• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.26 no.3
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• pp.232-239
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• 2013

Thin light-active layers of the $CuInSe_2$ solar cell were prepared on Mo-coated sodalime glass substrates by one-step electrodeposition and post-annealing. The structure, morphology, and composition of $CuInSe_2$ film could be controlled by deposition parameters, such as the composition of metallic precursors, the concentration of complexing agents, and the temperature of post-annealing with elemental selenium. A dense and uniform Cu-poor $CuInSe_2$ film was successfully obtained in a range of parametric variation of electrodeposition with a constant voltage of -0.5 V vs. a Ag/AgCl reference electrode. The post-annealing of the film at high temperature above $500^{\circ}C$ induced crystallization of $CuInSe_2$ with well-developed grains. The KCN-treatment of the annealed $CuInSe_2$ films further induced Cu-poor $CuInSe_2$ films without secondary phases, such as $Cu_2Se$. The structure, morphology, and composition of $CuInSe_2$ films were compared with respect to the conditions of electrodeposition and post-annealing using SEM, XRD, Raman, AES and EDS analysis. And the conditions for preparing device-quality $CuInSe_2$ films by electrodeposition were proposed.

• Proceedings of the KIEE Conference
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• 2007.07a
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• pp.1269-1270
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• 2007

Carbon nanotubes (CNTs) are directly grown on W-tips at $700^{\circ}C$ using an ICP-CVD method. Sharpening of W-tip is done by electrochemical etch and their diameters are limited to range from $3{\mu}m$ to $5{\mu}m$. Catalysts for CNTs growth are formed by RF and DC co-sputtering systems using Ni and Co. The composition ratio of Ni and Co has been evaluated by energy dispersive x-ray spectroscopy (EDS). The micro-images of CNTs are monitored by field emission scanning electron microscope (FESEM). It is observed from Raman study that the intensity of the D-peak is increased by increasing the amount of Co catalyst. Furthermore, the measurement of field emission properties of CNTs show that the CNT grown on a single Co catalyst possess the greatest performance such as $V_{th}$=1,115V and $I_{max}=164{\mu}A$.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.64-64
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• 2000

Since its discovery in 1991, the carbon nanotube has attracted much attention all over the world; and several method have been developed to synthesize carbon nanotubes. According to theoretical calculations, carbon nanotubes have many unique properties, such as high mechanical strength, capillary properties, and remarkable electronical conductivity, all of which suggest a wide range of potential applications in the future. Here we report the synthesis in the catalytic decomposition of acetylene at ~65 $0^{\circ}C$ over Ni deposited on SiO2, For the catalyst preparation, Ni was deposited to the thickness of 100-300A using effusion cell. Different approaches using porous materials and HF or NH3 treated samples have been tried for synthesis of carbon nanotubes. It is decisive step for synthesis of carbon nanotubes to form a round Ni particles. We show that the formation of round Ni particles by heat treatment without any pre-treatment such as chemical etching and observe the similar size of Ni particles and carbon nanotubes. Carbon nanotubes were synthesized by chemial vapour deposition ushin C2H2 gas for source material on Ni coated Si substrate. Ni film gaving 20~90nm thickness was changed into Ni particles with 30~90nm diameter. Heat treatment of Ni fim is a crucial role for the growth of carbon nanotube, High-resolution transmission electron microscopy images show that they are multi-walled nanotube. Raman spectrum shows its peak at 1349cm-1(D band) is much weaker than that at 1573cm-1(G band). We believe that carbon nanotubes contains much less defects. Long carbon nanotubes with length more than several $\mu$m and the carbon particles with round shape were obtained by CVD at ~$650^{\circ}C$ on the Ni droplets. SEM micrograph nanotubes was identified by SEM. Finally, we performed TEM anaylsis on the caron nanotubes to determine whether or not these film structures are truly caron nanotubes, as opposed to carbon fiber-like structures.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.175-175
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• 2000

