• Design & Manufacturing
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• v.15 no.3
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• pp.7-12
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• 2021

Plastic injection molds used for rapid heating and cooling must minimize surface damage due to friction and maintain excellent thermal and low electrical conductivity. Accordingly, various surface treatments are being applied. The properties of Al₂O₃ coating and DLC coating were compared to find the optimal surface treatment method. Al₂O₃ coating was deposited by thermal spray method. DLC films were deposited by sputtering process in room temperature and high temperature PECVD (Plasma enhanced chemical vapor deposition) process in 723 K temperature. For the evaluation of physical properties, the electrical and thermal conductivity including surface hardness, adhesion and wear resistance were analyzed. The electrical resistance of the all coated samples was showed insulation properties of 24 MΩ/sq or more. Especially, the friction coefficient of high temp. DLC coating was the lowest at 0.134.

• 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.

• Applied Chemistry for Engineering
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• v.28 no.1
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• pp.1-7
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• 2017

Polydimethylsiloxane (PDMS) can be deposited on various substrates using chemical vapor deposition process, which results in the formation of PDMS thin films with thickness below 5 nm. PDMS layers can be evenly deposited on surfaces of nanoparticles composed of various chemical compositions such as $SiO_2$, $TiO_2$, ZnO, C, Ni, and NiO, and the PDMS-coated surface becomes completely hydrophobic. These hydrophobic layers are highly resistant towards degradation under acidic and basic environments and UV-exposures. Nanoparticles coated with PDMS can be used in various environmental applications: hydrophobic silica nanoparticles can selectively interact with oil from oil/water mixture, suppressing fast diffusion of spill-oil on water and allowing more facile physical separation of spill-oil from the water. Upon heat-treatments of PDMS-coated $TiO_2$ under vacuum conditions, $TiO_2$ surface becomes completely hydrophilic, accompanying formation oxygen vacancies responsible for visible-light absorption. The post-annealed $PDMS-TiO_2$ shows enhanced photocatalytic activity with respect to the bare $TiO_2$ for decomposition of organic dyes in water under visible light illumination. We show that the simple PDMS-coating process presented here can be useful in a variety of field of environmental science and technology.

• The korean journal of orthodontics
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• v.36 no.6
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• pp.451-464
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• 2006

The purpose of this study was to search for an appropriate method of coating $TiO_2$ on orthodontic appliances. $TiO_2$ thin films were deposited on orthodontic wires and brackets using sol-gel, CVD (Chemical Vapor Deposition) and PE-CVD (Plasma Enhanced-CVD) methods. The roughness of $TiO_2$-coated surfaces was investigated via scanning electron microscope (SEM) and adhesive strength of $TiO_2$ thin films was measured by adhesive tape pull test. Methylene blue degradation test was carried out to evaluate the photocatalytic activity of $TiO_2$ and the corrosion resistance of $TiO_2$ thin films against fluoride solution was also analyzed by observing the surfaces of $TiO_2$-coated wires and brackets via SEM after immersion in sodium fluoride solution. Through the comparison of properties and photocatalytic activity of $TiO_2$ thin films according to the coating methods, the following results were obtained. Smoother surfaces of $TiO_2$ thin films were generated by CVD or PE-CVD methods than through the sol-gel method or the control. Adhesive strength of the $TiO_2$ thin films was highest in PE-CVD and gradually became lower in the order of CVD, then the sol-gel method. Photocatalytic activity of $TiO_2$ thin films on methylene blue was the highest in PE-CVD and gradually became lower in the order of CVD, then the sol-gel method. Corrosion resistance of $TiO_2$ thin films against fluoride solution was stronger in CVD and PE-CVD methods than in the sol-gel method. The results of this study suggest that the CVD or PE-CVD methods is more appropriate than the sol-gel method for $TiO_2$ coating on orthodontic wires and brackets.

