• The Journal of Korean Academy of Prosthodontics
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• v.45 no.1
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• pp.85-97
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• 2007

Statement of problem: Recently, anodic oxidation of cp-titanium is a popular method for treatment of titanium implant surfaces. It is a relatively easy process, and the thickness, structure, composition, and the microstructure of the oxide layer can be variably modified. Moreover the biological properties of the oxide layer can be controlled. Purpose: In this study, the roughness, microstructure, crystal structure of the variously treated groups (current, voltage, frequency, electrolyte, thermal treatment) were evaluated. And the specimens were soaked in simulated body fluid (SBF) to evaluate the effects of the surface characteristics and the oxide layers on the bioactivity of the specimens which were directly related to bone formation and integration. Materials and methods: Surface treatments consisted of either anodization or anodization followed thermal treatment. Specimens were divided into seven groups, depending on their anodizing treatment conditions: constant current mode (350V for group 2), constant voltage mode (155V for group 3), 60 Hz pulse series (230V for group 4, 300V for group 5), and 1000 Hz pulse series (400V for group 6, 460V for group 7). Non-treated native surfaces were used as controls (group 1). In addition, for the purpose of evaluating the effects of thermal treatment, each group was heat treated by elevating the temperature by $5^{\circ}C$ per minute until $600^{\circ}C$ for 1 hour, and then bench cured. Using scanning electron microscope (SEM), porous oxide layers were observed on treated surfaces. The crystal structures and phases of titania were identified by thin-film x-ray diffractmeter (TF-XRD). Atomic force microscope (AFM) was used for roughness measurement (Sa, Sq). To evaluate bioactivity of modified titanium surfaces, each group was soaked in SBF for 168 hours (1 week), and then changed surface characteristics were analyzed by SEM and TF-XRD. Results: On basis of our findings, we concluded the following results. 1. Most groups showed morphologically porous structures. Except group 2, all groups showed fine to coarse convex structures, and the groups with superior quantity of oxide products showed superior morphology. 2. As a result of combined anodization and thermal treatment, there were no effects on composition of crystalline structure. But, heat treatment influenced the quantity of formation of the oxide products (rutile / anatase). 3. Roughness decreased in the order of groups 7,5,2,3,6,4,1 and there was statistical difference between group 7 and the others (p<0.05), but group 7 did not show any bioactivity within a week. 4. In groups that implanted ions (Ca/P) on the oxide layer through current and voltage control, showed superior morphology, and oxide products, but did not express any bioactivity within a week. 5. In group 3, the oxide layer was uniformly organized with rutile, with almost no titanium peak. And there were abnormally more [101] orientations of rutile crystalline structure, and bonelike apatite formation could be seen around these crystalline structures. Conclusion: As a result of control of various factors in anodization (current, voltage, frequency, electrolytes, thermal treatment), the surface morphology, micro-porosity, the 2nd phase formation, crystalline structure, thickness of the oxide layer could be modified. And even more, the bioactivity of the specimens in vitro could be induced. Thus anodic oxidation can be considered as an excellent surface treatment method that will able to not only control the physical properties but enhance the biological characteristics of the oxide layer. Furthermore, it is recommended in near future animal research to prove these results.

• Korean Journal of Materials Research
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• v.5 no.1
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• pp.42-54
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• 1995

$Ta_2O_5$ thin film IS a promising material for the high dielectrics of ULSI DRAM. In this study, $Ta_2O_5$ thin film was grown on p-type( 100) Si wafer by thermal metal organic chemical vapo deposition ( MCCVD) method and the effect of operating varialbles including substrate temperature( $T_s$), bubbler temperature( $T_ \sigma$), reactor pressure( P ) was investigated in detail. $Ta_2O_5$ thin film were analyzed by SEM, XRD, XPS, FT-IR, AES, TEM and AFM. In addition, the effect of various anneal methods was examined and compared. Anneal methods were furnace annealing( FA) and rapid thermal annealing( RTA) in $N_{2}$ or $O_{2}$ ambients. Growth rate was evidently classified into two different regimes. : (1) surface reaction rate-limited reglme in the range of $T_s$=300 ~ $400 ^{\circ}C$ and (2: mass transport-limited regime in the range of $T_s$=400 ~ $450^{\circ}C$.It was found that the effective activation energies were 18.46kcal/mol and 1.9kcal/mol, respectively. As the bubbler temperature increases, the growth rate became maximum at $T_ \sigma$=$140^{\circ}C$. With increasing pressure, the growth rate became maximum at P=3torr but the refractive index which is close to the bulk value of 2.1 was obtained in the range of 0.1 ~ 1 torr. Good step coverage of 85. 71% was obtained at $T_s$=$400 ^{\circ}C$ and sticking coefficient was 0.06 by comparison with Monte Carlo simulation result. From the results of AES, FT-IR and E M , the degree of SiO, formation at the interface between Si and TazO, was larger in the order of FA-$O_{2}$ > RTA-$O_{2}$, FA-$N_{2}$ > RTA-$N_{2}$. However, the $N_{2}$ ambient annealing resulted in more severe Weficiency in the $Ta_2O_5$ thin film than the TEX>$O_{2}$ ambient.

