• Title/Summary/Keyword: XRD (x-ray diffraction)

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A Study on the Fabrication and Characteristics of ITO Thin Film Deposited by Magnetron Sputtering Method (마그네트론 스퍼터링법을 이용한 Indium-Tin Oxide 박막의 제작과 그 특성에 관한 연구)

  • 조길호;김여중;김성종;문경만;이명훈
    • Journal of Advanced Marine Engineering and Technology
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    • v.24 no.6
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    • pp.61-69
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    • 2000
  • Indium-Tin Oxide (ITO) films were prepared on the commercial glass substrate by the Magnetron Sputtering method. The target was a 90wt.% $In_2O_3$-10wt.% $SnO_2$with 99.99% purity. The ITO films deposited by changing the partial pressure of oxygen gas ($O_2$/(Ar+$O_2$)) of 2, 3 and 5% as well as by changing the substrate temperature of $300^{\circ}C$ or $500^{\circ}C$. The influence of substrate pre-annealing and pre-cleaning on the quality of ITO film were examined, in which the substrate temperature was $500^{\circ}C$ and oxygen partial pressure was 3%. The characteristics of films were examined by the 4-point probe, Hall effect measurement system, SEM, AFM, Spectrophotometer, and X-ray diffraction. The optimum ITO films have been obtained when the substrate temperature is $500^{\circ}C$ and oxygen partial pressure is 3%. At optimum condition, the film showed transmittance of 81%, sheet resistivity of $226\Omegatextrm{cm}^2$, resistivity($\rho$) of $5.4\times10^{-3}\Omega$cm, carrier concentration of $1.0\times10^{19}cm^{-3}$, and carrier mobility of $150textrm{cm}^2$Vsec. From XRD spectrum, c(222) plane was dominant in the case of substrate temperature at $300^{\circ}C$, without regarding to oxygen partial pressure. However, in the case of substrate temperature at $500^{\circ}C$, c(400) plane was grown together with c(222) plane, only for oxygen partial pressure of 2 and 3%. In both case of chemical and ultrasonic cleaning without pre-annealing the substrate, it showed much almost same sheet resistivity, resistivity($\rho$), transmittance, carrier concentration, and carrier mobility. In case of $500^{\circ}C$/60min pre-annealing before ITO film deposited, both transimittance and carrier mobility are better than no pre-annealing, because pre-annealing is supposed to remove alkari ions diffusion from substrate. ITO film deposited on the Corning 0080 sybstrate showed a little bit better sheet resistivity, resistivity($\rho$), transimittance, carrier concentration than the film deposited on commercial glass. But no differences between Corning substrate and pre-annealed commercial glass substrate are found.

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The electrical properties of PLZT thin films on ITO coated glass with various post-annealing temperature (ITO 기판에 제작된 PLZT 박막의 후열처리 온도에 따른 전기적 특성평가)

  • Cha, Won-Hyo;Youn, Ji-Eon;Hwang, Dong-Hyun;Lee, Chul-Su;Lee, In-Seok;Sona, Young-Guk
    • Journal of the Korean Vacuum Society
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    • v.17 no.1
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    • pp.28-33
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    • 2008
  • Lanthanum modified lead zirconate titanate ($Pb_{1.1}La_{0.08}Zr_{0.65}Ti_{0.35}O_3$) thin films were fabricated on indium doped tin oxide (ITO)-coated glass substrate by R.F magnetron sputtering method. The thin films were deposited at $500^{\circ}C$ and post-annealed with various temperature ($550-750^{\circ}C$) by rapid thermal annealing technique. The structure and morphology of the films were characterized with X-ray diffraction (XRD) and atomic force microscopy (AFM) respectively. The hysteresis loops and fatigue properties of thin films were measured by precision material analyzer. As the annealing temperature was increased, the remnant polarization value was increased from $10.6{\mu}C/cm^2$ to $31.4{\mu}C/cm^2$, and coercive field was reduced from 79.9 kV/cm to 60.9 kV/cm. As a result of polarization endurance analysis, the remnant polarization of PLZT thin films annealed at $700^{\circ}C$ was decreased 15% after $10^9$ switching cycles using 1MHz square wave form at ${\pm}5V$.