• Journal of the Korean Vacuum Society
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• v.20 no.2
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• pp.155-163
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• 2011

Carbon nanotubes (CNT) have been attracted much attention since they have been expected to be used in various areas by virtue of their outstanding physical, electrical, and chemical properties. In order to make full use of their prominent electric conductivity in some areas such as electron emission sources, device interconnects, and electrodes in energy storage devices, direct growth of CNT with vertical alignment is definitely beneficial issue because they can maintain mechanical stability and high conductivity at the interface between substrates. Here, we report direct growth of vertically aligned CNT (VCNT) on Cu foils using thermal chemical vapor deposition and characterize the field emission property of the VCNT. The VCNT's height was controlled by changing the growth temperature, growth time, and catalytic layer thickness. Optimum growth condition was found to be $800^{\circ}C$ for 20 min with acetylene and hydrogen mixtures on Fe catalytic layer of 1 nm thick. The diameter of VCNT grown was smaller than that of usual multi walled CNT. Based on the result of field emission characterization, we concluded that the VCNT on Cu foils can be useful in various potential applications where high conductivity through the interface between CNT and substrate is required.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2003.10a
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• pp.134-135
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• 2003

The dental implant materials required good mechanical properties, such as fatigue strength, combined with a high resistance to corrosion. For increasing fatigue resistance and delaying onset of stress corrosion cracking, shot peening has been used for > 50 years to extend service life of metal components. However, there is no information on the electrochemical behavior of shot peened and hydroxyapatite(HA) coated Ti-6Al-4V alloys. To increase fatigue strength, good corrosion resistance, and biocompatibility, the electrochemical characteristics of Ti/TiN/HA coated and shot peened Ti-6Al-4V alloys by electron beam physical vapor deposition(EB-PVD) have been researched by various electrochemical method in 0.9%NaCl. Ti-6Al-4V alloys were prepared under the condition of hydrogen and vacuum arc furnace. The produced materials were quenched at 1000$^{\circ}C$ under high purity dried Ar atmosphere and were hold at 500$^{\circ}C$ for 2 hrs to achieve the fatigue strength(1140㎫) of materials. Ti-6Al-4V alloys were prepared under the condition of hydrogen and vacuum arc furnace. Shot peening(SP) and sand blasting treatment was carried out for 1, 5, and 10min. On the surface of Ti-6Al-4V alloys using the steel balls of 0.5mm and alumina sand of 40$\mu\textrm{m}$ size. Ti/TiN/HA multilayer coatings were carried out by using electron-beam deposition method(EB-PVD) as shown Fig. 1. Bulk Ti, powder TiN and hydroxyapatite were used as the source of the deposition materials. Electrons were accelerated by high voltage of 4.2kV with 80 - 120mA on the deposition materials at 350$^{\circ}C$ in 2.0 X 10-6 torr vacuum. Ti/TiN/HA multilayer coated surfaces and layers were investigated by SEM and XRD. A saturated calomel electrode as a reference electrode, and high density carbon electrode as a counter electrode, were set according to ASTM GS-87. The potentials were controlled at a scan rate of 100 mV/min. by a potentiostat (EG&G Co.273A) connected to a computer system. Electrochemical tests were used to investigate the electrochemical characteristics of Ti/TiN/HA coated and shot peened materials in 0.9% NaCl solution at 36.5$^{\circ}C$. After each electrochemical measurement, the corrosion surface of each sample was investigated by SEM.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.279-279
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• 2007