Si(100) surfaces were exposed to gas-phase thermal-energy hydrogen atoms, H(g). We find that thermal H(g) atoms etch, amorphize, or penetrate into the crystalline silicon substrate, depending on the employed Ts range during the H(g) exposure. We find that etching is enhanced as Ts is lowered in the 300-700K range, while amorphous silicon hydride (a-Si:H) formation dominates at a Ts below 300K. This result was well explained by the fact that formation of the etching precursor, SiHx(a), and amorphization are both facilitated by a lower Ts, whereas the final step for etching, SiH3(a) + H(g) longrightarrow SiH3(g), is suppressed at a lower Ts. we also find that direct absorption of H(g) by the crystalline bulk of Si(100) substrate occurs within a narrow Ts window of 420-530K. The bulk-absorbed hydrogen evolved out molecularly from Si(100) at a Ts 80-120K higher than that for surface monohydride phase ($\beta$1) in temperature-programmed desorption. This bulk-phase H uptake increased with increasing H(g) exposure without saturation within our experimental limits. Direct absorption of H(g) into the bulk lattice occurs only when the surface is atomically roughened by surface etching. While pre-adsorbed hydrogen atoms on the surface, H(a), were readily abstracted and replaced by D(g), the H atoms previously absorbed in the crystalline bulk were also nearly all depleted, albeit at a much lower rate, by a subsequent D(g) at the peak temperature in TPD from the substrate sequentially treated with H(g) and D(g), together with a gas phase-like H2 Raman frequency of 4160cm-1, will be presented.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.72-72
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• 2010

탄소나노튜브(carbon nanotubes : CNTs)는 뛰어난 전기적, 물리적인 특성을 가지고 있기 때문에 다양한 분야에서 이를 활용하려는 노력들이 활발히 이루어지고 있다. CNTs의 전기적인 특성은 직경에 의해 결정되므로, 직경을 균일하게 제어하는 일이 CNTs를 기반으로 한 전자소자 응용에 가장 중요한 사항이라 할 수 있다. 일반적으로 화학기상증착법(chemical vapor deposition, CVD)으로 합성된 CNTs의 직경은 촉매의 크기에 의존하기 때문에, 촉매의 크기를 제어하기 위한 다양한 연구들이 활발히 진행되고 있다[1-3]. 하지만 CNTs의 성장온도 근처에서 촉매 입자는 표면 확산(surface diffusion)에 의해 응집(agglomeration)되기 때문에 작고 균일한 크기의 촉매를 얻기 어렵다. 본 연구에서는 Si(001) 기판 위에 지지층(supporting layer)인 Al의 두께를 변화시켜 증착하고, 열적산화과정을 통해 $Al_2O_3$ 층을 형성한 후 Fe을 증착하여 CNTs를 합성하였다. $Al_2O_3$ 지지층과 Fe 촉매입자의 구조와 화학적 상태를 원자힘현미경 (atomic force microscopy, AFM), 주사전자현미경 (scanning electron microscopy, SEM), 투과전자현미경 (transmission electron microscopy, TEM), X-선 광전자 분광기(X-ray photoelectron spectroscopy)를 통해 분석하였고, 성장된 CNTs는 SEM, TEM, 라만 분광법 (Raman spectroscopy)을 통해 분석하였다. 그 결과, $Al_2O_3$ 층은 두께에 따라 각기 다른 표면 거칠기(RMS roughness)와 결정립(grain)의 크기를 갖게 되며, 이러한 표면구조가 Fe 촉매입자의 표면확산에 의한 응집에 관여하여 CNTs의 직경에 영향을 미치는 것을 확인하였다. 또한 $Al_2O_3$ 지지층의 두께가 15 nm인 경우, Fe의 응집현상이 억제되어 좁은 직경분포를 지닌 고순도 단일벽 탄소나노튜브(Single-walled CNTs)가 성장되는 것을 확인하였다.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.141-141
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• 2010

