• Title/Summary/Keyword: plasma coating

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Al2O3 High Dense Single Layer Gas Barrier by Neutral Beam Assisted Sputtering (NBAS) Process

  • Jang, Yun-Seong;Hong, Mun-Pyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.157-157
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    • 2015
  • Recently, the growing interest in organic microelectronic devices including OLEDs has led to an increasing amount of research into their many potential applications in the area of flexible electronic devices based on plastic substrates. However, these organic devices require a gas barrier coating to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency OLEDs require an extremely low water vapor transition rate (WVTR) of $1{\times}10^{-6}g/m^2day$. The Key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required ($1{\times}10^{-6}g/m^2day$) is the suppression of defect sites and gas diffusion pathways between grain boundaries. In this study NBAS process was introduced to deposit enhanced film density single gas barrier layer with a low WVTR. Fig. 1. shows a schematic illustration of the NBAS apparatus. The NBAS process was used for the $Al_2O_3$ nano-crystal structure films deposition, as shown in Fig. 1. The NBAS system is based on the conventional RF magnetron sputtering and it has the electron cyclotron resonance (ECR) plasma source and metal reflector. $Ar^+$ ion in the ECR plasma can be accelerated into the plasma sheath between the plasma and metal reflector, which are then neutralized mainly by Auger neutralization. The neutral beam energy is controlled by the metal reflector bias. The controllable neutral beam energy can continuously change crystalline structures from an amorphous phase to nanocrystal phase of various grain sizes. The $Al_2O_3$ films can be high film density by controllable Auger neutral beam energy. we developed $Al_2O_3$ high dense barrier layer using NBAS process. We can verified that NBAS process effect can lead to formation of high density nano-crystal structure barrier layer. As a result, Fig. 2. shows that the NBAS processed $Al_2O_3$ high dense barrier layer shows excellent WVTR property as a under $2{\times}10^{-5}g/m^2day$ in the single barrier layer of 100nm thickness. Therefore, the NBAS processed $Al_2O_3$ high dense barrier layer is very suitable in the high efficiency OLED application.

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PEMOCVD of Ti(C,N) Thin Films on D2 Steel and Si(100) Substrates at Low Growth Temperatures

  • Kim, Myung-Chan;Heo, Cheol-Ho;Boo, Jin-Hyo;Cho,Yong-Ki;Han, Jeon-Geon
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.211-211
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    • 1999
  • Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.

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레이저 유도 형광법(Laser Induced Fluorescence)을 이용한 플라즈마 방전 표시기(Plasma Display Panel)내의 전계 측정에 관한 연구

  • 김정훈;이준학;최영욱;양진호;황기웅
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.232-232
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    • 1999
  • 교류형 플라즈마 방전 표시기(AC Plasma Display Panel, AC PDP)에 사용되는 플라즈마는 그 부피가 너무 작아서 플라즈마에 변화를 일으키지 않고 그 물성을 관측하기란 쉬운일이 아니다. 그래서 주로 PDP 내의 물성을 관측하는 데 시뮬레이션에 의존하게 된다. 그 물성중에 PDP내의 전계 분포에 대한 정보는 방전의 형성 및 소멸에 대한 많은 단서를 제공하고 있다. 특히 AC PDP의 경우, 유전체에 형성되는 벽적하(wall charge)가 방전의 형성 및 PDP 구동에 중요한 역할을 하는데, 이는 PDP 내의 전계 분포를 살펴봄으로써 대략 예측할 수 있다. 본 연구에서는 시뮬레이션에 의존하지 않고, 직접 레이저 유도 형광법을 이용하여 AC PDP 내의 전계를 측정하였다. 방전 가스인 헬륨(He)의 에너지 준위는 전계의 크기에 따라 에너지 준위가 변화하여, Rydberg(n$\geq$8) 준위가 여러 개의 준위로 나누어지는 현상이 일어나는데, 이를 Stack 효과라고 한다. 따라서 전계의 세기가 커짐에 따라서 각 준위와 준위 사이 값(splitting)이 커지는데, 이를 이용하면 전계를 측정할 수 있다. 즉, 헬륨 원자를 여기시키는 레이저 파장을 변화시키면서 관측되는 레이저 유도 형광 신호를 관측하면, 준위의 splitting을 관측할 수 있다. 본 연구에서는 PDP 내의 전계의 시간적 변화를 관측하였다. 50%, 40kHz의 구형파를 PDP의 두 전극에 가하였을 때, 플라즈마가 켜진 상태뿐만 아니라 플라즈마가 꺼진 후에도 전계에 의한 Splitting 신호가 관측이 되었는데, 전계로 환산하였을 때, 그 값은 대략 수 kV/cm의 값을 갖았는데, 이는 wall charge에 의한 값으로 사료된다.결과로 생각되어진다.플라즈마의 강도값을 입력하여 플라즈마의 radiation을 검출하고, 스퍼터링 공정중 실질적인 in-situ 정보로 이용하였다. PEM을 통하여 In/Sn의 플라즈마 강도변화를 조사하였다. 초기 In/Sn의 플라즈마 강도(intensity)는 강도를 100하여, 산소를 주입한 결과, plasma intensity가 35 줄어들었고, 이때 우수한 ITO 박막을 얻을 수 있었다. Pulsed DC power를 사용하여 아크 현상을 방지하였다. PET 상에 coating 된 ITO 박막의 표면저항과 광투과도는 4-point prove와 spectrophotometer를 이용하여 분석하였고, AES로 박막의 두께에 따른 성분비를 확인하였다. ITO 박막의 광투과도는 산소의 유량과 sputter 된 In/Sn ion의 plasma emission peak에 따라 72%-92%까지 변화하였으며, 저항은 37$\Omega$/$\square$ 이상을 나타내었다. 박막의 Sn/In atomic ratio는 0.12, O/In의 비율은 In2O3의 화학양론적 비율인 1.5보다 작은 1.3을 나타내었다.로 보인다.하면 수평축과 수직축의 분산 장벽의 비에 따라 cluster의 두께비가 달라지는 성장을 볼 수 있었고, 한 축 방향으로의 팔 넓이는 fcc(100) 표면의 경우 동일한 Ed+Ep값에 대응하는 팔 넓이와 거의 동일한 결과가 나타나는 것을 볼 수 있다. 따라서 이러한 비대칭적인 모양을 가지는 성장의 경우도 cluster 밀도, cluster 모양, cluster의 양 축 방향 길이 비, 양 축 방향의 평균 팔 넓이로부터 각 축 방향의 분산 장벽을 얻어낼 수 있을 것으로 보인다. 기대할 수 있는 여러

