• Progress in Superconductivity and Cryogenics
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• v.14 no.4
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• pp.5-11
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• 2012

In this review article, we focus on various co-evaporation technologies developed for the fabrication of high performance $REBa_2Cu_3O_{7-{\delta}}$ (RE: Y and Rare earth elements, REBCO) superconducting films. Compared with other manufacturing technologies for REBCO films such as sputtering, pulsed laser deposition (PLD), metal-organic deposition (MOD), and metal organic chemical vapor deposition (MOCVD), the co-evaporation method has a strong advantage of higher deposition rate because metal sources can be used as precursor materials. After the first attempt to produce REBCO films by the co-evaporation method in 1987, various co-evaporation technologies for high performance REBCO films have been developed during last several decades. The key points of each co-evaporation technology are reviewed in this article, which enables us to have a good insight into a new high throughput process, called as a Reactive Co-Evaporation by Deposition and Reaction (RCE-DR).

• Journal of the Korean institute of surface engineering
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• v.29 no.6
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• pp.803-808
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• 1996

Material and electrical characteristies of copper thin films prepared by metal organic chemical vapor deposition (MOCVD) have been investigated for interconnection applications in ultra large scale integration circuits (ULSI). The copper films have been deposited a TiN substrates using a metal organic precursor, hexafluoro acetylacetonate trimethyvinylsilane copper, VTMS(hfac)Cu (I). Deposition rate, grain size, surface morphology, and electrical resistvity of the copper films have been measuredfrom samples prepared at various experimental conditions, which include substrate temperature, chamber pressure, and carrier gas flow rate. Results of the experiment showed that the electrical property of the copper films is closely related to the crystallinity of the films. Lowest electrical resistivity, $2.4{\mu}{\Omega}.cm$ was obtained at the substrate temperature of $180^{\circ}C$, but the resistivity slightly increased with increasing substrate temperature due to the carbon content along the copper grain boundaries.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2012.05a
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• pp.150-150
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• 2012

본 연구는 1차원 나노 구조의 합성과 기초적 분석에 관한 연구로써 특히 무기 산화물 나노재료를 그 대상으로 하였다. 내용으로는 첫째, 1차원 코어 나노와이어의 합성을 하였고 Thermal evaporation, substrate의 가열, 그리고 MOCVD 를 사용한 결과들을 나열한다. 둘째, 코어-쉘 나노와이어를 제작하기 위하여 특히 쉘층의 제작방법을 연구하였는데 PECVD, ALD, 그리고 sputtering에 의한 결과들을 나열하고 간단히 설명한다. Thermal evaporation에 의한 1차원 나노와이어 합성의 경우는 MgO의 예를 들었는데 MgO 나노와이어는 Au가 증착된 기판을 열처리하여 Au dot를 형성하고 이의 morphology를 조절하여 최적의 나노와이어 합성조건을 선정하였다. 이로써 기판 morphology가 나노선의 성장및 형상에 영향을 준다는 사실을 알게 되었다. 이 사실은 In2O3기판을 사용하고 이의 표면거칠기를 열처리로 조절하므로써 역시 나노와이어의 성장을 촉진하는 방법을 찾아내었다. 또한 thermal evaporation공법은 source분말의 선택에 따라 다양한 소재를 제작가능하다는 결과를 제시하였다. 예를 들면 SiOx 층이 precoating된 chamber내에서 MgO 나노선을 합성하는 것과 동일한 조건으로 실험을 진행하면 Mg2SiO4 나노와이어가 형성된 것을 확인하였다. 또한 Sn과 MgB2 분말을 함께 적용할 경우 Sn tip을 가진 MgO 나노와이어를 얻을 수 있었다. 이는 Sn이 동시에 촉매의 역할을 하였기 때문일 것으로 추정된다. 한편 Sn과 Bi 혼합분말을 적용한 경우 Bi2Sn2O7 신소재 tip을 포함한 SnO2 나노와이어를 얻을 수 있었다. 이 경우 Bi원자가 적절한 촉매의 역할을 수행한 것으로 사료된다. Substrate의 가열공법에서는 Si wafer상에 각종 금속 즉 Au, Ag, Cu, Co, Mo, W, Pt, Pd등 초박막을 DC sputter 로 형성한후 annealing하는 기술을 사용하였다. 특기할 만한 것은 Co를 사용한 경우 나노와이어의 spring구조를 얻을 수 있었다는 점이다. MOCVD에 의하여는 Ga2O3및 Bi2O3 나노와이어를 비교적 저온에서 합성하였고 In2O3의 경우는 독특한 나노구조를 형성하였고 이의 결정학적 특성에 대하여 조사하였다.

