• 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.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2002.11a
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• pp.29-29
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• 2002

공구강 등 산업용 재료로 널리 사용되는 카바이드 계 재료는 입자 크기 및 분포에 따라 기계적 성질이 변화하므로, 이를 제어하고 조절하는 기술에 관하여 많은 연구가 진행되어 왔다. 본 연구에서는 TiCN-WC-Co 복합초경계 에서 소결 공정 및 조성변화에 따른 입자 모양을 관찰하고 이에 따른 업자 성장 거동을 고찰하였다. 일반적으로 입자 조대화 양상과 고상 입자의 모양과는 밀접한 관계가 있다. 각진 입자의 경우에 는 계면이 원자적으로 singular 하여 원자의 홉착이 어렵기 때문에 임계값 이상의 성장 구동력을 받 는 몇몇 입자만 성장하는 비정상 입자 성장이 일어날 수 있다. 반면에 계면이 rough한 퉁큰 엽자의 경우에는 원자 홉착에 필요한 구동력이 존재하지 않아 성장 구동력을 받는 모든 입자들이 성장하기 때문에 정상 입자 성장을 하게 된다. 이와 같이 입자 모양에 따른 입자 성장 거동은 전체 미세구조를 결정하게 되며, 이에 따른 물리 화학적 물성을 변화시킨다. 이러한 입자 성장 원리를 적용하 면 복합초경계 (TiCN-WC-Co)에서도 입자성장이 억제되고 치밀한 소결체를 제조할 수 있을 것이다. 본 실험에서는 평균입도가 각각 0.1, 1.33, 2$\mu\textrm{m}$인 TiCN, WC, Co 분말을 사용하여 $((I00_{-x)}TiCN+_xWC)-30Co$ (wt%) 조성에서 TiCN/WC 비를 변화시키면서 업자 모양과 입자성장 거동을 관찰하였다. 청량된 분말은 WC 초경 볼로 밀렁하고, 건조한 후, 100 mesh 체로 조립화 하였다. 이 분말을 100 MPa의 압력으로 냉간정수압성형 하고 $10^{-2}$ torr의 진공분위기의 graphite f furnace에서 carbon black으로 packing 하여 액상형성 온도 이상에서 소결하였다. 소결된 시편은 경면 연마하여 주사전자현미경으로 미세 조직을 관찰하였다. TiCN-30Co 조성 시편은 corner-round 모양의 입자 모양으로 소결 시간 증가에 따라 빠른 입자 성장을 나타내었다 .(7STiCN+2SWC)-30Co 조성 시변의 경우 일반적으로 보고된 바와 같이 core/shell 구조를 나타내었으며, core는 TiC-rich 상이었고, shell은 (Ti,W)(C,N) 복합 탄화물 상이었다. WC 함량이 중가함에 따라 입자의 corner-round 영역이 증가하였으며 (SOTiCN-SOWC)-30Co 조성 근처에서는 거의 둥근 형태의 입자 모양을 나타내었다. 또한 TiCN - 30Co 조성 시편에 비하여 WC가 첨가된 시펀들은 작은 평균입자크기를 나타내었다. 본 연구의 결과는 shell 영역 조성 변화는 계면에너지 이방성과 기지상 내의 펑형 입자 모양을 변화시키고 나아가 입자 성장 속도 에도 영향을 미친다는 것을 보여준다.

• Journal of Powder Materials
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• v.24 no.4
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• pp.302-307
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• 2017

In this study, Fe-Cu-C alloy is sintered by spark plasma sintering (SPS). The sintering conditions are 60 MPa pressure with heating rates of 30, 60 and $9^{\circ}C/min$ to determine the influence of heating rate on the mechanical and microstructure properties of the sintered alloys. The microstructure and mechanical properties of the sintered Fe-Cu-C alloy is investigated by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). The temperature of shrinkage displacement is changed at $450^{\circ}C$ with heating rates 30, 60, and $90^{\circ}C/min$. The temperature of the shrinkage displacement is finished at $650^{\circ}C$ when heating rate $30^{\circ}C/min$, at $700^{\circ}C$ when heating rate $60^{\circ}C/min$ and at $800^{\circ}C$ when heating rate $90^{\circ}C/min$. For the sintered alloy at heating rates of 30, 60, and $90^{\circ}C/min$, the apparent porosity is calculated to be 3.7%, 5.2%, and 7.7%, respectively. The hardness of the sintered alloys is investigated using Rockwell hardness measurements. The objective of this study is to investigate the densification behavior, porosity, and mechanical properties of the sintered Fe-Cu-C alloys depending on the heating rate.