• KSBB Journal
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• v.15 no.4
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• pp.331-336
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• 2000

The antimutagenic activity of the extract of Artemisia capillaris THUNB on the mutagenicity induced by benzo(a)pyrene [B(a)P] in the presense of S9 mixture was studied using bacterial mutagenic assay system. Samples harvested in summer and autumn were extracted using ethanol and hot water. Among these extracts the water extract of summer sample had the strongest inhibitory effect against the mutagenenicity of B(a)P, The water extract of Artemisia capillaris THUNB was separated again into ethanol soluble and insoluble parts. The ethanol insoluble part(El) of water extract exhibited higher inhibition effects than the ethanol soluble part against the mutagenic activity of B(a)P. El showed dose-dependent activity on the mutagenicity of B(a)P in SOS Chromotest and Ames test. The 50% inbibition concentraction $(IC_{50}$ of El were $200{\mu}g/assay$ $600{\mu}g/plate$ and $800{\mu}b/plate$ in E. coil PQ37 S. typhimurium TA100 and TA98 respectively. El were showed desmutagenic effect but had no effect on the DNA repair system for B(a)P-induced mutagenesis. HPLC analysis showed that the formation of aflatoxin M1 by cytochrome P-450 1A1 known as playing an impotant role on B(a) P-induced mutagenicity was highly inhibited by El. Therefore we encluded that B(a)P-induced mutagencity can be reduced possible due to the interference of el with cytochrome P-450 1A1-dependent bioactivation.

• Journal of the Korean Vacuum Society
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• v.20 no.1
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• pp.7-13
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• 2011

[ $L1_0$ ]phase FePd nano-dot structures were successfully fabricated on self-organized Fe/Au bilayers. With atomic force microscopy, it is determined that surface morphologies of initially flat Fe/Au bilayer films were agglomerated and transformed their shape into nano-dots structures with increasing annealing temperature. With this bilayer as a template, FePd multilayers were deposited at various temperatures, i.e. $300^{\circ}C$, $350^{\circ}C$, $400^{\circ}C$, and $450^{\circ}C$. Surface morphologies of FePd superlattice had a near resemblance to self-organized bilayer. According to X-ray diffraction results, it is confirmed that $L1_0$ superlattice structures of FePd were obtained from samples which were annealed above $350^{\circ}C$. Results of X-ray photoelectron spectroscopy depth-profile analysis showed that chemical composition is identical to deposition sequence. As a result, without additional etching processes, fabrication of chemically ordered FePd superlattice nano-dots was achieved.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.21 no.8
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• pp.222-227
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• 2020

Pb(Zr,Ti)O₃(denoted as PZT) in the perovskite phase is used as a dielectric, piezoelectric, and super appetizer material owing to its ferroelectric properties. A PZT film was formed by an RF magnetron sputtering process by preparing a target composed of Pb_1.3(Zr_0.52Ti_0.48)O₃. The PZT film was formed by dividing the material into a mono-layer PZT produced continuously with the same sputtering power and a bi-layer PZT produced with two-stage sputtering power. The bi-layer PZT consisted of a lower layer produced under low-power sputtering conditions and an upper layer produced under the same conditions as the mono-layer PZT. XRD revealed small amounts of pyrochlore phase in the mono-layer PZT, but only the perovskite phase was detected in the bi-layer PZT. SEM and AFM revealed the upper part of the bi-layer PZT to be more compact and smooth. Moreover, the bi-layered PZT showed superior symmetry polarization and a significantly reduced leakage current of less than 1×10-5 A/cm². This phenomenon observed in bi-layer PZT was attributed to the induction of growth into a pure perovskite phase by suppressing the formation of a pyrochlore phase in the upper PZT layer where the densely formed lower PZT layer was produced sequentially.

