UHV - LCVD 장치를 이용한 박막제작에 관한 연구 (Ⅰ) - 장치 제작을 중심으로 -

최원국(Won Kook Choi),윤덕주(Dug Ju Yun),공병인(Byung In Gong),김창현(Chang Hyun Kim),황정남(Chung Nam Whang),정광호(Kwang Ho Jeong) 한국진공학회(ASCT) 1993 Applied Science and Convergence Technology Vol.2 No.2

Si₃N₄와 SiO₂ 박막을 고순도로 생장시키기 위하여 UHV-LCVD 장치를 제작하였다. 이 장치는 CVD 반응실, 시료주입 장치, 가스주입 장치, 광여기를 위한 레이저 창, 질량분석 장치로 구성되어 있다. UHV-LCVD 는 low pressure, low vacuum CVD에 비해 제작상의 어려움이 따르나 초고진공 분위기에서 반응 가스의 양을 정확히 조절하여 고순도의 박막을 제작할 수 있었다. UHV-LCVD system was constructed for high quality silicon nitride thin film fabrication. This system consisted of a reaction chamber, an introduction chamber with sample load lock entry, a carbinet for gas manipulation controlling gas flow, a CO₂ laser and a Fourier transform mass spectrometer. Although the UHV-LCVD system construction was more sophisticated than low pressure CVD, highly pure thin films were fabricated by controlling gas mixing ratio and flow rate in ultra high vacuum surroundings.

저에너지 고출력 이온빔을 이용한 polyvinylidene fluoride 표면의 초친수성화

박종용,정연식,최원국,Park Jong-Yong,Jung Yeon-Sik,Choi Won-Kook 한국재료학회 2005 한국재료학회지 Vol.15 No.6

Polyvinylidene fluoride (PVDF) surface was irradiated and became superhydrophilic by low energy (180 eV) and high flux $(\~10^{15}/cm{\cdot}s)$ ion beam. As an ion source, a closed electron Hall drift thruster of $\phi=70mm$ outer channel size without grid was adopted. Ar, $O_2$ and $N_2O$ were used for source gases. When $N_2O^+$ and $O_2^+$ reactive gas ion beam were irradiated with the ion fluence of $5\times10^{15}/cm^2$, the wetting angle for deionized water was drastically dropped from $61^{\circ}\;to\;4^{\circ}\;and\;2^{\circ}$, respectively. Surface energy was also increased up to from 44 mN/m to 81 mN/m. Change of chemical component in PVDF surface was analyzed by x-ray photoelectron spectroscopy. Such a great increase of the surface energy was intimately related with the increase of hydrophilic group component in reactive ion irradiated PVDF surfaces. By using an atomic force microscopy, the root-mean-square of surface roughness of ion irradiated PVDF was not much altered compared to that of pristine PVDF.

라디칼 빔 보조 분자선 증착법 (Radical Beam Assisted Molecular Beam Epitaxy) 법에 의해 성장된 ZnO 박막의 발광 특성에 관한 연구

서효원,변동진,최원국,Suh, Hyo-Won,Byun, Dong-jin,Choi, Won-Kook 한국재료학회 2003 한국재료학회지 Vol.13 No.6

II-Ⅵ ZnO compound semiconductor thin films were grown on $\alpha$-Al$_2$O$_3$(0001) single crystal substrate by radical beam assisted molecular beam epitaxy and the optical properties were investigated. Zn(6N) was evaporated using Knudsen cell and O radical was assisted at the partial pressure of 1$\times$10$^{4}$ Torr and radical beam source of 250-450 W RF power. In $\theta$-2$\theta$ x-ray diffraction analysis, ZnO thin film with 500 nm thickness showed only ZnO(0002)and ZnO(0004) peaks is believed to be well grown along c-axis orientation. Photoluminescence (PL) measurement using He-Cd ($\lambda$=325 nm) laser is obtained in the temperature range of 9 K-300 K. At 9 K and 300 K, only near band edge (NBE) is observed and the FWHM's of PL peak of the ZnO deposited at 450 RF power are 45 meV and 145 meV respectively. From no observation of any weak deep level peak even at room temperature PL, the ZnO grains are regarded to contain very low defect density and impurity to cause the deep-level defects. The peak position of free exciton showed slightly red-shift as temperature was increased, and from this result the binding energy of free exciton can be experimentally determined as much as $58\pm$0.5 meV, which is very closed to that of ZnO bulk. By van der Pauw 4-point probe measurement, the grown ZnO is proved to be n-type with the electron concentration($n_{e}$ ) $1.69$\times$10^{18}$$cm^3$, mobility($\mu$) $-12.3\textrm{cm}^2$/Vㆍs, and resistivity($\rho$) 0.30 $\Omega$$\cdot$cm.

