• Title/Summary/Keyword: Vapor Deposition Process

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Process technology and the formation of the TiN barrier metal by physical vapor deposition (PVD 방법에 의한 TiN barrier metal 형성과 공정개발)

  • 최치규;강민성;박형호;염병렬;서경수;이종덕;김건호;이정용
    • Journal of the Korean Vacuum Society
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    • v.6 no.3
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    • pp.255-262
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    • 1997
  • Titanium nitride (TiN) films were prepared by reactive sputter deposition in mixed gas of Ar+$N_2$. The volume percentage of $N_2$ in the working gas was chosen so as to grow stoichiometric TiN films and the substrate temperature during film growth was set from room temperature to $700^{\circ}C$. Stoichiometric $Ti_{0.5}N){0.5}$ films with (111) texture were grown at temperatures over $600^{\circ}C$, while films prepared at temperatures below $600^{\circ}C$ showed N-rich TiN. The composition X and y in the $Ti_xN_y$ films determined by XPS and RBS varied within 5% with the substrate temperature. The sheet resistance of the TiN films decreases as the substrate temperature increased. TiN film prepared at $600^{\circ}C$ showed 14.5$\Omega\Box$, and it decreased to 8.9$\Omega\Box$ after the sample was annealed at $700^{\circ}C$, 30 sec in Ar-gas ambient by RTA. By far, high quality stoichiometric TiN films by reactive sputtering in the mixed gas ambient could be prepared at substrate temperature over $600^{\circ}C$.

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Fabrication of ${\gamma}-Fe_2O_3$ Thin Film for Chemical Sensor Application (화학센서용 다공성 ${\gamma}-Fe_2O_3$ 박막 제조)

  • Kim, Bum-Jin;Lim, Il-Sung;Jang, Gun-Eik
    • Journal of Sensor Science and Technology
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    • v.8 no.2
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    • pp.171-176
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    • 1999
  • ${\gamma}-Fe_2O_3$ thin films on $Al_2O_3$ substrate were prepared by the oxidation of $Fe_3O_4$ thin films processed by PECVD(Plasma-Enhanced Chemical Vapor Deposition) technique. The phase transformation of ${\gamma}-Fe_2O_3$ thin films was mainly controlled by the substrate temperature and oxidation process of $Fe_3O_4$ phase. $Fe_3O_4$ phase was obtained at the deposition temperature of $200{\sim}300^{\circ}C$. $Fe_3O_4$ phase could be transformed into ${\gamma}-Fe_2O_3$ phase under controlled oxidation at $280{\sim}300^{\circ}C$. $Fe_3O_4$ and ${\gamma}-Fe_2O_3$ obtained by oxidation of $Fe_3O_4$ phase had the same spinel structure and were coexisted. The oxidized ${\gamma}-Fe_2O_3$ thin film on $Al_2O_3$ substrate showed a porous island structure.

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Characteristics of $Al_2O_3/TiO_2$ multi-layers as moisture permeation barriers deposited on PES substrates using ECR-ALD

  • Gwon, Tae-Seok;Mun, Yeon-Geon;Kim, Ung-Seon;Mun, Dae-Yong;Kim, Gyeong-Taek;Park, Jong-Wan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.457-457
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    • 2010
  • Flexible organic light emitting diodes (F-OLEDs) requires excellent moisture permeation barriers to minimize the degradation of the F-OLEDs device. Specifically, F-OLEDs device need a barrier layer that transmits less than $10^{-6}g/m^2/day$ of water and $10^{-5}g/m^2/day$ of oxygen. To increase the life time of F-OLEDs, therefore, it is indispensable to protect the organic materials from water and oxygen. Severe groups have reported on multi-layerd barriers consisting inorganic thin films deposited by plasma enhenced chemical deposition (PECVD) or sputtering. However, it is difficult to control the formation of granular-type morphology and microscopic pinholes in PECVD and sputtering. On the contrary, atomic layer deoposition (ALD) is free of pinhole, highly uniform, conformal films and show good step coverage. Thus, $Al_2O_3/TiO_2$ multi-layer was deposited onto the polyethersulfon (PES) substrate by electron cyclotron resonance atomic layer deposition (ECR-ALD), and the water vapor transmission rates (WVTR) were measured. WVTR of moisture permeation barriers is dependent upon density of films and initial state of polymer surface. A significant reduction of WVTR was achieved by increasing density of films and by applying low plasma induced interlayer on the PES substrate. In order to minimize damage of polymer surface, a 10 nm thick $TiO_2$ was deposited on PES prior to a $Al_2O_3$ ECR-ALD process. High quality barriers were developed from $Al_2O_3$ barriers on the $TiO_2$ interlayer. WVTR of $Al_2O_3$ by introducing $TiO_2$ interlayer was recorded in the range of $10^{-3}g/m^2.day$ at $38^{\circ}C$ and 100% relative humidity using a MOCON instrument. The WVTR was two orders of magnitude smaller than $Al_2O_3$ barriers directly grown on PES substrate without the $TiO_2$ interlayer. Thus, we can consider that the $Al_2O_3/TiO_2$ multi-layer passivation can be one of the most suitable F-OLEDs passivation films.