• Korean Chemical Engineering Research
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• v.43 no.4
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• pp.495-502
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• 2005

Copper was plated on the tungsten substrate by use of a direct copper electroless plating. The optimum deposition conditions were found to be with a concentration of $CuSO_4$ 7.615 g/L, EDTA of 10.258 g/L, and glyoxylic acid of 7 g/L, respectively. The solution temperature was maintained at $60^{\circ}C$. The pH was varied from 11.0 to 12.8. After the deposition, the properties of the copper film were investigated with X-ray diffractometer (XRD), Field emission secondary electron microscope (FESEM), Atomic force microscope (AFM), X-ray photoelectron spectroscope (XPS), and Rutherford backscattering spectroscope (RBS). The best deposition condition was founded to be the solution pH of 11.8. In the case of 10 min deposition at the pH of 11.8, the grain shape was spherical, Cu phase was pure without impurity peak ($Cu_2O$ peak), and the surface root mean square roughness was about 11 nm. The thickness of the film turned out to be 140 nm after deposition for 12 min and the deposition rate was found to be about 12 nm/min. Increase in pH induced a formation of $Cu_2O$ phase with a long rectangular grain shape. The pH control seems to play an important role for the orientation of Cu in electroless deposition. The deposited copper concentration was 99 atomic percent according to RBS. The resulting Cu/W film yielded a good adhesive strength, because Cu/W alloy forms during electroless deposition.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.409-409
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• 2014

Recently hexagonal boron nitride (h-BN), III-V compound of boron and nitrogen with strong covalent $sp^2$ bond, is a 2 dimensional insulating material with a large direct band gap up to 6 eV. Its outstanding properties such as strong mechanical strength, high thermal conductivity, and chemical stability have been reported to be similar or superior to graphene. Because of these excellent properties, h-BN can potentially be used for variety of applications such as dielectric layer, deep UV optoelectronic device, and protective transparent substrate. Ultra flat and charge impurity-free surface of h-BN is also an ideal substrate to maintain electrical properties of 2 dimensional materials such as graphene. To synthesize a single or a few layered h-BN, chemical vapor deposition method (CVD) has been widely used by using an ammonia borane as a precursor. Ammonia borane decomposes into hydrogen (gas), monomeric aminoborane (solid), and borazine (gas) that is used for growing h-BN layer. However, very active monomeric aminoborane forms polymeric aminoborane nanoparticles that are white non-crystalline BN nanoparticles of 50~100 nm in diameter. The presence of these BN nanoparticles following the synthesis has been hampering the implementation of h-BN to various applications. Therefore, it is quite important to grow a clean and high quality h-BN layer free of BN particles without having to introduce complicated process steps. We have demonstrated a synthesis of a high quality h-BN monolayer free of BN nanoparticles in wafer-scale size of $7{\times}7cm^2$ by using CVD method incorporating a simple filter system. The measured results have shown that the filter can effectively remove BN nanoparticles by restricting them from reaching to Cu substrate. Layer thickness of about 0.48 nm measured by AFM, a Raman shift of $1,371{\sim}1,372cm^{-1}$ measured by micro Raman spectroscopy along with optical band gap of 6.06 eV estimated from UV-Vis Spectrophotometer confirm the formation of monolayer h-BN. Quantitative XPS analysis for the ratio of boron and nitrogen and CS-corrected HRTEM image of atomic resolution hexagonal lattices indicate a high quality stoichiometric h-BN. The method presented here provides a promising technique for the synthesis of high quality monolayer h-BN free of BN nanoparticles.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.477-477
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• 2008

