• 한국재료학회지
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• 제24권5호
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• pp.243-248
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• 2014

Silicon-carbon composite was prepared by the magnesiothermic reduction of mesoporous silica and subsequent impregnation with a carbon precursor. This was applied for use as an anode material for high-performance lithium-ion batteries. Well-ordered mesoporous silica(SBA-15) was employed as a starting material for the mesoporous silicon, and sucrose was used as a carbon source. It was found that complete removal of by-products ($Mg_2Si$ and $Mg_2SiO_4$) formed by side reactions of silica and magnesium during the magnesiothermic reduction, was a crucial factor for successful formation of mesoporous silicon. Successful formation of the silicon-carbon composite was well confirmed by appropriate characterization tools (e.g., $N_2$ adsorption-desorption, small-angle X-ray scattering, X-ray diffraction, and thermogravimetric analyses). A lithium-ion battery was fabricated using the prepared silicon-carbon composite as the anode, and lithium foil as the counter-electrode. Electrochemical analysis revealed that the silicon-carbon composite showed better cycling stability than graphite, when used as the anode in the lithium-ion battery. This improvement could be due to the fact that carbon efficiently suppressed the change in volume of the silicon material caused by the charge-discharge cycle. This indicates that silicon-carbon composite, prepared via the magnesiothermic reduction and impregnation methods, could be an efficient anode material for lithium ion batteries.

• Bulletin of the Korean Chemical Society
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• 제29권10호
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• pp.1965-1968
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• 2008

The effects of carbon-coated silicon/graphite (Si/Gr.) composite anode on the electrochemical properties were investigated. The nanosized silicon particle shows a good cycling performance with a reasonable value of the first reversible capacity as compared with microsized silicon particle. The carbon-coated silicon/graphite composite powders have been prepared by pyrolysis method under argon/10 wt% propylene gas flow at $700{^{\circ}C}$ for 7 h. Transmission electron microscopy (TEM) analysis indicates that the carbon layer thickness of 5 nm was coated uniformly onto the surface silicon powder. It is confirmed that the insertion of lithium ions change the crystalline silicon phase into the amorphous phase by X-ray diffraction (XRD) analysis. The carbon-coated composite silicon/graphite anode shows excellent cycling performance with a reversible value of 700 mAh/g. The superior electrochemical characteristics are attributed to the enhanced electronic conductivity and low volume change of silicon powder during cycling by carbon coating.

• Journal of Electrochemical Science and Technology
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• 제2권2호
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• pp.116-123
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• 2011

Herein, a novel preparation method of highly homogeneous carbon-silicon composite materials was presented. In contrast to conventional solvent evaporation method, a milled silicon-graphite or its oxidized material were directly reacted with petroleum-derived pitch precursor. After thermal reaction under high pressure, pitch-graphite-silicon composite was prepared. Carbon-graphite-silicon composite were prepared by an air-oxidization and following carbonization. From energy dispersive spectroscopy, it was observed that small Si particles were highly embedded within carbon, which was confirmed by disappearance of Si peaks in Raman spectra. Furthermore, X-ray diffraction and Raman spectra revealed that carbon crystallinity decreased when the strongly oxidized silicon-graphite was added, which was probably due to oxygen-induced cross-linking. From the anode application in lithium ion batteries, carbon-graphite-silicon composite anode displayed a high capacity ($565\;mAh\;g^{-1}$), a good initial efficiency (68%) and an good cyclability (88% retention at 50 cycles), which were attributed to the high dispersion of Si particles within cabon. In case of the strongly oxidized silicongraphite addtion, a decrease of reversible capacity was observed due to its low crystallinity.

• 전기화학회지
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• 제22권3호
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• pp.112-121
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• 2019

본 연구에서는 마이크로 크기의 실리콘 입자와 탄소나노튜브를 활용하여 고용량을 갖는 실리콘/탄소나노튜브/탄소 복합입자를 제조하여 리튬이차전지용 음극활물질로서의 적용가능성을 확인하고자 하였다. 실리콘/탄소나노튜브/탄소 복합입자 제조를 위해 분무건조 방식을 이용하여 실리콘입자가 탄소나노튜브에 의해 균일하게 분산되어 비정질탄소로 결합된 구조를 갖는 구형의 복합입자를 제조하였다. 제조한 복합입자는 실리콘 입자 주변에 탄소나노튜브의 네트워크 구조를 형성하며 비정질 탄소에 의해 실리콘 입자와 탄소나노튜브의 입자들이 결합한 상태를 유지하는 구조로 이루어진다. 이러한 복합입자의 구조적인 특성으로 인해 계속적인 충방전 과정에서 실리콘의 부피팽창이 효과적으로 완충되고 이에 따라 전기적 접촉 손실 및 SEI 막 형성에 따른 비가역 반응이 제어되어 우수한 수명 특성 및 충전출력 특성을 갖는 것으로 나타난다.

• Carbon letters
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• 제8권4호
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• pp.335-339
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• 2007

Carbon/silicon composites were synthesized by mixing silicon powders with petroleum pitch and subsequent heat-treatment. The resultant composites were composed of carbon and nano-size crystalline silicon identified by XRD and EDX. FIB images and SEM images were taken respectively to detect the existence of silicon impregnated in carbon and the distribution of silicon on the carbon surface. The obtained carbon/silicon materials were assembled as half cell anodes for lithium ion secondary battery and their electrochemical properties were tested. The pitch/silicon composite (3 : 1 wt. ratio) heat treated at $1000^{\circ}C$ and mixed with 55.5 wt.% of graphite showed relatively good electrochemical properties such as the initial efficiency of 78%, the initial discharge capacity of 605 mAh/g, and the discharge capacity of 500 mAh/g after 20 cycles.