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Hybrid Water Treatment of Carbon Ultrafiltration Membrane and Polypropylene Beads Coated with Photocatalyst: Effect of Organic Materials, Photo-oxidation, and Adsorption in Water Back-flushing (탄소 한외여과막 및 광촉매 코팅 폴리프로필렌 구의 혼성 수처리: 물 역세척 시 유기물 및 광산화, 흡착의 영향)

  • Park, Jin Yong;Jung, Chung Ho
    • Membrane Journal
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    • v.22 no.5
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    • pp.359-368
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    • 2012
  • For hybrid water treatment of high turbidity water, we used the hybrid module that was composed of photocatalyst packing between tubular membrane outside and module inside. Photocatalyst was PP (polypropylene) bead coated with $TiO_2$ powder by CVD (chemical vapor deposition) process. Water back-flushing of 10 sec was performed per every period of 10 min to minimize membrane fouling for modified solution was prepared with humic acid and kaolin. Resistance of membrane fouling ($R_f$) decreased as humic acid concentration changed from 10 mg/L to 2 mg/L, and finally the highest total permeate volume ($V_T$) could be obtained at 2 mg/L, which was the same with the previous results. Then, treatment efficiencies of turbidity and humic acid were above 98.9% and 88.7%, respectively. As results of treatment portions of UF, UF + $TiO_2$, and UF + $TiO_2$ + UV processes, turbidity was treated little by photocatalyst adsorption, and photo-oxidation. However, treatment portions of humic acid by adsorption and photo-oxidation were 2.5% and 12.3%, respectively. Compared with the previous results, treatment portions of humic acid by adsorption and photo-oxidation were different depending on membrane material and pore size. As simplified the process, the membrane fouling resistance after 180 minutes' operation ($R_{f,180}$) increased and the final permeate flux decreased a little.

Property of Nickel Silicides with 10 nm-thick Ni/Amorphous Silicon Layers using Low Temperature Process (10 nm-Ni 층과 비정질 실리콘층으로 제조된 저온공정 나노급 니켈실리사이드의 물성 변화)

  • Choi, Youngyoun;Park, Jongsung;Song, Ohsung
    • Korean Journal of Metals and Materials
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    • v.47 no.5
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    • pp.322-329
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    • 2009
  • 60 nm- and 20 nm-thick hydrogenated amorphous silicon (a-Si:H) layers were deposited on 200 nm $SiO_2/Si$ substrates using ICP-CVD (inductively coupled plasma chemical vapor deposition). A 10 nm-Ni layer was then deposited by e-beam evaporation. Finally, 10 nm-Ni/60 nm a-Si:H/200 nm-$SiO_2/Si$ and 10 nm-Ni/20 nm a-Si:H/200 nm-$SiO_2/Si$ structures were prepared. The samples were annealed by rapid thermal annealing for 40 seconds at $200{\sim}500^{\circ}C$ to produce $NiSi_x$. The resulting changes in sheet resistance, microstructure, phase, chemical composition and surface roughness were examined. The nickel silicide on a 60 nm a-Si:H substrate showed a low sheet resistance at T (temperatures) >$450^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate showed a low sheet resistance at T > $300^{\circ}C$. HRXRD analysis revealed a phase transformation of the nickel silicide on a 60 nm a-Si:H substrate (${\delta}-Ni_2Si{\rightarrow}{\zeta}-Ni_2Si{\rightarrow}(NiSi+{\zeta}-Ni_2Si)$) at annealing temperatures of $300^{\circ}C{\rightarrow}400^{\circ}C{\rightarrow}500^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate had a composition of ${\delta}-Ni_2Si$ with no secondary phases. Through FE-SEM and TEM analysis, the nickel silicide layer on the 60 nm a-Si:H substrate showed a 60 nm-thick silicide layer with a columnar shape, which contained both residual a-Si:H and $Ni_2Si$ layers, regardless of annealing temperatures. The nickel silicide on the 20 nm a-Si:H substrate had a uniform thickness of 40 nm with a columnar shape and no residual silicon. SPM analysis shows that the surface roughness was < 1.8 nm regardless of the a-Si:H-thickness. It was confirmed that the low temperature silicide process using a 20 nm a-Si:H substrate is more suitable for thin film transistor (TFT) active layer applications.