For more than three decades, the gate dielectrics in CMOS devices are $SiO_2$ because of its blocking properties of current in insulated gate FET channels. As the dimensions of feature size have been scaled down (width and the thickness is reduced down to 50 urn and 2 urn or less), gate leakage current is increased and reliability of $SiO_2$ is reduced. Many metal oxides such as $TiO_2$, $Ta_2O_4$, $SrTiO_3$, $Al_2O_3$, $HfO_2$ and $ZrO_2$ have been challenged for memory devices. These materials posses relatively high dielectric constant, but $HfO_2$ and $Al_2O_3$ did not provide sufficient advantages over $SiO_2$ or $Si_3N_4$ because of reaction with Si substrate. Recently, $HfO_2$ have been attracted attention because Hf forms the most stable oxide with the highest heat of formation. In addition, Hf can reduce the native oxide layer by creating $HfO_2$. However, new gate oxide candidates must satisfy a standard CMOS process. In order to fabricate high density memories with small feature size, the plasma etch process should be developed by well understanding and optimizing plasma behaviors. Therefore, it is necessary that the etch behavior of $HfO_2$ and plasma parameters are systematically investigated as functions of process parameters including gas mixing ratio, rf power, pressure and temperature to determine the mechanism of plasma induced damage. However, there is few studies on the the etch mechanism and the surface reactions in $BCl_3$ based plasma to etch $HfO_2$ thin films. In this work, the samples of $HfO_2$ were prepared on Si wafer with using atomic layer deposition. In our previous work, the maximum etch rate of $BCl_3$/Ar were obtained 20% $BCl_3$/ 80% Ar. Over 20% $BCl_3$ addition, the etch rate of $HfO_2$ decreased. The etching rate of $HfO_2$ and selectivity of $HfO_2$ to Si were investigated with using in inductively coupled plasma etching system (ICP) and $BCl_3/Cl_2$/Ar plasma. The change of volume densities of radical and atoms were monitored with using optical emission spectroscopy analysis (OES). The variations of components of etched surfaces for $HfO_2$ was investigated with using x-ray photo electron spectroscopy (XPS). In order to investigate the accumulation of etch by products during etch process, the exposed surface of $HfO_2$ in $BCl_3/Cl_2$/Ar plasma was compared with surface of as-doped $HfO_2$ and all the surfaces of samples were examined with field emission scanning electron microscopy and atomic force microscope (AFM).

• Membrane Journal
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• v.16 no.4
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• pp.294-302
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• 2006

Silver polymer electrolytes are very promising membrane materials for the separation of olefin/paraffn mixtures. Olefin molecules are known to be transported through reversible complex formation with silver ions entrapped iii polymer matrix. However, they have poor long-term stability, which is very important fur the industrial application; the selectivity through the membrane decreases gradually with time mostly due to the reduction of silver ions ($Ag^+$) into silver nanoparticles ($Ag^0$). In this study, the stability of silver polymer electrolyte was investigated for poly(vinyl pyrrolidone) (PVP) and $AgBF_4$ system containing a surfactant, i.e. $C_{18}H_{35}(OCH_2CH_2)_{20}OH$ (Brij98) as a stabilizer. The reduction behavior of silver ions to silver nanoparticles in PVP was also investigated by atomic force microscopy (AFM) and UV-visible spectroscopy. It was found that the growth of silver nanoparticles was slower and selectivity of polymer electrolyte for propylene in propylene/propane was maintained longer time when Brij98 was added as a stabilizer.

• Journal of the Korean Vacuum Society
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• v.22 no.6
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• pp.313-320
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• 2013

The $AlAs_xSb_{1-x}$ step-graded buffer (SGB) layer was grown on the Silicon (Si) substrate to overcome lattice mismatch between Si substrate and $Al_{0.3}Ga_{0.7}As$/GaAs multiple quantum wells (MQWs). The value of root-mean-square (RMS) surface roughness for 5 nm-thick GaAs grown on $AlAs_xSb_{1-x}$ step-graded buffer layer was ~1.7 nm. $Al_{0.3}Ga_{0.7}As$/GaAs MQWs with AlAs/GaAs short period superlattice (SPS) were formed on the $AlAs_xSb_{1-x}$/Si substrate. Photoluminescence (PL) peak at 10 K for the $Al_{0.3}Ga_{0.7}As$/GaAs MQW structure showed relatively low intensity at ~813 nm. The RMS surface roughness of the $Al_{0.3}Ga_{0.7}As$/GaAs MQW structure was ~42.9 nm. The crystal defects were observed on the cross-sectional transmission electron microscope (TEM) images of the $Al_{0.3}Ga_{0.7}As$/GaAs MQW structure. The decrease of PL intensity and increase of RMS surface roughness would be due to the formation of the crystal defects.