• Korean Journal of Materials Research
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• v.9 no.12
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• pp.1196-1204
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• 1999

We have carried out copper MOCVD(metalorganic chemical vapor deposition) onto the reactive sputtered PVD-TiN and rapid thermal converted RTP-TiN substrates using direct liquid injection for effective delivery of the (hfac)Cu(vtmos) [$C_{10}H_{13}O_{5}CuF_{6}$Si: 1,1,1,5,5,5-hexafluoro-2,4- pentadionato (vinyltrimethoxysilane) copper (I)] precursor. Especially, the influences of deposition conditions and the substrate type on growth rate, crystal structure, microstructure, and electrical resistivity of copper deposits have been discussed. It is found that the film growth with 0.2ccm precursor flow rate become mass-transfer controlled up to Ar flow rate of 200sccm and pick-up rate controlled at a vaporizer above 1.0Torr reactor pressure. The surface-reaction controlled region from 155 to 225$^{\circ}C$ at 0.6Torr reactor pressure results in the apparent activation energies of 12.7~14.1kcal/mol, and above 224$^{\circ}C$ the growth rate with $H_2$ addition could be improved compared to the pure Ar carrier. The Cu/RTP-TiN structures which have high copper nucleation density in initial stage of growth show more pronounced (111) preferred orientations and lower electrical resistivities than those on PVD-TiN. The variation of electrical resistivity with substrate temperature reflects the three types of film microstructure changes, showing the lowest value for the deposit at 165$^{\circ}C$ with small grains of good contacts.

• Progress in Superconductivity
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• v.13 no.2
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• pp.127-132
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• 2011

Many research groups have been manufacturing coated conductor by various processes such as PLD, MOD, and MOCVD, but the methods with production cost suitable for wide and massive application of coated conductor did not develop yet. Spray pyrolysis method adopting ultrasonic atomization was tried as one of the possible option. GdBCO precursor films have been deposited on IBAD substrate by spray pyrolysis method at low temperature and converted to GdBCO by post heat treatment. Ultrasonic atomization was used to generate fine droplets from precursor solution of Gd, Ba, and Cu nitrate dissolved in water. Primary GdBCO films were deposited at $500^{\circ}C$ and oxygen partial pressure of 1 torr. After that, the films were converted at various temperatures and low oxygen partial pressures. C-Axis oriented films were obtained IBAD substrates at conversion temperature of around $870^{\circ}C$ and oxygen partial pressures of 500 mtorr ~ 1 torr in a vacuum. Thick c-axis epitaxial film with the thickness of 0.4 ~ 0.5 ${\mu}m$ was obtained on IBAD substrate. C-axis epitaxial GdBCO films were successfully prepared by ex-situ methods using nitrate precursors on IBAD metal substrate. Converted GdBCO films have very dense microstructures with good grain connectivity. EDS composition analysis of the film showed a number of Cu-rich phase in surface. The precursor solution having high copper concent with the composition of Gd : Ba : Cu = 1 : 2 : 4 showed the better grain connectivity and electrical conductivity.

• Korean Journal of Materials Research
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• v.4 no.6
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• pp.681-686
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• 1994

Microwave Detector Using $YBa_{2}Cu_{3}O_{7-x}$, Grain Boundary Junction $YBa_{2}Cu_{3}O_{7-x}$ superconductor thin films were deposited on $LaAIO_{3}$ (100) single crystal substrates using a metal organic chemical vapor deposition (MOCVD) method. These films showed the critical temperature of about 9OK and critical current density of over $10^5/A \textrm{cm}^2$at 77K. These films showed granular structure with 0.5~1.5$\mu \textrm{m}$ grains. Bridge-type junctions, 6$\mu \textrm{m}$ in width and 6pm in length, were fabricated using the photolithography and the Ar ion milling techniques. Current-voltage (I-V) characteristics of these junctions with the microwave irradiation at 77K were studied. The critical current densities decreased as the irradiated microwave power increased. When microwaves were irradiated on the bridge at 77K. the I-V charateristics showed constant voltage stcp(Shapiro steps) at $\Delta$=nho/2e.

• Bulletin of the Korean Chemical Society
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• v.20 no.3
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• pp.355-361
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• 1999

To improve the volatility and stability of lead complexes, the principle of stabilization by saturating the metal coordination sphere by intramolecular coordination through a β-diketonates with an ethereal group has was tested. Several new lead complexes with alkoxyalkyl-substituted β-diketonates, Pb(R1C(O)CHC(O)(CH2)3OR2)2(Rl=t-Bu, Me, OMe, i-Pr, R2=Me, Et), or carboxylate, Pb(OC(O)(CH2)3OEt)2, were prepared by the reaction between Pb(OAc)2 and corresponding alkoxyalkyl-substituted β-diketonates, and they were found to have a viscous liquid phase. The nature of the head (β-diketonate or carboxylate) or tails and substituents of β-diketonates appeared not to be important for the formation of the liquid phase. It is worth mentioning that Pb(OAc)2, which has limited use due to its low solubility, was successfully adopted as a starting material for the preparation of new lead complexes. Easy hydrolysis, reaction with HCl, and 13C NMR spectra indicated that tail portions were not coordinated to the metal as a copper derivative, Cu(t-BuC(O)CHC(O)(CH2)3OMe)2. All these complexes were not volatile enough for the MOCVD experiments, but a methyl derivative, Pb(MeC(O)CHC(O)(CH2)3OEt)2, showed some sublimation. The methoxy derivative, Pb(MeOC(O)CHC(O)(CH2)3OEt)2, was thermally unstable due to possible equilibrium between species coordinating with a keto oxygen atom and an ethereal atom of a methoxy group, which was confirmed by IR and 13C NMR spectra.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.443-443
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• 2014