A Study on Properites of PV Solar cell AZO thin films post-annealing by RTP technique (RTP 공정을 통한 태양전지용 AZO 박막의 후열처리 특성연구)

  • Yang, Hyeon-Hun;Kim, Han-Wool;Han, Chang-Jun;So, Soon-Youl;Park, Gye-Choon;Lee, Jin;Chung, Hea-Deok;Lee, Suk-Ho;Back, Su-Ung;Na, Kil-Ju;Jeong, Woon-Jo
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.127.1-127.1
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    • 2011
  • In this paper, ZnO:Al thin films with c-axis preferred orientation were prepared on Soda lime glass substrates by RF magnetron sputtering technique. AZO thin film were prepared in order to clarify optimum conditions for growth of the thin film depending upon process, and then by changing a number of deposition conditions and substrate temperature conditions variously, structural and electrical characteristics were measured. For the manufacture of the AZO were vapor-deposited in the named order. It is well-known that post-annealing is an important method to improve crystal quality. For the annealing process, the dislocation nd other defects arise in the material and adsorption/decomposition occurs. The XRD patterns of the AZO films deposited with grey theory prediction design, annealed in a vacuum ambient($2.0{\times}10-3$Torr)at temperatures of 200, 300, 400 and $500^{\circ}C$ for a period of 30min. The diffraction patterns of all the films show the AZO films had a hexagonal wurtzite structure with a preferential orientation along the c-axis perpendicular to the substrate surface. As can be seen, the (002)peak intensities of the AZO films became more intense and sharper when the annealing temperature increased. On the other hand, When the annealing temperature was $500^{\circ}C$ the peak intensity decreased. The surface morphologies and surface toughness of films were examined by atomic force microscopy(AFM, XE-100, PSIA). Electrical resistivity, Gall mobility and carrier concentration were measured by Hall effect measuring system (HL5500PC, Accent optical Technology, USA). The optical absorption spectra of films in the ultraviolet-visibleinfrared( UV-Vis-IR) region were recorder by the UV spectrophotometer(U-3501, Hitachi, Japan). The resistivity, carrier concentration, and Hall mobility of ZnS deposited on glass substrate as a function of post-annealing.

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Growth of SiC Oxidation Protective Coating Layers on graphite substrates Using Single Source Precursors