The effect of thermal anneal on the characteristics of structural properties and the enhancement of luminescence and photovoltaic (PV) characteristics of silicon-rich silicon-nitride films were investigated. By using an ultra high vacuum ion beam sputtering deposition, B-doped silicon-rich silicon-nitride (SRSN) thin films, with excess silicon content of 15 at. %, on P-doped (n-type) Si substrate was fabricated, sputtering a highly B doped Si wafer with a BN chip by N plasma. In order to examine the influence of thermal anneal, films were then annealed at different temperature up to $1100^{\circ}C$ under $N_2$ environment. Raman, X-ray diffraction, and X-ray photoemission spectroscopy did not show any reliable evidence of amorphous or crystalline Si clusters allowing us concluding that nearly no Si nano-cluster could be formed through the precipitation of excess Si from SRSN matrix during thermal anneal. Instead, results of Fourier transform infrared and X-ray photoemission spectroscopy clearly indicated that defective, amorphous Si-N matrix of films was changed to be well-ordered thanks to high temperature anneal. The measurement of spectral ellipsometry in UV-visible range was carried out and we found that the optical absorption edge of film was shifted to higher energy as the anneal temperature increased as the results of thermal anneal induced formation of $Si_3N_4$-like matrix. These are consistent with the observation that higher visible photoluminescence, which is likely due to the presence of Si-N bonds, from anneals at higher temperature. Based on these films, PV cells were fabricated by the formation of front/back metal electrodes. For all cells, typical I-V characteristic of p-n diode junction was observed. We also tried to measure PV properties using a solar-simulator and confirmed successful operation of PV devices. Carrier transport mechanism depending on anneal temperature and the implication of PV cells based on SRSN films were also discussed.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.9-10
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• 2010

Since the discovery of graphene by mechanical exfoliation from graphite[1], various fabrication methods are available today such as chemical exfoliation, epitaxial graphene on SiC substrates, etc. In view of industrialization, the mechanical exfoliation method may not be an option. Epitaxial graphene on SiC substrates, in this respect, is by far more practical because the method consists of conventional thermal treatments familiar to semiconductor industry. Still, the use of the SiC substrate itself, and hence the incompatibility with the Si technology, lessens the importance of this technology in its future industrialization. In this context, we have tackled the problem of forming graphene on Si substrates (GOS). Our strategy is to form an ultrathin (~80 nm) SiC layer on top of a Si substrate, and to graphitize the top SiC layers by a vacuum annealing. We have actually succeeded in forming the GOS structure [2,3,4]. Raman-scattering microscopy indicates presence of few-layer graphene (FLG) formed on our annealed SiC/Si heterostructure, with the G ($1580\;cm^{-1}$) and the G'($2700\;cm^{-1}$) bands, both related to ideal graphene, clearly observed. Presence of the D ($1350\;cm^{-1}$) band indicates presence of defects in our GOS films, whose elimination remains as a challenge in the future. To obtain qualified graphene films on Si substrate, formation of qualified SiC films is crucial in the first place, and is achieved by tuning the growth parameters into a process window[5]. With a potential for forming graphene films on large-scale Si wafers, GOS is a powerful candidate as a key technology in bringing graphene into silicon technology.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.80-80
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• 2010

Graphene has attracted tremendous attention for the last a few years due to it fascinating electrical, mechanical, and chemical properties. Up to now, several methods have been developed exclusively to prepare graphene, which include micromechanical cleavage, polycrystalline Ni employing chemical vapor deposition technique, solvent thermal reaction, thermal desorption of Si from SiC substrates, chemical routes via graphite intercalation compounds or graphite oxide. In particular, polycrystalline Ni foil and conventional chemical vapor deposition system have been widely used for synthesis of large-area graphene. [1-3] In this study, synthesis of mono-layer graphene on a Ni foil, the mixing ratio of hydrocarbon ($CH_4$) gas to hydrogen gas, microwave power, and growth time were systemically optimized. It is possible to synthesize a graphene at relatively lower temperature ($500^{\circ}C$) than those (${\sim}1000^{\circ}C$) of previous results. Also, we could control the number of graphene according to the growth conditions. The structural features such as surface morphology, crystallinity and number of layer were investigated by scanning electron microscopy (SEM) and atomic force microscopy (AFM), transmission electron microscopy (TEM) and resonant Raman spectroscopy with 514 nm excitation wavelength. We believe that our approach for the synthesis of mono-layer graphene may be potentially useful for the development of many electronic devices.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.79-79
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• 2010