CIS 박막을 제조하기 위한 방법으로 셀렌화(selenization)방식, MOCVD방식, 동시진공증발(co-evaporation)방식, 전착(electrodeposition)방식 등이 있으나, 이러한 방식을 이용하여 CuInSe2 박막을 제조하는 경우 어떤 방법으로든 다원화합물의 조성 및 결정성을 조절하기가 매우 어려운 단점이 있었다. 기판의 온도를 일정 온도로 유지하도록 하고, 증발원을 가열하여 이에 내포된 물질(이원화합물 또는 단일원소)을 증발시켜 기판에 증착이 이루어지도록 하거나, 기판의 온도를 승온시키고 구리 이원화합물을 내포한 증발원을 가열해 물질을 증발시켜 기판에 증착이 이루어지도록 하는 방법으로 기판에 박막이 형성되도록 한다. 기판의 대면적화로 인해 균일한 박막의 형성이 어려워지고 있으며, 이중 15% 이상의 고효율을 보인 방법은 3-stage process를 이용한 동시진공증발방식으로, Cu, In, Ga, Se 등의 각 원소를 동시에 진공 증발시키면서 조성을 조절하여 태양전지에 적절한 전기적, 광학적 특성을 가지는 Cu(In,Ga)Se2 (CIGS)박막을 증착시키는 방법이다. 일반적으로, 실험실에서 연구되고 있는 장비의 구조는 증발원이 아래에 장착되어서 상향 증착되는 방식이다. 본 연구에서 사용된 장비는 하향 증발원이 측면에 장착되어서 하향 증착되는 방식으로 구성하였다. 증착되는 면방향으로, 적외선온도계(pyrometer)가 설치된 시창(viewport)의 오염 등으로 인하여, 지속적인 공정이 이루어지기 힘든 점을 개선하여 증착기판의 후면에 적외선 온도계를 설치하여 기판의 온도변화를 감지하여 공정에 반영할 수 있도록 하였다. 본 연구에서는 하향식 진공 증발원, 기판후면 온도모니터링모듈 등을 개발 장착하여, CIGS 박막을 제조하였으며, 버퍼층은 moving 스퍼터링법으로 ZnS를 증착하였고, 투명전극층은 PLD(Pulsed Laser Deposition)를 이용하여 제조하였다. 가장 높은 광변환효율을 보인 Al/ZnO/CdS/Mo/SLG박막시료는 유효면적 $0.45cm^2$에 광변환효율 15.65 %, Jsc : $33.59mA/cm^2$, Voc : 0.64 V, FF : 73.09 %를 얻을 수 있었으며, CdS를 ZnS로 대체한 Al/ZnO/ZnS/Mo/SLG박막시료는 유효면적 $0.45cm^2$에 광변환효율 12.45 %, Jsc : $33.62mA/cm^2$, Voc : 0.59 V, FF : 62.35 %를 얻을 수 있었다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2001.11a
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• pp.35-35
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• 2001

agnesium Oxide (MgO) with a NaCI structure is well known to exhibit high secondary electron emission, excellent high temperature chemical stability, high thermal conductance and electrical insulating properties. For these reason MgO films have been widely used for a buffer layer of high $T_c$ superconducting and a protective layer for AC-plasma display panels to improve discharge characteristics and panel lifetime. Up to now MgO films have been synthesized by lE-beam evaporation, Molecular Beam Epitaxy (MBE) and Metalorganic Chemical Vapor Deposition (MOCVD), however there have been some limitations such as low film density and micro-cracks in films. Therefore magnetron sputtering process were emerged as predominant method to synthesis high density MgO films. In previous works, we designed and manufactured unbalanced magnetron source with high power density for the deposition of high quality MgO films. The magnetron discharges were sustained at the pressure of O.lmtorr with power density of $110W/\textrm{cm}^2$ and the maximum deposition rate was measured at $2.8\mu\textrm{m}/min$ for Cu films. In this study, the syntheses of MgO films were carried out by unbalanced magnetron sputtering with various $O_2$ partial pressure and specially target power densities, duty cycles and frequency using pulsed DC power supply. And also we investigated the plasma states with various $O_2$ partial pressure and pulsed DC conditions by Optical Emission Spectroscopy (OES). In order to confirm the relationships between plasma states and film properties such as microstructure and secondary electron emission coefficient were analyzed by X-Ray Diffraction(XRD), Transmission Electron Microscopy(TEM) and ${\gamma}-Focused$ Ion Beam (${\gamma}-FIB$).