• Bulletin of the Korean Chemical Society
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• 제31권5호
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• pp.1257-1261
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• 2010

The electrochemical performances of anode composites comprising elemental silicon (Si), silicon monoxide (SiO), and graphite (C) were investigated. The composite devoid of elemental silicon (SiO:C = 1:1) and its carbon coated composite showed reduced capacity degradation with measured values of 606 and 584 mAh/g at the fiftieth cycle. The capacity retention nature when the composites were cycled followed the order of Si:SiO:C = 3:1:4 < Si:SiO:C = 2:2:4 < SiO:C = 1:1 < SiO:C = 1:1 (carbon coated). A comparison of the capacity retention properties for the composites in terms of the silicon content showed that a reduced silicon content increased the stability of the composite electrodes. Even though the carbon-coated composite delivered low capacity during cycling compared to the other composites, its low capacity degradation made the anode a better choice for lithium ion batteries.

• 한국분말재료학회지
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• 제22권1호
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• pp.15-20
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• 2015

The composite of porous silicon (Si) and amorphous carbon (C) is prepared by pyrolysis of a nano-porous Si + pitch mixture. The nano-porous Si is prepared by mechanical milling of magnesium powder with silicon monoxide (SiO) followed by removal of MgO with hydrochloric acid (etching process). The Brunauer-Emmett-Teller (BET) surface area of porous Si ($64.52m^2g^{-1}$) is much higher than that before etching Si/MgO ($4.28m^2g^{-1}$) which indicates pores are formed in Si after the etching process. Cycling stability is examined for the nano-porous Si + C composite and the result is compared with the composite of nonporous Si + C. The capacity retention of the former composite is 59.6% after 50 charge/discharge cycles while the latter shows only 28.0%. The pores of Si formed after the etching process is believed to accommodate large volumetric change of Si during charging and discharging process.

• Carbon letters
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• 제5권3호
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• pp.108-112
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• 2004

Effect of silicon infiltration on the bend and tensile strength of 2D cross-ply carbon-carbon composites are studied. It is observed that bend strength higher than tensile strength in both types of composite is due to the different mode of fracture and loading direction. After silicon infiltrations bend and tensile strength suddenly decreases of carbon-carbon composites. This is due to the fact that, after silicon infiltration, silicon in the immediate vicinity of carbon forms the strong bond between carbon and silicon by formation silicon carbide and un-reacted silicon as free silicon. Therefore, these composites consist of three components carbon, silicon carbide and silicon. Due to mismatch between these three components secondary cracks developed and these cracks propagate from $90^{\circ}$ oriented plies to $0^{\circ}$ oriented plies by damaging the fibers (i.e., in-situ fiber damages). Hence, secondary cracks and in-situ fiber damages are responsible for degradation of mechanical properties of carbon-carbon composites after silicon infiltration which is revealed by microstructure investigation study by scanning electron microscope.

• 한국안전학회지
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• 제33권1호
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• pp.1-6
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• 2018

The effects of the fiber direction, specimen size and temperature on the compressive strength of carbon fiber reinforced silicon carbide composite (C/SiC composite) manufactured by liquid silicon infiltration(LSI) is investigated. Tests were conducted in accordance with ASTM C 695 at room temperature and elevated temperatures. Experiments are conducted with two different specimens considering grain direction. With grain (W/G) specimens have a carbon fibers parallel to the load direction, but across grain (A/G) specimens have a perpendicular carbon fibers. To verify the specimen size effect of C/SiC composite, two types of specimens are manufactured. One has a one to two ratio of diameter to height and the other has a one to one ratio. The compressive strength of C/SiC composite increased as temperature rise. As specimens are larger, compressive strength of A/G specimens increased, however compressive strength of W/G decreased.

• Korean Chemical Engineering Research
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• 제56권4호
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• pp.561-567
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• 2018

본 연구에서는 리튬이온전지 실리콘 음극소재의 사이클 안정성 향상을 위해 실리콘/탄소 음극소재의 전기화학적 특성을 조사하였다. Tetraethyl orthosilicate (TEOS) 로부터 스토버법 및 마그네슘 열 환원법을 통하여 다공성 실리콘을 제조하고, 제조된 다공성 실리콘과 피치의 질량비에 따라 실리콘/탄소 음극소재를 제조하였다. 실리콘/탄소 음극소재의 물리적 특성은 XRD와 TGA를 통해 분석하였다. 1.0 M $LiPF_6$ (EC : DEC = 1 : 1 vol%) 전해액에서 실리콘/탄소 음극소재의 충 방전 사이클, 율속, 순환전압전류, 임피던스 테스트를 통해 전기화학적 특성을 조사하였다. 제조된 실리콘/탄소 음극소재 실리콘 : 탄소 = 5 : 95 일때 453 mAh/g의 향상된 용량을 나타내었으며, 사이클 성능 또한 두 번째 사이클 이후 30 사이클까지 매우 우수한 사이클 안정성을 나타냄을 확인하였다.