• Journal of Powder Materials
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• v.12 no.2 s.49
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• pp.117-121
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• 2005

Platinum catalysts for the DMFC (Direct Methanol Fuel Cell) were impregnated on several carbon supports and their catalytic activities were evaluated with cyclic voltammograms of methanol electro-oxidation. To increase the activities of the Pt/C catalyst, carbon supports with high electric conductivity such as mesoporous carbon, carbon nanofiber, and carbon nanotube were employed. The Pt/e-CNF (etched carbon nanofiber) catalyst showed higher maximum current density of $70 mA cm^{-2}$ and lower on-set voltage of 0.54 V vs. NHE than the Pt/Vulcan XC-72 in methanol oxidation. Although the carbon named by CNT (carbon nanotube) series turned out to have larger BET surface area than the carbon named by CNF (carbon nanofiber) series, the Pt catalysts supported on the CNT series were less active than those on the CNF series due to their lower electric conductivity and lower availability of pores for Pt loading. Considering that the BET surface area and electric conductivity of the e-CNF were similar to those of the Vulcan XC-72, smaller Pt particle size of the Pt/e-CNF catalyst and stronger metal-support interaction were believed to be the main reason for its higher catalytic activity.

• Journal of the Korean institute of surface engineering
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• v.38 no.2
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• pp.65-68
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• 2005

The effect of crystal orientation and microstructure on the mechanical properties of $TaN_x$ was investigated. $TaN_x$ films were grown on $SiO_2$ substrates by ultrahigh vacuum unbalanced magnetron sputter deposition in mixed $Ar/N_2$ discharges at 20 mTorr (2.67 Pa) and at $350^{\circ}C$. Unlike the Ti-N system, in which TiN is the terminal phase, a large number of N-rich phases in the Ta-N system could lead to layers which had nano-sized lamella structure of coherent cubic and hexagonal phases, with a correct choice of nitrogen fraction in the sputtering mixture and ion irradiation energy during growth. The preferred orientations and the micro-structure of $TaN_x$ layers were controlled by varing incident ion energy $E_i\;(=30eV\~50eV)$ and nitrogen fractions $f_{N2}\;(=0.1\~0.15)$. $TaN_x$ layers were grown on (0002)-Ti underlayer as a crystallographic template in order to relieve the stress on the films. The structure of the $TaN_x$ film transformed from Bl-NaCl $\delta-TaN_x$ to lamellar structured Bl-NaCl $\delta-TaN_x$ + hexagonal $\varepsilon-TaN_x$ or Bl-NaCl $\delta-TaN_x$ + hexagonal $\gamma-TaN_x$ with increasing the ion energy at the same nitrogen fraction $f_{N2}$. The hardness of the films also increased by the structural change. At the nitrogen fraction of $0.1\~0.125$, the structure of the $TaN_x$ films was changed from $\delta-TaN_x\;+\;\varepsilon-TaN_x\;to\;\delta-TaN_x\;+\;\gamma-TaN_x$ with increasing the ion energy. However, at the nitrogen fraction of 0.15 the film structure did not change from $\delta-TaN_x\;+\;\varepsilon-TaN_x$ over the whole range of the applied ion energy. The hardness increased significantly from 21.1 GPa to 45.5 GPa with increasing the ion energy.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.100-101
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• 2012