저 에너지 표면 개질 이온원이 설치된 진공 웹 공정을 이용한 2층 flexible copper clad laminate 제작

최형욱,박동희,최원국,Choi, Hyoung-Wook,Park, Dong-Hee,Choi, Won-Kook 한국재료학회 2007 한국재료학회지 Vol.17 No.10

In order to fabricate adhesiveless 2-layer flexible copper clad laminate (FCCL) used for COF (chip on film) with high peel strength, polyimide (PI; Kapton-EN, $38\;{\mu}m$) surface was modified by reactive $O_2^+$ and $N_2O^+$ ion beam irradiation. 300 mm-long linear electron-Hall drift ion source was used for ion irradiation with ion current density (J) higher than $0.5\;mA/cm^2$ and energy lower than 200 eV. By vacuum web coating process, PI surface was modified by linear ion source and then 10-20 nm thick Ni-Cr and 200 nm thick Cu film were in-situ sputtered as a tie layer and seed layer, respectively. Above this sputtered layer, another $8-9{\mu}m$ thick Cu layer was grown by electroplating and subsequently acid and base resistance and thermal stability were tested for examining the change of peel strength. Peel strength for the FCCLs treated by both $O_2^+$ and $N_2O^+$ ion irradiation showed similar magnitudes and increased as the thickness of tie layer increased. FCCL with Cu (200 nm)/Ni-Cr (20 nm)/PI structure irradiated with $N_2O^+$ at $1{\times}10^{16}/cm^2$ ion fluence was proved to have a strong peel strength of 0.73 kgf/cm for as-received and 0.34 kgf/cm after thermal test.

진공 웹코터로 제작된 대면적 ITO/PET의 특성 연구

김지환,박동희,김종빈,변동진,최원국,Kim, Ji-Hwan,Park, Dong-Hee,Kim, Jong-Bin,Byun, Dong-Jin,Choi, Won-Kook 한국재료학회 2007 한국재료학회지 Vol.17 No.10

Indium tin oxide, which is used as transparent conducting layer in flexible device, is deposited on PET film by a magnetron sputtering in 300 mm wide roll-to-roll process (vacuum web coating). Sheet resistance, specific resistance and transmittance is differed by sputtering parameters such as working pressures, oxygen partial pressure, and thickness of ITO layer. ITO layer is deposited about 90 nm at roll speed of 0.24 m/min and its sputtering power is 3 kW. From the XRD spectrum deposited ITO layer is verified as amorphous. Under working pressure varied from $3{\times}10^{-4}\;Torr$ to $2{\times}10^{-3}\;Torr$, sheet resistance is lowest at the working pressure of $1{\times}10^{-3}\;Torr$ and its value is from $110\;{\Omega}/{\square}$ to $260\;{\Omega}/{\square}$ at the thickness of 90 nm. Oxygen partial pressure also varies sheet resistance and is optimized at the regime from 0.2% ($1.8{\times}10^{-6}\;Torr$) to 0.6% ($6{\times}10^{-6}\;Torr$). In this oxygen partial pressure sheet resistance is lower than $150\;{\Omega}/{\square}$. As ITO layer thickness increases, sheet resistance decreases down to $21\;{\Omega}/{\square}$ and specific resistance is about $7.5{\times}10.4{\Omega}cm$ in 340 nm thickness ITO layer. Transmittance is measured at the wavelength of 550 nm and is about 90% for 180 nm thickness ITO/PET.

탄소 전극 형상 변화에 따른 전기화학 커패시터 특성 향상

민형섭,김상식,정덕수,최원국,오영제,이전국,Min, Hyung-Seob,Kim, Sang-Sig,Cheong, Deock-Soo,Choi, Won-Kook,Oh, Young-Jei,Lee, Jeon-Kook 한국재료학회 2009 한국재료학회지 Vol.19 No.10

Activated carbon (AC) with very large surface area has high capacitance per weight. However, such activation methods tend to suffer from low yields, below 50%, and are low in electrode density and capacitance per volume. Carbon NanoFibers (CNFs) had high surface area polarizability, high electrical conductivity and chemical stability, as well as extremely high mechanical strength and modulus, which make them an important material for electrochemical capacitors. The electrochemical properties of immobilized CNF electrodes were studied for use as in electrical double layer capacitor (EDLC) applications. Immobilized CNFs on Ni foam grown by thermal chemical vapor deposition (CVD) were successfully fabricated. CNFs had a uniform diameter range from 50 to 60 nm. Surface area was 56 m$^2$/g. CNF electrodes were compared with AC and multi wall carbon nanotube (MWNT) electrodes. The electrochemical performance of the various electrodes was examined with aqueous electrolyte of 2M KOH. Equivalent series resistance (ESR) of the CNF electrodes was lower than that of AC and MWNT electrodes. The specific capacitance of 47.5 F/g of the CNF electrodes was achieved with discharge current density of 1 mA/cm$^2$.

