• Korean Chemical Engineering Research
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• 제46권1호
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• pp.99-105
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• 2008

본 연구에서는 MLCC용 $BaTiO_3$에 첨가되는 $Cr_2O_3$와 $Mn_2O_3$의 나노코팅에 의한 core-shell 구조의 $BaTiO_3$ 분말을 제조하였다. 예비실험을 통해서 $KMnO_4$ 및 $K_2Cr_2O_4$ 그리고 sulfur를 사용하는 최적의 액상반응조건이 확립되었다. 본 연구에서는 두 첨가제 분말을 합성하였고 동일한 반응조건으로 두 첨가제를 $BaTiO_3$ 분말표면에 코팅하였다. 코팅은 one-step과 two-step의 두 방법으로 구분하여 시행하였고 그 결과를 분석 비교하였다. 결론적으로 말해서, $Cr_2O_3$와 $Mn_2O_3$의 두 첨가제는 용이한 반응조건에서 높은 수율로 우수한 품질의 코팅막을 형성하므로써, 첨가제 함량과 코팅막 특성의 정밀한 조절이 용이함을 보여주었다.

• 한국분말재료학회지
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• 제12권2호
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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.

• 한국표면공학회지
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• 제38권2호
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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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2009년도 제38회 동계학술대회 초록집
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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.

• 한국전기전자재료학회논문지
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• 제25권8호
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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 $m^2/g$.

• 대한환경공학회지
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• 제32권6호
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• pp.547-554
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• 2010

본 연구에서는 나노구조의 새로운 망간산화물 입자(즉, 블랙-버네사이트)를 합성하여 물질특성 및 1,4-naphthoquinone (1,4-NPQ)을 대상으로 반응매개체 존재 하에서의 산화-변환반응 효율을 조사하였고, 그 결과를 기존의 McKenzie 방법으로 얻은 망간산화물(즉, 브라운-버네사이트)의 결과와 비교 분석하였다. XRD 분석 결과 합성한 망간산화물 입자의 결정상은 버네사이트(${\delta}-MnO_2$)임을 확인하였으며, SEM 측정결과 입자표면은 섬유상의 구조에 의한 나노크기의 미세기공을 가진 볼모양(ball-like)의 형태를 보였다. 배치실험 결과, 나노구조의 망간산화물에 의한 1,4-NPQ 제거는 유사-1차 반응을 따랐으며 기존 망간산화물과 비교해 BET 비표면적 값이 작음(41.05 vs 19.80 $m^2/g$)에도 불구하고 약 2.3배의 높은 속도 상수값을 보였다. 이러한 결과는 블랙-버네사이트에서의 상대적으로 높은 결정성과 나노구조의 표면 특성에 기인한 것으로 해석되며, 블랙-버네사이트 입자가 퀴논화합물에 대하여 상대적으로 높은 반응성을 보임을 알 수 있다. 반응산물에 대한 HPLC 크로마토그램 분석 결과로부터 블랙 버네사이트 입자에 의한 1,4-NPQ의 제거는 반응 매개체인 catechol 존재 하에서의 상호-결합반응을 통한 중합체 생성을 통해 제거됨을 확인하였다.

• Korean Chemical Engineering Research
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• 제43권4호
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• pp.517-524
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• 2005

유기 첨가물을 함유하는 분무용액으로부터 분무열분해 공정에 의해 바륨 티타네이트($BaTiO_3$) 분말을 합성하였다. 분무용액에 첨가되는 유기물의 종류 및 첨가량이 분무열분해 공정에 의해 합성된 $BaTiO_3$ 분말들의 결정구조 및 형태 특성에 미치는 영향을 조사하였다. 유기 첨가물로서 구연산, 에틸렌 글리콜 및 폴리에틸렌 글리콜을 첨가한 경우에 있어서는 유기 첨가물의 종류에 따라 하소 전후에 서로 다른 형태의 $BaTiO_3$ 분말들이 얻어졌다. 분무용액에 구연산을 첨가한 경우에 합성된 $BaTiO_3$ 분말들은 하소 후에 균일한 크기의 나노 분말들로 구성 되어진 나노 구조체를 가졌다. 분무용액에 첨가된 구연산의 양이 증가할수록 하소 후에 얻어진 분말들의 결정구조가 준안정상인 입방정상에서 정방정상으로의 상변환성이 증가하였다. 고농도의 구연산을 함유한 분무용액으로부터 합성된 $BaTiO_3$ 분말들은 하소 후에 좋은 정방정계 결정구조, 균일하며 미세한 크기 및 고표면적을 가졌다. 분무열분해 공정에 의해 합성된 $BaTiO_3$ 분말들은 밀링 공정 후에 균일한 크기 및 형태를 가졌다.