The plasma damage free and room temperature processedthin film deposition technology is essential for realization of various next generation organic microelectronic devices such as flexible AMOLED display, flexible OLED lighting, and organic photovoltaic cells because characteristics of fragile organic materials in the plasma process and low glass transition temperatures (Tg) of polymer substrate. In case of directly deposition of metal oxide thin films (including transparent conductive oxide (TCO) and amorphous oxide semiconductor (AOS)) on the organic layers, plasma damages against to the organic materials is fatal. This damage is believed to be originated mainly from high energy energetic particles during the sputtering process such as negative oxygen ions, reflected neutrals by reflection of plasma background gas at the target surface, sputtered atoms, bulk plasma ions, and secondary electrons. To solve this problem, we developed the NBAS (Neutral Beam Assisted Sputtering) process as a plasma damage free and room temperature processed sputtering technology. As a result, electro-optical properties of NBAS processed ITO thin film showed resistivity of $4.0{\times}10^{-4}{\Omega}{\cdot}m$ and high transmittance (>90% at 550 nm) with nano- crystalline structure at room temperature process. Furthermore, in the experiment result of directly deposition of TCO top anode on the inverted structure OLED cell, it is verified that NBAS TCO deposition process does not damages to the underlying organic layers. In case of deposition of transparent conductive oxide (TCO) thin film on the plastic polymer substrate, the room temperature processed sputtering coating of high quality TCO thin film is required. During the sputtering process with higher density plasma, the energetic particles contribute self supplying of activation & crystallization energy without any additional heating and post-annealing and forminga high quality TCO thin film. However, negative oxygen ions which generated from sputteringtarget surface by electron attachment are accelerated to high energy by induced cathode self-bias. Thus the high energy negative oxygen ions can lead to critical physical bombardment damages to forming oxide thin film and this effect does not recover in room temperature process without post thermal annealing. To salve the inherent limitation of plasma sputtering, we have been developed the Magnetic Field Shielded Sputtering (MFSS) process as the high quality oxide thin film deposition process at room temperature. The MFSS process is effectively eliminate or suppress the negative oxygen ions bombardment damage by the plasma limiter which composed permanent magnet array. As a result, electro-optical properties of MFSS processed ITO thin film (resistivity $3.9{\times}10^{-4}{\Omega}{\cdot}cm$, transmittance 95% at 550 nm) have approachedthose of a high temperature DC magnetron sputtering (DMS) ITO thin film were. Also, AOS (a-IGZO) TFTs fabricated by MFSS process without higher temperature post annealing showed very comparable electrical performance with those by DMS process with $400^{\circ}C$ post annealing. They are important to note that the bombardment of a negative oxygen ion which is accelerated by dc self-bias during rf sputtering could degrade the electrical performance of ITO electrodes and a-IGZO TFTs. Finally, we found that reduction of damage from the high energy negative oxygen ions bombardment drives improvement of crystalline structure in the ITO thin film and suppression of the sub-gab states in a-IGZO semiconductor thin film. For realization of organic flexible electronic devices based on plastic substrates, gas barrier coatings are required to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency flexible AMOLEDs needs an extremely low water vapor transition rate (WVTR) of $1{\times}10^{-6}gm^{-2}day^{-1}$. The key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required (under ${\sim}10^{-6}gm^{-2}day^{-1}$) is the suppression of nano-sized defect sites and gas diffusion pathways among the grain boundaries. For formation of high quality single inorganic gas barrier layer, we developed high density nano-structured Al2O3 single gas barrier layer usinga NBAS process. The NBAS process can continuously change crystalline structures from an amorphous phase to a nano- crystalline phase with various grain sizes in a single inorganic thin film. As a result, the water vapor transmission rates (WVTR) of the NBAS processed $Al_2O_3$ gas barrier film have improved order of magnitude compared with that of conventional $Al_2O_3$ layers made by the RF magnetron sputteringprocess under the same sputtering conditions; the WVTR of the NBAS processed $Al_2O_3$ gas barrier film was about $5{\times}10^{-6}g/m^2/day$ by just single layer.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.356-356
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• 2010

Tribological behaviors of the hard film on soft substrate system were explored using the hard thin film of diamond-like carbon (DLC) coated the soft polymer of polydimethysiloxane (PDMS). A DLC film with the Young's modulus of 100 GPa was coated on PDMS substrate with Young's modulus of 10 MPa using plasma enhanced chemical vapor deposition (PECVD) technique. The deposition time was varied from 10 sec to 10 min, resulting in nanoscale roughness of wrinkle patterns with the thickness of 20 nm to 510 nm, respectively, at a bias voltage of $400\;V_b$, working pressure 10 mTorr. Nanoscale wrinkle patterns with 20-100 nm in width and 10-30 nm height were formed on DLC coating due to the residual stress in compression and difference in Young's modulus. Nanoscale roughness effect on tribological behaviors was observed by performing a tribo-experiment using the ball-on-disk type tribometer with a steel ball of 6 mm in diameter at the sliding speed of 220 rpm, normal load of 1N and 25% humidity at ambient temperature of $25^{\circ}C$. Friction force were measured with respect to thickness change of coated DLC thin film on PDMS. It was found that with increases the thickness of DLC coating on PDMS, the coefficient of friction decreased by comparison to that of the uncoated PDMS. The wear tracks before and after tribo-test were analyzed using SEM and AFM.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.25 no.8
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• pp.664-669
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• 2012