  • Kim, Myung-Chan;Heo, Cheol-Ho;Park, Jin-Hyo;Park, Seung-Jun;Han, Jeon-Geon
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.122-122
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    • 1999
  • Graphite with its advantages of high thermal conductivity, low thermal expansion coefficient, and low elasticity, has been widely used as a structural material for high temperature. However, graphite can easily react with oxygen at even low temperature as 40$0^{\circ}C$, resulting in CO2 formation. In order to apply the graphite to high temperature structural material, therefore, it is necessary to improve its oxidation resistive property. Silicon Carbide (SiC) is a semiconductor material for high-temperature, radiation-resistant, and high power/high frequency electronic devices due to its excellent properties. Conventional chemical vapor deposited SiC films has also been widely used as a coating materials for structural applications because of its outstanding properties such as high thermal conductivity, high microhardness, good chemical resistant for oxidation. Therefore, SiC with similar thermal expansion coefficient as graphite is recently considered to be a g행 candidate material for protective coating operating at high temperature, corrosive, and high-wear environments. Due to large lattice mismatch (~50%), however, it was very difficult to grow thick SiC layer on graphite surface. In theis study, we have deposited thick SiC thin films on graphite substrates at temperature range of 700-85$0^{\circ}C$ using single molecular precursors by both thermal MOCVD and PEMOCVD methods for oxidation protection wear and tribological coating . Two organosilicon compounds such as diethylmethylsilane (EDMS), (Et)2SiH(CH3), and hexamethyldisilane (HMDS),(CH3)Si-Si(CH3)3, were utilized as single source precursors, and hydrogen and Ar were used as a bubbler and carrier gas. Polycrystalline cubic SiC protective layers in [110] direction were successfully grown on graphite substrates at temperature as low as 80$0^{\circ}C$ from HMDS by PEMOCVD. In the case of thermal MOCVD, on the other hand, only amorphous SiC layers were obtained with either HMDS or DMS at 85$0^{\circ}C$. We compared the difference of crystal quality and physical properties of the PEMOCVD was highly effective process in improving the characteristics of the a SiC protective layers grown by thermal MOCVD and PEMOCVD method and confirmed that PEMOCVD was highly effective process in improving the characteristics of the SiC layer properties compared to those grown by thermal MOCVD. The as-grown samples were characterized in situ with OES and RGA and ex situ with XRD, XPS, and SEM. The mechanical and oxidation-resistant properties have been checked. The optimum SiC film was obtained at 85$0^{\circ}C$ and RF power of 200W. The maximum deposition rate and microhardness are 2$mu extrm{m}$/h and 4,336kg/mm2 Hv, respectively. The hardness was strongly influenced with the stoichiometry of SiC protective layers.

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A Study on the Comparison of Brazed Joint of Zircaloy-4 with PVD-Be and Zr-Be Amorphous alloys as Filler Metals (PVD-Be와 비정질 Zr-Be 합금을 용가재로 사용한 Zircaloy-4의 브레이징 접합부의 비교 연구)

  • Hwang, Yong-Hwa;Kim, Jae-Yong;Lee, Hyung-Kwon;Koh, Jin-Hyun;Oh, Se-Yong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.7 no.2
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    • pp.113-119
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    • 2006
  • Brazing is an important manufacturing process in the fabrication of Heavy Water Reactor fuel rods, in which bearing and spacer pads are joined to Zircaloy-4 cladding tubes. The physical vapor deposition(PVD) technique is currently used to deposit metallic Be on the surfaces of pads as a filler metal. Amorphous Zr-Be binary alloys which are manufactured by rapid solidification process are under developing to substitute the conventional PVD-Be coating. In the present study, brazed joint with PVD and amorphous alloys of $Zr_{1-x}Be_{x}(0.3{\le}x{\le}0.5)$ as filler metals are compared by mechanism, microstructure and hardness. The thickness of brazed joint with amorphous alloys became much smaller than that of PVD-Be. The erosion of base metal did not occur in the brazed joint with amorphous alloys. The brazing mechanism for PVD-Be seems to be Be diffusion into Zr-4 with capillary action resulting from eutectic reaction while that for amorphous alloys are associated with the liquid phase formation in the brazed joint. The brazed joint microstructure with PVD-Be consists of dendrite while that with amorphous alloys is globular. The $Zr_{0.7}Be_{0.3}$ alloy shows the smooth interface with little erosion in the base metal and is recommended a most suitable brazing filler metal for Zircaloy-4.

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Large-Area Synthesis of High-Quality Graphene Films with Controllable Thickness by Rapid Thermal Annealing