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Hot Corrosion Behavior of Plasma Sprayed 4 mol% Y2O3-ZrO2 Thermal Barrier Coatings with Volcanic Ash (플라즈마 용사법으로 제작된 4mol% Y2O3-ZrO2 열차폐코팅의 화산재에 의한 고온열화거동)

  • Lee, Won-Jun;Jang, Byung-Koog;Lim, Dae-Soon;Oh, Yoon-Suk;Kim, Seong-Won;Kim, Hyung-Tae;Araki, Hiroshi;Murakami, Hideyuki;Kuroda, Seiji
    • Journal of the Korean Ceramic Society
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    • v.50 no.6
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    • pp.353-358
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    • 2013
  • The hot corrosion behavior of plasma sprayed 4 mol% $Y_2O_3-ZrO_2$ (YSZ) thermal barrier coatings (TBCs) with volcanic ash is investigated. Volcanic ash that deposited on the TBCs in gas-turbine engines can attack the surface of TBCs itself as a form of corrosive melt. YSZ coating specimens with a thickness of 430-440 ${\mu}m$ are prepared using a plasma spray method. These specimens are subjected to hot corrosion environment at $1200^{\circ}C$ with five different duration time, from 10 mins to 100 h in the presence of corrosive melt from volcanic ash. The microstructure, composition, and phase analysis are performed using Field emission scanning electron microscopy, including Energy dispersive spectroscopy and X-ray diffraction. After the heat treatment, hematite ($Fe_2O_3-TiO_2$) and monoclinic YSZ phases are found in TBCs. Furthermore the interface area between the molten volcanic ash layers and YSZ coatings becomes porous with increases in the heat treatment time as the YSZ coatings dissolved into molten volcanic ash. The maximum thickness of this a porous reaction zone is 25 ${\mu}m$ after 100 h of heat treatment.

Cyclic Oxidation Behavior of Vacuum Plasma Sprayed NiCoCrAlY Overlay Coatings (진공 플라즈마 용사법을 통해 형성된 NiCoCrAlY 오버레이 코팅의 반복 산화 거동)