저온에서 Hydropolymer를 이용한 ZnO 나노입자 염료 감응형 태양전지

권병욱,손동익,박동희,양정도,최원국,Kwon, Byoung-Wook,Son, Dong-Ick,Park, Dong-Hee,Yang, Jeong-Do,Choi, Won-Kook 한국재료학회 2010 한국재료학회지 Vol.20 No.9

To fabricate $TiO_2$ nanoparticle-based dye sensitized solar cells (DSSCs) at a low-temperature, DSSCs were fabricated using hydropolymer and ZnO nanoparticles composites for the electron transport layer around a low-temperature ($200^{\circ}C$). ZnO nanoparticle with 20 nm and 60 nm diameter were used and Pt was deposited as a counter electrode on ITO/glass using an RF magnetron sputtering. We investigate the effect of ZnO nanoparticle concentration in hydropolymer and ZnO nanoparticle solution on the photoconversion performance of the low temperature fabricated ($200^{\circ}C$) DSSCs. Using cis-bis(isothiocyanato)bis(2,20 bipyridy1-4,40 dicarboxylato) ruthenium (II) bis-tetrabutylammonium (N719) dye as a sensitizer, the corresponding device performance and photo-physical characteristics are investigated through conventional physical characterization techniques. The effect of thickness of the ZnO photoelectrode and the morphology of the ZnO nanoparticles with the variations of hydropolymer to ZnO ratio on the photoconversion performance are also investigated. The morphology of the ZnO layer after sintering was examined using a field emission scanning electron microscope (FE-SEM). 60 nm ZnO nanoparticle DSSCs showed an incident photon-to-current conversion efficiency (IPCE) value of about 7% higher than that of 20 nm ZnO nanoparticle DSSCs. The maximum parameters of the short circuit current density ($J_{sc}$), the open circuit potential ($V_{oc}$), fill factor (ff), and efficiency ($\eta$) in the 60 nm ZnO nanoparticle-based DSSC devices were 4.93 mA/$cm^2$, 0.56V, 0.40, and 1.12%, respectively.

이온보조반응법으로 처리한 알루미나 코아의 인장결합강도에 관한 연구

김형섭,우이형,권긍록,최부병,최원국,Kim, Hyeong-Seob,Woo, Yi-Hyung,Kwon, Kung-Rock,Choi, Boo-Byung,Choi, Won-Kook 대한치과보철학회 2000 대한치과보철학회지 Vol.38 No.5

This study was undertaken to evaluate the tensile bond strength of In-Ceram alumina core treat-ed by ion assisted reaction(IAR). Ion assisted reaction is a prospective surface modification technique without damage by a keV low energy ion beam irradiation in reactive gas environments or reactive ion itself. 120 In-Ceram specimens were fabricated according to manufacturer's directions and divided into six groups by surface treatment methods of In-Ceram alumina core. SD group(control group): sandblasting SL group: sandblasting + silane treatment SC group: sandblasting + Siloc treatment IAR I group: sandblasting + Ion assisted reaction with argon ion and oxygen gas IAR II group: sandblasting + Ion assisted reaction with oxygen ion and oxygen gas IAR III group: sandblasting + Ion assisted reaction with oxygen ion only For measuring of tensile bond strength, pairs of specimens within a group were bonded with Panavia 21 resin cement using special device secured that the film thickness was $80{\mu}m$. The results of tensile strength were statistically analyzed with the SPSS release version 8.0 programs. Physical change like surface roughness of In-Ceram alumina core treated by ion assistad reaction was evaluated by Contact Angle Measurement, Scanning Electron Microscopy, Atomic Force Microscopy; chemical surface change was evaluated by X-ray Photoelectron Spectroscopy. The results as follows: 1. In tensile bond strength, there were no statistically significant differences with SC group, IAR groups and SL group except control group(P<0.05). 2. Contact angle measurement showed that wettability of In-Ceram alumina core was enhanced after IAR treatment. 3. SEM and AFM showed that surface roughness of In-Ceram alumina core was not changed after IAR treatment. 4. XPS showed that IAR treatment of In-Ceram alumina core was enabled to create a new functional layer. A keV IAR treatment of In-Ceram alumina core could enhanced tensile bond strength with resin cement. In the future, this ion assisted reaction may be used effectively in various dental materials as well as in In-Ceram to promote the bond strength to natural tooth structure.