• Applied Chemistry for Engineering
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• v.19 no.2
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• pp.185-190
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• 2008

In order to increase the surface area of electrodes for electrosorption, porous carbon electrodes were fabricated by a wet phase inversion method. A carbon slurry consisting of a mixture of activated carbon powder (ACP), polyvinylidene fluoride (PVdF), and N-methyl-2-pyrrolidone (NMP) as a solvent was cast directly on a graphite sheet. The cast film was then immersed in pure water for phase inversion. The physical and electrochemical properties of the electrodes were investigated using scanning electron microscopy (SEM), porosimetry, and cyclic voltammetry. The SEM images verified that the pores of various sizes were formed uniformly on the electrode surface. The average pore sizes determined for the electrodes fabricated with various NMP contents ranged from 64.2 to 82.4 nm and the size increased as the NMP content increased. All of the voltammograms showed a typical behavior of charging and discharging characteristic at the electric double layer. The electrical capacitance ranged from 3.88 to $5.87F/cm^2$ depending on the NMP contents, and the electrical capacitance increased as the solvent content decreased. The experimental results showed that the solvent content is an important variable controlling pore size and ultimately the capacitance of the electrode.

• Applied Chemistry for Engineering
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• v.19 no.2
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• pp.145-150
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• 2008

In this work we have studied the antifouling properties of the hydrophobic sol-gel modified sensing membrane and its optical properties for sensor application. E. coli JM109, B. cereus 318 and P. pastoris X-33 were cultivated in confocal cultivation dishes with glass surface, respectively. The glass surface was coated with the hydrophobic sol-gels prepared by the dimethoxy-dimethyl-silane (DiMe-DMOS) and tetramethyl-orthosilicate (TMOS). After cultivation, microorganisms adhered on the surface coated with sol-gels and glass surface were dyed by gram-staining method and the numbers of microorganisms were analyzed based on the image data of the scanning electronic microscope (SEM). A great number of microorganisms, about $2{\sim}3{\times}10^4/mm^2$, was adhered on the glass surfaces which no hydrophobic sol-gels were coated. But, the antifouling effect of the hydrophobic sol-gels was large, that microorganisms of less than $200{\sim}300/mm^2$ were adhered on the coated glass surface. The performance of the sensing membranes for detection of pH and dissolved oxygen was enhanced by recoating the light insulation layer prepared with the mixture of the hydrophobic sol-gel and graphite particles.

• 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.

• Applied Chemistry for Engineering
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• v.19 no.2
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• pp.222-227
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• 2008

In this work we have studied the antifouling properties of the hydrophobic sol-gel modified sensing membrane and its optical properties for sensor application. E. coli JM109, B. cereus 318 and P. pastoris X-33 were cultivated in confocal cultivation dishes with glass surface, respectively. The glass surface was coated with the hydrophobic sol-gels prepared by the dimethoxy-dimethyl-silane (DiMe-DMOS) and tetramethyl-orthosilicate (TMOS). After cultivation, microorganisms adhered on the surface coated with sol-gels and glass surface were dyed by gram-staining method and the numbers of microorganisms were analyzed based on the image data of the scanning electronic microscope (SEM). A great number of microorganisms, about $2{\sim}3{\times}10^4/mm^2$, was adhered on the glass surfaces which no hydrophobic sol-gels were coated. However, the antifouling effect of the hydrophobic sol-gels was large, that microorganisms of less than $200{\sim}300/mm^2$ were adhered on the coated glass surface. The performance of the sensing membranes for detection of pH and dissolved oxygen was enhanced by recoating the light insulation layer prepared with the mixture of the hydrophobic sol-gel and graphite particles.