비휘발성 메모리 Fe-RAM은 빠른 정보처리 속도와 전원공급이 차단되었을 때도 계속 정보를 유지할 수 있는 비휘발성 특징과 더불어 저전압, 저전력 구동의 장점이 있어서, 차세대 메모리로 많은 주목을 받고 있다. FeRAM에 사용되는 강유전체는 주로 Pb(Zr,Ti)$O_3$가 적용되었는데, 최근에는 비납계 강유전체의 연구도 활발히 이루어지고 있다. 이러한 비납계 강유전체 중에서 가장 특성이 우수한 물질은 $(Bi,La)_4Ti_3O_{12}$ (BLT) 이다. 그런데 BLT는 결정 방향에 따른 강한 이방성의 강유전 특성을 나타내기 때문에 BLT 박막을 이용하여 Fe-RAM 소자 등을 제작하기 위해서는 결정의 방향성을 세심하게 제어하는 것이 매우 중요하다. 지금까지 연구된 BLT 박막의 방향성 조절결과를 보면, BLT 박막을 스핀 코팅 법 (spin coating method)으로 증착하고, 핵생성 열처리 단계를 조절하여 무작위 방향성을 갖는 박막을 제조하는 방법이 일반적이었다. 그런데 이러한 스핀 코팅법에서의 핵생성 단계의 제어는 공정 조건 확보가 너무 어려운 단점이 있다. 이러한 어려움을 극복할 수 있는 대안은 스퍼터링 증착법(sputtering deposition method), PLD (pulsed laser deposition)법 등과 같은 PVD (physical vapor deposition) 법의 증착방법을 적용하는 것이다. PVD 법으로 증착하는 경우에는 이미 박막 내에 무수한 결정핵이 존재하기 때문에 핵생성 단계가 필요가 없게 된다. PVD 증착법의 적용을 위해서는 타겟의 제조 및 평가 실험이 선행되어야 한다. 그런데 벌크 BLT 재료의 소결공정 조건과 전기적 특성에 관한 연구 결과는 거의 발표가 되지 않고 있다. 본 실험에서는 $Bi_2O_3,\;TiO_2,\;La_2O_3,\;Nb_2O_5\;and\;Al_2O_3$ 분말들을 이용하여 최적의 조성을 구하기 위하여 $Nb^{+5}$ 와 $Al^{+3}$을 $Ti^{+4}$ 자리에 소량 치환시켜 제조하였다. 혼합된 분말을 하소 후 pellet 형태로 성형하여 소결을 실시하였다. 시편을 1mm 두께로 연마하고, 양면에 silver 전극을 인쇄하여 전기적 특성을 측정하였다. 측정결과 $Ti^{+4}$ 자리에 $Nb^{+5}$를 치환하여 제조한 시편에서 $2P_r{\sim}31\;{\mu}c/cm^2$정도의 매우 우수한 특성을 얻었다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.06a
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• pp.277-277
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• 2007

$(Bi,La)_4Ti_3O_{12}$ (BLT) 물질은 결정 방향에 따른 강한 이방성의 강유전 특성을 나타낸다. 따라서 BLT 박막을 이용하여 FeRAM 소자 등을 제작하기 위해서는 결정의 방향성을 세심하게 제어하는 것이 매우 중요하다. 현재까지 연구된 BLT 박막의 방향성 조절 결과를 보면, BLT 박막을 스핀 코팅 법 (spin coating method)으로 중착하고, 핵생성 열처리 단계를 조절하여 무작위 방향성 (random orientation)을 갖는 박막을 제조하는 방법이 일반적이었다. 그런데 이러한 스핀 코팅법에서의 핵생성 단계의 제어는 공정 조건 확보가 너무 어려운 단점이 있다. 이러한 어려움을 극복할 수 있는 대안은 스퍼터링 증착법 (sputtering deposition method), PLD법 (pulsed laser deposition method) 등과 같은 PVD (physical vapor deposition) 법의 증착방법을 적용하는 것이다. PVD 법으로 증착하는 경우에는 이미 박막 내에 무수한 결정핵이 존재하기 때문에 핵생성 단계가 필요 없게 된다. PVD 증착법의 적용을 위해서는 타겟 (target)의 제조 및 평가 실험이 선행되어야 한다. 그런데 벌크 BLT 재료의 소결공정 조건과 전기적 특성에 관한 연구 결과는 거의 발표 되지 않고 있다. 본 실험에서는 $Bi_2O_3$, $TiO_2$ and $La_2O_3$ 분말을 이용하여 최적의 조성을 구하기 위하여 Bi양을 변화시키며 타겟을 제조 하였다. 혼합된 분말을 하소 후 pallet 형태로 성형하여 소결을 실시하였다. 시편을 1mm 두께로 연마하고, 표면에 silver 전극을 인쇄하여 전기적 특성을 측정하였다. Bi양이 3.28몰 첨가된 조성에서 최대의 잔류분극 (2Pr) 값을 얻었고, 이때의 값은 약 $18{\mu}C/cm^2$ 정도였다. 최적화된 조성 ($Bi_{3.28}La_{0.75}Ti_3O_{12}$)으로 BLT 타겟을 제조하여 PLD법으로 박막을 제조하였다. 박막 제조 시 압력은 $1{\times}10^{-1}\;{\sim}\;1{\times}10^{-4}\;Torr$ 범위에서 변화시켰다. $1{\times}10^{-1}\;Torr$ 압력을 제외하고는 모든 압력에서 BLT 박막이 증착되었다. 중착된 박막을 $650\;{\sim}\;800^{\circ}C$에서 30분간 열처리를 실시하고 전기적 특성을 평가한 결과, $1{\times}10^{-2}\;Torr$에서 증착한 박막에서 양호한 P-V (polarization-voltage) 이력곡선을 얻을 수 있었고, 이때의 잔류분극 (2Pr) 값은 약 $6\;{\mu}C/cm^2$ 이었다. 주사전자현미경 (SEM)을 이용하여 BLT 박막 표면의 미세구조도 관찰하였는데, 스핀코팅 법으로 증착한 경우에 관찰되었던 조대화된 입자들은 관찰되지 않았고, 상당히 양호한 입자 크기 균일도를 나타내었다.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.229-229
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• 2010

