anode electrode material for a lithium ion battery.

• Korean Chemical Engineering Research
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• v.59 no.3
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• pp.326-332
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• 2021

In this study, a spherical carbon composite material containing nano-silicon was synthesized using hydrothermal synthesis, and coated with petroleum pitch to prepare an anode material to investigate the electrochemical characteristics. Hydrothermal synthesis was performed by varying molar concentration, and the pitch was coated using THF as an organic solvent to prepare a composite material. The physical properties of anode materials were analyzed using SEM, EDS, XRD and TGA, and the electrochemical performances were investigated by cycle, C-rate, cyclic voltammetry and electrochemical impedance tests in 1.0 M LiPF₆ electrolyte (EC : DMC : EMC = 1 : 1 : 1 vol%). The pitch-coated silicon/carbon composite (Pitch@Si/C-1.5) with sucrose of 1.5 M showed a spherical shape. In addition, a high initial capacity of 1756 mAh/g, a capacity retention ratio of 82% after 50 cycles, and an excellent rate characteristic of 81% at 2 C/0.1 C were confirmed.

• Korean Chemical Engineering Research
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• v.62 no.3
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• pp.262-268
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• 2024

In this study, the MXene/Si composite was prepared by electrostacic assembly with 2-dimensional structured titanium carbide (MXene) and nano silicon for anode material of high-performance lithium-ion battery. Ti₃C₂T_x MXene was synthesized by etching the Ti₃AlC₂ MAX with LiF/HCl, and the surface of nano silicon was charged to positively using CTAB (Cetyltrimethylammonium bromide). The MXene/Si anode composite was successfully manufactured by simple mixing process of synthesized MXene and charged silicon. The physical and electrochemical properties of prepared composite were investigated with MXene-silicon composition ratio, and the surface of electrode after cycles was analyzed to evaluate stability of the electrode. The MXene/Si composites demonstrated high initial discharge capacities of 1962.9, 2395.2 and 2504.3 mAh/g as the silicon composition ratio increased to 2, 3 and 4 compared to MXene, respectively. MXene/Si-4, which is MXene and silicon ratio with 1 : 4, exhibited 1387.5 mAh/g of reversible capacity, 74.5% of capacity retention at 100 cycles and high capacity of 700.5 mAh/g at high rate of 4.0 C. As the results, the MXene/Si composite prepared by electrostatic-assenbly could be applied to anode materials for high-performance LIBs.

• Clean Technology
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• v.24 no.4
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• pp.332-338
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• 2018

Currently graphite is used as an anode active material for lithium ion battery. However, since the maximum theoretical capacity of graphite is limited to $372mA\;h\;g^{-1}$, a new anode active material is required for the development of next generation high capacity and high energy density lithium ion battery. The maximum theoretical capacity of Si is $4200mA\;h\;g^{-1}$, which is about 10 times higher than the maximum theoretical capacity of graphite. However, since the volume expansion rate is almost 400%, the irreversible capacity increases as the cycle progresses and the discharge capacity relative to the charge is remarkably reduced. In order to solve these problems, it is possible to control the particle size of the Si anode active material to reduce the mechanical stress and the volume change of the reaction phase, thereby improving the cycle characteristics. Therefore, in order to minimize the decrease of the charge / discharge capacity according to the volume expansion rate of the Si particles, the improvement of the cycle characteristics was carried out by pulverizing Si by a dry method with excellent processing time and cost. In this paper, Si is controlled to nano size using vibrating mill and the physicochemical and electrochemical characteristics of the material are measured according to experimental variables.

• Journal of the Korean Electrochemical Society
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• v.12 no.2
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• pp.162-166
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• 2009

The carbon-coated Si/Cu powders were synthesized by mechanical ball-milling and hydrocarbon gas decomposition methods at high temperature. The carbon-coated Si/Cu powder was used as anode for lithium secondary battery and its electrochemical behavior was investigated. In addition, the carbon-coated Si/Cu/graphite composite anode material was prepared using natural graphite powder and their electrochemical characteristics were compared with natural graphite anode. The specific capacity of carbon-coated Si/Cu anode increased to the initial 10 cycles. The carbon-coated Si/Cu/graphite composite anode exhibited the reversible specific capacity of 450mAh/g and the first cycle efficiency of 81.3% at $0.25mA/cm^2$. The cycling performance of the composite anode was similar to that of pure graphite anode except the reversible specific capacity value.

• Korean Chemical Engineering Research
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• v.57 no.1
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• pp.118-123
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• 2019

In this study, the electrochemical characteristics of Graphite/Silicon/Pitch anode composites were analyzed to improve the low theoretical capacity of graphite as a lithium ion battery. The Graphite/Silica composites were synthesized by bonding silica onto polyvinylpyrrolidone coated graphite. The surface of used silica was treated with (3-Aminopropyl)triethoxysilane(APTES). Graphite/Silicon/Pitch composites were prepared by carbonization of petroleum pitch, the fabrication processes including the magnesiothermic reduction of nano silica to obtain silicon and varying the mass ratio of silica. The Graphite/Silicon/Pitch composites were analysed by XRD, SEM and XRD. Also the electrochemical performances of Graphite/Silicon/Pitch composite as the anode of lithium ion battery were investigated by constant current charge/discharge, rate performance, cyclic voltammetry and electrochemical impedance tests in the electrolyte of $LiPF_6$ dissolved in organic solvents (EC:DMC:EMC=1:1:1 vol%). The Graphite/Silicon/Pitch anode composite (silica 28.5 in weight) has better capacity (537 mAh/g). The cycle performance has an excellent capacity retention to 30th cycle of 95% and the retention rate capability of 98% in 0.1 C/0.2 C.

• Composites Research
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• v.35 no.6
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• pp.365-370
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• 2022

According to the rapid growth of electric vehicle (EVs) and E-mobility market, Li-ion batteries are one of the most progressive technologies. The demand of LIBs with high energy capacity, rate performance and fast charging is continuously increasing, hence high-performance LIBs should be developed. Si is considered as the most promising anode material to improve energy density because of its high theoretical capacity. However, Si suffers large volume chances during the charging and discharge process, leading to the fast degradation of cycle performance. Therefore, polymeric binders play a key role in electrochemical performance of Si anode by efficiently enduring the Si expansion and maintaining the binding networks in electrode. In this review, we explain the role of polymeric binders in electrode and introduce the anode binders with enhanced mechanical and chemical properties which can improve electrochemical performances of Si-based anode.

• 한국전기화학회:학술대회논문집
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• 2003.07a
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• pp.117-122
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• 2003