RF 스퍼터링법으로 사파이어 기판 위에 성장한 ZnO와 ZnO : A1 박막의 질소 및 수소 후열처리에 따른 Photoluminescence 특성

조정,윤기현,정형진,최원국,Cho, Jung,Yoon, Ki-Hyun,Jung, Hyung-Jin,Choi, Won-Kook 한국재료학회 2001 한국재료학회지 Vol.11 No.10

2wt% $Al_2O_3-doped$ ZnO (AZO) thin films were deposited on sapphire (0001) single crystal substrate by parellel type rf magnetron sputtering at 55$0^{\circ}C$. The as-grown AZO thin films was polycrystalline and showed only broad deep defect-level photoluminescence (PL). In order to examine the change of PL property, AZO thin films were annealed in $N_2$ (N-AZO) and $H_2$ (H-AZO) at the temperature of $600^{\circ}C$~$1000^{\circ}C$ through rapid thermal annealing. After annealed at $800^{\circ}C$, N-AZO shows near band edge emission (NBE) with very small deep-level emission, and then N-AZO annealed at $900^{\circ}C$ shows only sharp NBE with 219 meV FWHM. In Comparison with N-AZO, H-AZO exhibits very interesting PL features. After $600^{\circ}C$ annealing, deep defect-level emission was quire quenched and NBE around 382 nm (3.2 eV) was observed, which can be explained by the $H_2$passivation effect. At elevated temperature, two interesting peaks corresponding to violet (406 nm, 3.05 eV) and blue (436 nm, 2.84 eV) emission was firstly observed in AZO thin films. Moreover, peculiar PL peak around 694 nm (1.78 eV) is also firstly observed in all the H-AZO thin films and this is believed good evidence of hydrogenation of AZO. Based on defect-level scheme calculated by using the full potential linear muffin-tin orbital (FP-LMTO), the emission 3.2 eV, 3.05 eV, 3.84 eV and 1.78 eV of H-AZO are substantially deginated as exciton emission, transition from conduction band maximum to $V_{ Zn},$ from $Zn_i$, to valence band maximum $(V_{BM})$ and from $V_{o} to V_BM}$, respectively.

초음파 열분해법를 이용한 ZnO 성장

김길영,정연식,변동진,최원국,Kim, Gil-Young,Jung, Yeon-Sik,Byun, Dong-Jin,Choi, Won-Kook 한국세라믹학회 2005 한국세라믹학회지 Vol.42 No.4

단결정 사파이어 (0001) 기판 위에 저가의 초산아연(Zinc Acetate Dehydrate; ZAH) 전구체를 이용하여 초음파 열분해법과 Ar 가스를 이용한 ZnO 박막을 성장시켰다. Thermogravimetry-Differential Scanning Calorimetry(TG-DSC) 초산아연의 열분해 과정을 조사하여 $380^{\circ}C$ 이상에서 ZnO로 분해되는 것을 확인하였다. $380-700^{\circ}C$에서 증착된 ZnO 박막은 모두 ZnO (002), (101) 결정면으로 부터의 회절피크를 보여주고 있었으며, $400^{\circ}C$ 박막의 경우 c-압축 스트레인 ${\Sigma}Z=0.2\%$, 압축 응력 $\sigma=-0.907\;GPa$이 작용하고 있음을 알 수 있었다. 전자 현미경을 이용한 미세 구조의 관찰을 통하여 $380-600^{\circ}C$에서는 초산아연과 ZnO 초미세 입자가 혼합된 aggregate 형태의 결정립을 형성하고 있었으며, nanoblade 형태의 미세구조를 보였다. 한편 $700^{\circ}C$에서 증착된 박막내의 결정립은 찌그러진 육방정계의 형태를 취하고 있으며, 10-25nm 정도의 부결정림 초미세 ZnO 입자로 이루어져 있음을 알 수 있었다. 초미세 입자의 형성을 임의 핵형성 기구(random nucleation mechanism)로 설명하였고, photoluminescence(PL) 측정을 통하여 광 특성을 조사하였다. ZnO was deposited on sapphire single crystal substrate by an ultrasonic pyrolysis of Zinc Acetate Dehydrate (ZAH) with carrying Ar gas. Through Thermogravimetry-Differential Scanning Calorimetry(TG-DSC), zinc acetate dihydrate was identified to be dissolved into ZnO above $380^{\circ}C$. ZnO deposited at $380-700^{\circ}C$ showed polycrystalline structures with ZnO (101) and ZnO (002) diffraction peaks like bulk ZnO in XRD, and from which c-axis strain ${\Sigma}Z=0.2\%$ and compressive biaxial stress$\sigma=-0.907\;GPa$ was obtained for the ZnO deposited $400^{\circ}C$. Scanning electron microscope revealed that microstructures of the ZnO were dependent on the deposition temperature. ZnO grown below temperature $600^{\circ}C$ were aggregate consisting of zinc acetate and ZnO particles shaped with nanoblades. On the other hand the grain of the ZnO deposited at $700^{\circ}C$ showed a distorted hexagonal shape and was composed of many ultrafine ZnO powers of 10-25 nm in size. The formation of these ulrafine nm scale ZnO powers was explained by the model of random nucleation mechanism. The optical property of the ZnO was analyzed by the photoluminescence (PL) measurement.