With the scaling down of ultra large integrated circuits (ULSI) to the sub-50 nm technology node, the need for an ultra-thin, continuous and conformal diffusion barrier and Cu seed layer is increasing. However, diffusion barrier and Cu seed layer formation with a physical vapor deposition (PVD) method has become difficult as the technology node is reduced to 30 nm and beyond. Recent work on self-forming barrier processes using PVD Cu alloys have attracted great attention due to the capability of conformal ultra-thin barrier formation using a simple technique. However, as in the case of the conventional barrier and Cu seed layer, PVD of the Cu alloy seed layer will eventually encounter the difficulty in conformal deposition in narrow line trenches and via holes. Atomic layer deposition (ALD) has been known for its good step coverage and precise thickness control, and is a candidate technique for the formation of a thin conformal barrier layer and Cu seed layer. Conformal Cu-Mn seed layers were deposited by plasma enhanced atomic layer deposition (PEALD) at low temperature ($120^{\circ}C$), and the Mn content in the Cu-Mn alloys were controlled form 0 to approximately 10 atomic percent with various Mn precursor feeding times. Resistivity of the Cu-Mn alloy films decreased by annealing due to out-diffusion of Mn atoms. Out-diffused Mn atoms were segregated to the surface of the film and interface between a Cu-Mn alloy and $SiO_2$, resulting in self-formed $MnO_x$ and $MnSi_xO_y$, respectively. No inter-diffusion was observed between Cu and $SiO_2$ after annealing at $500^{\circ}C$ for 12 h, indicating an excellent diffusion barrier property of the $MnSi_xO_y$. The adhesion between Cu and $SiO_2$ was enhanced by the formation of $MnSi_xO_y$. Continuous and conductive Cu-Mn seed layers were deposited with PEALD into 32 nm $SiO_2$ trench, enabling a low temperature process, and the trench was perfectly filled using electrochemical plating (ECD) under conventional conditions. Thus, it is the resultant self-forming barrier process with PEALD Cu-Mn alloy film as a seed layer for plating Cu that has further potential to meet the requirement of the smaller than 30 nm node.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.188-188
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• 2012

Graphene, with its unique physical and structural properties, has recently become a proving ground for various physical phenomena, and is a promising candidate for a variety of electronic device and flexible display applications. Compared to indium tin oxide (ITO) electrodes, which have a typical sheet resistance of ${\sim}60{\Omega}$/sq and ~85% transmittance in the visible range, the chemical vapor deposition (CVD) synthesized graphene electrodes have a higher transmittance in the visible to IR region and are more robust under bending. Nevertheless, the lowest sheet resistance of the currently available CVD graphene electrodes is higher than that of ITO. In this study, we report a creative strategy, irradiation of microwave at room temperature under vacuum, for obtaining size-homogeneous gold nano-particle doping on graphene. The gold nano-particlization promoted by microwave irradiation was investigated by transmission electron microscopy, electron energy loss spectroscopy elemental mapping. These results clearly revealed that gold nanoparticle with ${\geq}30$ nm in mean size were decorated along the surface of the graphene after microwave irradiation. The fabrication high-performance transparent conducting film with optimized doping condition showed a sheet resistance of ${\geq}100{\Omega}$/sq. at ~90% transmittance. This approach advances the numerous applications of graphene films as transparent conducting electrodes.