  • Chu, Jae Hwan;Kwak, Jinsung;Kwon, Tae-Yang;Park, Soon-Dong;Go, Heungseok;Kim, Sung Youb;Park, Kibog;Kang, Seoktae;Kwon, Soon-Yong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.130.2-130.2
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    • 2013
  • Today, chemical vapor deposition (CVD) of hydrocarbon gases has been demonstrated as an attractive method to synthesize large-area graphene layers. However, special care should be taken to precisely control the resulting graphene layers in CVD due to its sensitivity to various process parameters. Therefore, a facile synthesis to grow graphene layers with high controllability will have great advantages for scalable practical applications. In order to simplify and create efficiency in graphene synthesis, the graphene growth by thermal annealing process has been discussed by several groups. However, the study on growth mechanism and the detailed structural and optoelectronic properties in the resulting graphene films have not been reported yet, which will be of particular interest to explore for the practical application of graphene. In this study, we report the growth of few-layer, large-area graphene films using rapid thermal annealing (RTA) without the use of intentional carbon-containing precursor. The instability of nickel films in air facilitates the spontaneous formation of ultrathin (<2~3 nm) carbon- and oxygen-containing compounds on a nickel surface and high-temperature annealing of the nickel samples results in the formation of few-layer graphene films with high crystallinity. From annealing temperature and ambient studies during RTA, it was found that the evaporation of oxygen atoms from the surface is the dominant factor affecting the formation of graphene films. The thickness of the graphene layers is strongly dependent on the RTA temperature and time and the resulting films have a limited thickness less than 2 nm even for an extended RTA time. The transferred films have a low sheet resistance of ~380 ${\Omega}/sq$, with ~93% optical transparency. This simple and potentially inexpensive method of synthesizing novel 2-dimensional carbon films offers a wide choice of graphene films for various potential applications.

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Property of Nickel Silicides with Hydrogenated Amorphous Silicon Thickness Prepared by Low Temperature Process (나노급 수소화된 비정질 실리콘층 두께에 따른 저온형성 니켈실리사이드의 물성 연구)

  • Kim, Jongryul;Choi, Youngyoun;Park, Jongsung;Song, Ohsung
    • Korean Journal of Metals and Materials
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    • v.46 no.11
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    • pp.762-769
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    • 2008
  • Hydrogenated amorphous silicon(a-Si : H) layers, 120 nm and 50 nm in thickness, were deposited on 200 $nm-SiO_2$/single-Si substrates by inductively coupled plasma chemical vapor deposition(ICP-CVD). Subsequently, 30 nm-Ni layers were deposited by E-beam evaporation. Finally, 30 nm-Ni/120 nm a-Si : H/200 $nm-SiO_2$/single-Si and 30 nm-Ni/50 nm a-Si:H/200 $nm-SiO_2$/single-Si were prepared. The prepared samples were annealed by rapid thermal annealing(RTA) from $200^{\circ}C$ to $500^{\circ}C$ in $50^{\circ}C$ increments for 30 minute. A four-point tester, high resolution X-ray diffraction(HRXRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and scanning probe microscopy(SPM) were used to examine the sheet resistance, phase transformation, in-plane microstructure, cross-sectional microstructure, and surface roughness, respectively. The nickel silicide on the 120 nm a-Si:H substrate showed high sheet resistance($470{\Omega}/{\Box}$) at T(temperature) < $450^{\circ}C$ and low sheet resistance ($70{\Omega}/{\Box}$) at T > $450^{\circ}C$. The high and low resistive regions contained ${\zeta}-Ni_2Si$ and NiSi, respectively. In case of microstructure showed mixed phase of nickel silicide and a-Si:H on the residual a-Si:H layer at T < $450^{\circ}C$ but no mixed phase and a residual a-Si:H layer at T > $450^{\circ}C$. The surface roughness matched the phase transformation according to the silicidation temperature. The nickel silicide on the 50 nm a-Si:H substrate had high sheet resistance(${\sim}1k{\Omega}/{\Box}$) at T < $400^{\circ}C$ and low sheet resistance ($100{\Omega}/{\Box}$) at T > $400^{\circ}C$. This was attributed to the formation of ${\delta}-Ni_2Si$ at T > $400^{\circ}C$ regardless of the siliciation temperature. An examination of the microstructure showed a region of nickel silicide at T < $400^{\circ}C$ that consisted of a mixed phase of nickel silicide and a-Si:H without a residual a-Si:H layer. The region at T > $400^{\circ}C$ showed crystalline nickel silicide without a mixed phase. The surface roughness remained constant regardless of the silicidation temperature. Our results suggest that a 50 nm a-Si:H nickel silicide layer is advantageous of the active layer of a thin film transistor(TFT) when applying a nano-thick layer with a constant sheet resistance, surface roughness, and ${\delta}-Ni_2Si$ temperatures > $400^{\circ}C$.