최근, 차세대 디스플레이, 터치스크린, 전자파 차폐 및 흡수 등의 분야에 응용하기 위해서 현재 주로 사용되고 있는 ITO박막을 대체하기 위한 연구가 활발하게 진행 되고 있다. ITO 박막은 희소원소인 인듐에서 기인하는 높은 비용뿐만 아니라 매장량도 한계가 있어 대체 재료의 개발이 시급하게 요구되고 있다. 더구나, 다양한 차세대 응용에 있어서는 투명전도성 뿐만 아니라 휠 수 있는 유연성까지 요구되어 ITO박막을 대체할 새로운 투명전도성 유연 박막의 개발에 관한 연구들이 활발히 이루어지고 있다. 탄소나노튜브(CNT)는 금속을 능가하는 이론적인 전기전도도를 갖고 있으며, 높은 탄성등의 우수한 기계적 성질을 갖고 있어, 전도성 확보 및 유연성 구현이라는 투명전도성 플렉서블 박막소재에 요구되는 사항들을 충족시킬 뿐만 아니라, 최근의 대량 합성법등의 개발로 저가에 공급할 수 있다는 장점들이 있어 ITO대체 재료로서 주목을 받고 있다. 그러나, CNT는 튜브 사이에 강한 반데르발스 인력을 가지고 있어 용매 중에 분산하는데 많은 어려움이 있으며, 액상 분산과정을 통한 CNT기반의 플렉서블 박막 제작에 있어서 큰 과제로 남아있다. 본 연구에서는 플라즈마 기능화 처리를 통하여 CNT에 친수성을 부여하였고, 초음파 처리를 통하여 에탄올 중에 CNT를 균일하게 분산한 후, 스프레이 분사법을 이용해 투명 유연기판인 PET고분자 필름위에 균일 박막을 제작하였다. CNT는 아세틸렌 가스를 이용한 열화학증기증착법으로 1mm 이상의 길이를 갖는 수직배향 CNT를 합성하였으며, 이를 아르곤 및 암모니아 플라즈마로 기능화 처리를 실시하였다. 플라즈마 처리를 통해 기능화 된 탄소나노튜브는 플라즈마 처리되지 않은 탄소나노튜브와 분산 속도에서 현저한 차이를 보였다. 제작한 CNT 기반의 투명전도성 유연박막들은 막두께에 따른 전도도 및 투광도의 관계를 조사하였고, 기판에 분사된 CNT 박막의 표면 특성은 AFM, Raman, 접촉각 실험 등을 통하여 분석하였다.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.288-288
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• 2013

Lithium-ion battery (LIB) is one of the most important rechargeable battery and portable energy storage for the electric digital devices. In particular, study about the higher energy capacity and longer cycle life is intensively studied because of applications in mobile electronics and electric vehicles. Generally, the LIB's capacity can be improved by replacing anode materials with high capacitance. The graphite, common anode materials, has a good cyclability but shows limitations of capacity (~374 mAh/g). On the contrary, silicon (Si) and germanium(Ge), which is same group elements, are promising candidate for high-performance LIB electrodes because it has a higher theoretical specific capacity. (Si:4200 mAh/g, Ge:1600 mAh/g) However, it is well known that Si volume change by 400% upon full lithiation (lithium insertion into Si), which result in a mechanical pulverization and poor capacity retention during cycling. Therefore, variety of nanostructure group IV elements, including nanoparticles, nanowires, and hollow nanospheres, can be promising solution about the critical issues associated with the large volume change. However, the fundamental research about correlation between the composition and structure for LIB anode is not studied yet. Herein, we successfully synthesized various structure of nanowire such as Si-Ge, Ge-Carbon and Si-graphene core-shell types and analyzed the properties of LIB. Nanowires (NWs) were grown on stainless steel substrates using Au catalyst via VLS (Vapor Liquid Solid) mechanism. And, core-shell NWs were grown by VS (Vapor-Solid) process on the surface of NWs. In order to characterize it, we used FE-SEM, HR-TEM, and Raman spectroscopy. We measured battery property of various nanostructures for checking the capacity and cyclability by cell-tester.