  • Yoo, Yeon Woo;Nam, Uk Hee;Park, Hunkwan;Park, Youngjin;Lee, Sunghun;Byon, Eungsun
    • Journal of Surface Science and Engineering
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    • v.52 no.6
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    • pp.283-288
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    • 2019
  • MCrAlY overaly coatings are used as oxidation barrier coatings to prevent degradation of the underlying substrate in high temperature and oxidizing environment of the hot section of gas turbines. Therefore, oxidation resistance in high temperature is important property of MCrAlY coatings. Also, coefficients of thermal expansion (CTE) of MCrAlY have middle value of that of Ni-based superalloys and oxides, which have the effect of preventing the delamination of the surface oxides. Cyclic oxidation test is one of the most useful methods for evaluating the high temperature durability of coatings used in gas turbines. In this study, NiCoCrAlY overlay coatings were formed on Inconel 792(IN 792) substrates by vacuum plasma spraying process. Vacuum plasma sprayed NiCoCrAlY coatings and IN 792 susbstrates were exposed to 1000℃ one-hour cyclic oxidation environment. NiCoCrAlY coatings showed lower weight gain in short-term oxidation. In long-term oxidation, IN 792 substrates showed higher weight loss due to delamination of surface oxide but NiCoCrAlY coatings showed lower weight loss. X-ray diffraction (XRD) analysis showed α-Al2O3 and NiCr2O4 was formed during the cyclic oxidation test. Through cross-section observation using scanning electron microscopy (SEM) and electron back scatter diffraction (EBSD) analysis, thermally grown oxide (TGO) layer composed of α-Al2O3 and NiCr2O4 was formed and the thickness of TGO increased during 1000℃ cyclic oxidation test. β phase in upper side of NiCoCrAlY coating was depleted due to oxidation of Al and outer beta depletion zone thickness also increased as the cyclic oxidation time increased.

Heat Treatment Effects on the Phase Evolutions of Partially Stabilized Grade Zirconia Plasma Sprayed Coatings

  • Park, Han-Shin;Kim, Hyung-Jun;Lee, Chang-Hee
    • Journal of Surface Science and Engineering
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    • v.34 no.5
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    • pp.486-493
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    • 2001
  • Partially stabilized zirconia (PSZ) is an attractive material for thermal barrier coating. Zirconia exists in three crystallographic phases: cubic, tetragonal and monoclinic. Especially, the phase transformation of tetragonal phase to monoclinic phase accompanies significant volume expansion, so this transition generally results in cracking and contributes to the failure of the TBC system. Both the plasma sprayed ZrO$_2$-8Y$_2$O$_3$ (YSZ) coat and the ZrO$_2$,-25CeO$_2$,-2.5Y$_2$O$_3$ (CYSZ) coat are isothermally heat -treated at 130$0^{\circ}C$ and 150$0^{\circ}C$ for 100hr and cooled at different cooling rates. The monoclinic phase is not discovered in all the CYSZ annealed at 130$0^{\circ}C$ and 150$0^{\circ}C$. In the 150$0^{\circ}C$ heat-treated specimens, the YSZ contains some monoclinic phase while none exists in the 130$0^{\circ}C$ heat-treated YSZ coat. For the YSZ, the different phase transformation behaviors at the two temperatures are due to the stabilizer concentration of high temperature phases and grain growth. For the YSZ with 150$0^{\circ}C$-100hr annealing, the amount of monoclinic phase increased with the slower cooling rate. The extra oxygen vacancy, thermal stress, and c to t'phase transformation might suppress the t to m martensitic phase transformation.

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A Diamond-like Film Formation from (CH$_4$ + H$_2$) Gas Mixture with the LPCVD Apparatus (LPCVD 장치를 이용한 메탄과 수소 혼합기체로부터 다이아몬드 박막의 제조)

  • Kim Sang Kyun;Choy Jin-Ho;Choo Kwng Yul
    • Journal of the Korean Chemical Society
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    • v.34 no.5
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    • pp.396-403
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    • 1990
  • We describe how to design and construct a LPCVD (Low Pressure Chemical Vapor Deposition) apparatus which can be applicable to the study of reaction mechanism in general CVD experiments. With this apparatus we have attempted to make diamond like carbon films on the p-type (111) Si wafer from (H$_2$ + CH$_4$) gas mixtures. Two different methods have been tried to get products. (1)The experiment was carried out in the reactor with two different inlet gas tubes. One coated with phosphoric acid was used for supplying microwave discharged hydrogen gas stream, and methane has been passed through the other tube without the microwave discharge. In this method we got only amorphous carbon cluster products. (2) The gas mixture (H$_2$ + CH$_4$) has been passed through the discharge tube with the Si wafer located in and/or near the microwave plasma. In this case diamond-like carbon products could be obtained.