• Applied Chemistry for Engineering
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• v.19 no.4
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• pp.407-412
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• 2008

As an activation procedure, in this study, the oxidation treatment of needle cokes with a dilute nitric acid and sodium chlorate $(NaClO_3)$, combined with heat treatment, was attempted. The structures of acid-treated and pyrolyzed coke were examined with XRD, FESEM, elemental analyzer, BET, and Raman spectroscopy. The behavior of double layer capacitance was investigated with the analysis of charge and discharge. The structure of needle coke treated with acid was revealed to a single phase of (001) diffraction peak after 24 h. On the other hand, thecoke oxidized by heat treatment was reduced to a graphite structure of (002) at $300^{\circ}C$. The distorted graphene layer structure, derived from the process of oxidation and reduction of the inter-layer, makes the pores by the electric field activation at the first charge, and generates the double layer capacitance from the second charge. The cell using pyrolyzed coke with 24 h acid treatment and $300^{\circ}C$ heat treatment exhibited the maximum capacitance per weight and volume of 33 F/g and 30 F/mL at the two-electrode system in the potential range of 0~2.5 V.

• Applied Chemistry for Engineering
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• v.27 no.6
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• pp.612-619
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• 2016

In this research, an alumino-borosilicate foamed glass with sound absorption property was prepared using the waste borosilicate glass obtained from the recycling process of waste liquid crystal display (LCD) panel. A 100 g of pulverized waste borosilicate glass with the particle size of under 325 mesh, was mixed with 0.3 g (wt/wt) of graphite, each 1.5 g (wt/wt) of $Na_2CO_3$, $Na_2SO_4$ and $CaCO_3$ as a foaming agent, and 6.0 g (wt/wt) of $H_3BO_3$ and 3.0 g (wt/wt) of $Al_2O_3$ as a pore control agent. Following mixture was under the foaming process for 20 minutes at a foaming temperature of $950^{\circ}C$. The result yielded the foaming agent with 45% of the opened porosity and 0.5-0.7 of the sound absorbing coefficient. This alumino-borosilicate foamed glass with the sound absorption property showed excellent physical and mechanical properties such as density of $0.21g/cm^3$, bending strength of $55N/cm^2$ and compression strength of $298N/cm^2$ which can be ideally used as sound absorption materials with heat-resisting and chemical-resisting property.

• Journal of the Korean institute of surface engineering
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• v.46 no.2
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• pp.68-74
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• 2013

For the coating of diamond films on WC-Co tools, a buffer interlayer is needed because Co catalyzes diamond into graphite. W and Ti were chosen as candidate interlayer materials to prevent the diffusion of Co during diamond deposition. W or Ti interlayer of $1{\mu}m$ thickness was deposited on WC-Co substrate under Ar in a DC magnetron sputter. After seeding treatment of the interlayer-deposited specimens in an ultrasonic bath containing nanometer diamond powders, $2{\mu}m$ thick nanocrystalline diamond (NCD) films were deposited at $600^{\circ}C$ over the metal layers in a 2.45 GHz microwave plasma CVD system. The cross-sectional morphology of films was observed by FESEM. X-ray diffraction and visual Raman spectroscopy were used to confirm the NCD crystal structure. Micro hardness was measured by nano-indenter. The coefficient of friction (COF) was measured by tribology test using ball on disk method. After tribology test, wear tracks were examined by optical microscope and alpha step profiler. Rockwell C indentation test was performed to characterize the adhesion between films and substrate. Ti and W were found good interlayer materials to act as Co diffusion barriers and diamond nucleation layers. The COFs on NCD films with W or Ti interlayer were measured as less than 0.1 whereas that on bare WC-Co was 0.6~1.0. However, W interlayer exhibited better results than Ti in terms of the adhesion to WC-Co substrate and to NCD film. This result is believed to be due to smaller difference in the coefficients of thermal expansion of the related films in the case of W interlayer than Ti one. By varying the thickness of W interlayer as 1, 2, and $4{\mu}m$ with a fixed $2{\mu}m$ thick NCD film, no difference in COF and wear behavior but a significant change in adhesion was observed. It was shown that the thicker the interlayer, the stronger the adhesion. It is suggested that thicker W interlayer is more effective in relieving the residual stress of NCD film during cooling after deposition and results in stronger adhesion.