Nano-structured one-dimensional $Na_2Ti_6O_{13}$ particles were synthesized by a molten salt process. Effects of processing parameters on the microstructure and band gap energy of the $Na_2Ti_6O_{13}$ powder were studied in this paper. For the synthesis of the $Na_2Ti_6O_{13}$ particles, two different raw materials of tubular shaped Na-titanate (Na-TiNT) and spherical shaped $TiO_2$ were utilized. Synthesizing with the raw material of Na-TiNT, around 70nm thick 1D-$Na_2Ti_6O_{13}$ with the bandgap energy of 3.5 eV was obtained at $810^{\circ}C$. Below $810^{\circ}C$ or without the presence of NaCl, 1D-$Na_2Ti_6O_{13}$ was in a relatively short in length and agglomerated state. With the processing temperature increased, the thickness of the 1D-$Na_2Ti_6O_{13}$ was also observed to be increased. On the other hand, when $TiO_2$ was employed as a raw material, the mixed amount of $Na_2CO_3$ played an important role in transforming the morphology and phase of the raw material, affecting the bandgap energy of the synthesized product. Specific surface area of the synthesized 1D-$Na_2Ti_6O_{13}$ was significantly affected by the raw and mixed materials as well as processing temperature. When Na-TiNT was processed at $810^{\circ}C$ with NaCl, the specific surface area of the 1D-$Na_2Ti_6O_{13}$ showed the best value of 30.63 $m^2/g$.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.6
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• pp.547-554
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• 2010

In this study, new manganese oxide (i.e., black-birnessite) particles with nanostructures were prepared and its physico-chemical properties and oxidative-transformation efficiency on 1,4-naphthoquinine(1,4-NPQ) in the presence of reactive mediator was investigated. The results were also compared with that of the manganese oxide (i.e., brown-birnessite) particles synthesized by classical McKenzie method. Analysis of XRD and SEM data show that the particles are a single phase corresponding to a birnessite-based manganese oxide with cotton ball-like shapes containing nanofibers. In batch experiments, removals of 1,4-NPQ by the black-birnessite follows pseudo-first-order kinetics and the rate constant values obtained are greater about 2.3 times than that of the brown-birnessite in spite of its lower surface area (41.0 vs 19.80 $m^2/g$). The results can be explained by the higher crystallinity and nano structured features of the back-birnessite particles, which give higher reactivity for the removals of the quinone compound. HPLC analysis of the reaction products confirmed that the balck-birnessites removed 1,4-NPQ through cross-coupling reaction in the presence of catechol as a reactive mediator.

• Korean Chemical Engineering Research
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• v.43 no.4
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• pp.517-524
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• 2005

Barium titanate ($BaTiO_3$) particles were prepared by spray pyrolysis from spray solution containing organic additives. The effects of the type and amount of organic precursors on the crystal structure and morphology of the $BaTiO_3$ particles were investigated. It was found that the morphology of $BaTiO_3$ particles before and after calcination depended on the type of organic additives such as citric acid, ethylene glycol and polyethylene glycol. Among these organic additives, citric acid was the most effective to prepare $BaTiO_3$ particles with nano-structured morphology consisting with uniform size nanometer particles after calcination. It was also found that the phase transformability of the metastable cubic phase to the tetragonal one during calcination could be improved by increasing the content of citric acid in the spray solution. As a result, $BaTiO_3$ particles prepared from spray solution containing high concentration of citric acid had good tetragonality, uniform and fine size, and high BET surface area after calcination. $BaTiO_3$ particles prepared by spray pyrolysis had nanometer size and uniform morphology after simple ball milling process.