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Water Repellency on a Nanostructured Superhydrophobic Carbon Fibers Network

  • Ko, Tae-Jun;Her, Eun-Kyu;Shin, Bong-Su;Kim, Ho-Young;Lee, Kwang-Ryeol;Hong, Bo-Ki;Kim, Sae-Hoon;Oh, Kyu-Hwan;Moon, Myoung-Woon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.224-224
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    • 2012
  • For decades, carbon fiber has expanded their application fields from reinforced composites to energy storage and transfer technologies such as electrodes for super-capacitors and lithium ion batteries and gas diffusion layers for proton exchange membrane fuel cell. Especially in fuel cell, water repellency of gas diffusion layer has become very important property for preventing flooding which is induced by condensed water could damage the fuel cell performance. In this work, we fabricated superhydrophobic network of carbon fiber with high aspect ratio hair-like nanostructure by preferential oxygen plasma etching. Superhydrophobic carbon fiber surfaces were achieved by hydrophobic material coating with a siloxane-based hydrocarbon film, which increased the water contact angle from $147^{\circ}$ to $163^{\circ}$ and decreased the contact angle hysteresis from $71^{\circ}$ to below $5^{\circ}$, sufficient to cause droplet roll-off from the surface in millimeter scale water droplet deposition test. Also, we have explored that the condensation behavior (nucleation and growth) of water droplet on the superhydrophobic carbon fiber were significantly retarded due to the high-aspect-ratio nanostructures under super-saturated vapor conditions. It is implied that superhydrophobic carbon fiber can provide a passage for vapor or gas flow in wet environments such as a gas diffusion layer requiring the effective water removal in the operation of proton exchange membrane fuel cell. Moreover, such nanostructuring of carbon-based materials can be extended to carbon fiber, carbon black or carbon films for applications as a cathode in lithium batteries or carbon fiber composites.

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HISTOMORPHOMETRIC AND REMOVAL TORQUE VALUES COMPARISION OF ROUGH SURFACE TITANIUM IMPLANTS (임프란트 표면처리 방법에 따른 골유착의 조직계측학적 분석 및 제거회전력 비교 연구)

  • Lee, Sang-Chul;Song, Woo-Sik
    • Maxillofacial Plastic and Reconstructive Surgery
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    • v.23 no.5
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    • pp.396-405
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    • 2001
  • Osseointegrated implants are used for the fixation of dental prosthesis with good long-term clinical results. In an attempt to improve the quantity and quality of the bone-implant interface, numerous implant modification have been used. Implants surface modifications have been used such as titanium-plasma sprayed, hydroxyapatite-coating, sandblasted, sandblasted and acid-etched, acid-etched. Rough surface implants have greater implant surface area and enhance the bone-implant interface and improve stabilization. The purpose of present study was to evaluate light microscopic and scanning microscopic examinations and removal torque value of newly developed calcium phosphate blast and acid-etched implant in the femur of rabbits. Titanium plasma sprayed(TPS) implant served as controls. After 12 weeks of healing of the femurs of 12 rabitts, the implant-containing segments of femur were removed on bloc and bone block including sections. Histologic examination and histomorphometric and removal torque values comparision were made for two implants. Obtained results are follows: 1. Newly developed calcium phosphate blasted and acid-etched implants were in close contact with bone under light microscopic examinations. 2. New implants showed mean bone-to implant contact 59.8%, whereas TPS implants showed mean bone-to implant contact 54.5% (statistically no difference p<0.05). 3. New implants showed mean bone density 56.7%, whereas TPS implants showed mean bone density 49.2% (statistically difference p<0.05). 4. New implants demonstrated mean removal torque values 40.5Ncm, whereas the mean removal torque values of TPS implants ranged 39.3Ncm. No statistical differences(p<0.05) were observed between two groups of implants nor was there any difference between the two implants at the clinical level.

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Discharging Characteristics of Green cell Using MgO-Coated $Zn_2SiO_4:Mn^{2+}$ Phosphor in Plasma Display Panel

  • Han, Bo-Yong;Jeoung, Byung-Woo;Hong, Gun-Young;Yoo, Jae-Soo;Ha, Chang-Hun;Whang, Ki-Woong
    • 한국정보디스플레이학회:학술대회논문집
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    • 2004.08a
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    • pp.575-578
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    • 2004
  • The charging tendency of $Zn_2SiO_4:Mn^{2+}$ phosphor surface was modified in order to improve discharging characteristic of green cell in an ac-plasma display panel (ac-PDP). The Zinc-silicate ($Zn_2SiO_4:Mn^{2+}$) green-emitting phosphor was coated with magnesium oxide(MgO), which is viable to have positive charge on the surface. After fabricating the green cell with MgO-coated $Zn_2SiO_4:Mn^{2+}$, the electrical and optical properties in the cell were examined. It was found that the dynamic voltage margin could be increased while the address time was reduced. It may be ascribed to the change of charging tendency of $Zn_2SiO_4:Mn^{2+}$ phosphor by MgO coating, which makes it possible to stable wall-charge accumulation. When $Zn_2SiO_4:Mn^{2+}$ phosphor was coated with 1.3wt%-MgO, the address time was reduced 1.2 ${\mu}s$ and the address voltage lowered 25 V without any misfiring problem, compared to those of typical $Zn_2SiO_4:Mn^{2+}$ phosphor layer. The luminescence intensity of green cell using MgO-coated phosphor layer was also improved by 10%.

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