Enhanced Light Harvesting by Fast Charge Collection Using the ITO Nanowire Arrays in Solid State Dye-sensitized Solar Cells

  • Han, Gill Sang;Yu, Jin Sun;Jung, Hyun Suk
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.463-463
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    • 2014
  • Dye-sensitized solar cells (DSSCs) have generated a strong interest in the development of solid-state devices owing to their low cost and simple preparation procedures. Effort has been devoted to the study of electrolytes that allow light-to-electrical power conversion for DSSC applications. Several attempts have been made to substitute the liquid electrolyte in the original solar cells by using (2,2',7,7'-tetrakis (N,N-di-p-methoxyphenylamine)-9-9'-spirobi-fluorene (spiro-OMeTAD) that act as hole conductor [1]. Although efficiencies above 3% have been reached by several groups, here the major challenging is limited photoelectrode thickness ($2{\mu}m$), which is very low due to electron diffusion length (Ln) for spiro-OMeTAD ($4.4{\mu}m$) [2]. In principle, the $TiO_2$ layer can be thicker than had been thought previously. This has important implications for the design of high-efficiency solid-state DSSCs. In the present study, we have fabricated 3-D Transparent Conducting Oxide (TCO) by growing tin-doped indium oxide (ITO) nanowire (NWs) arrays via a vapor transport method [3] and mesoporous $TiO_2$ nanoparticle (NP)-based photoelectrodes were prepared using doctor blade method. Finally optimized light-harvesting solid-state DSSCs is made using 3-D TCO where electron life time is controlled the recombination rate through fast charge collection and also ITO NWs length can be controlled in the range of over $2{\mu}m$ and has been characterized using field emission scanning electron microscopy (FE-SEM). Structural analyses by high-resolution transmission electron microscopy (HRTEM) and X-Ray diffraction (XRD) results reveal that the ITO NWs formed single crystal oriented [100] direction. Also to compare the charge collection properties of conventional NPs based solid-state DSSCs with ITO NWs based solid-state DSSCs, we have studied intensity modulated photovoltage spectroscopy (IMVS), intensity modulated photocurrent spectroscopy (IMPS) and transient open circuit voltages. As a result, above $4{\mu}m$ thick ITO NWs based photoelectrodes with Z907 dye shown the best performing device, exhibiting a short-circuit current density of 7.21 mA cm-2 under simulated solar emission of 100 mW cm-2 associated with an overall power conversion efficiency of 2.80 %. Finally, we achieved the efficiency of 7.5% by applying a CH3NH3PbI3 perovskite sensitizer.

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Structural and Electrical Properties of Fluorine-doped Zinc Tin Oxide Thin Films Prepared by Radio-Frequency Magnetron Sputtering

  • Pandey, Rina;Cho, Se Hee;Hwang, Do Kyung;Choi, Won Kook
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.335-335
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    • 2014
  • Over the past several years, transparent conducting oxides have been extensively studied in order to replace indium tin oxide (ITO). Here we report on fluorine doped zinc tin oxide (FZTO) films deposited on glass substrates by radio-frequency (RF) magnetron sputtering using a 30 wt% ZnO with 70 wt% SnO2 ceramic targets. The F-doping was carried out by introducing a mixed gas of pure Ar, CF4, and O2 forming gas into the sputtering chamber while sputtering ZTO target. Annealing temperature affects the structural, electrical and optical properties of FZTO thin films. All the as-deposited FZTO films grown at room temperature are found to be amorphous because of the immiscibility of SnO2 and ZnO. Even after the as-deposited FZTO films were annealed from $300{\sim}500^{\circ}C$, there were no significant changes. However, when the sample is annealed temperature up to $600^{\circ}C$, two distinct diffraction peaks appear in XRD spectra at $2{\Theta}=34.0^{\circ}$ and $52.02^{\circ}$, respectively, which correspond to the (101) and (211) planes of rutile phase SnO2. FZTO thin film annealed at $600^{\circ}C$ resulted in decrease of resistivity $5.47{\times}10^{-3}{\Omega}cm$, carrier concentration ~1019 cm-3, mobility~20 cm2 V-1s-1 and increase of optical band gap from 3.41 to 3.60 eV with increasing the annealing temperatures and well explained by Burstein-Moss effect. Change of work function with the annealing temperature was obtained by ultraviolet photoemission spectroscopy. The increase of annealing temperature leads to increase of work function from ${\phi}=3.80eV$ (as-deposited FZTO) to ${\phi}=4.10eV$ ($600^{\circ}C$ annealed FZTO) which are quite smaller than 4.62 eV for Al-ZnO and 4.74 eV for SnO2. Through X-ray photoelectron spectroscopy, incorporation of F atoms was found at around the binding energy of 684.28 eV in the as-deposited and annealed FZTO up to 400oC, but can't be observed in the annealed FZTO at 500oC. This result indicates that F atoms in FZTO films are loosely bound or probably located in the interstitial sites instead of substitutional sites and thus easily diffused into the vacuum from the films by thermal annealing. The optical transmittance of FZTO films was higher than 80% in all specimens and 2-3% higher than ZTO films. FZTO is a possible potential transparent conducting oxide (TCO) alternative for application in optoelectronics.

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Deterioration of the Rock-carved Seated Buddha at Golguram Hermitage, Gyeongju and Effect of the Ethylsilicate Consolidant (경주 골굴암 마애여래좌상 구성암석의 손상과 에틸실리케이트 암석강화제의 효과)

  • Do, Jin Young
    • Journal of the Mineralogical Society of Korea
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    • v.30 no.2
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    • pp.71-81
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    • 2017
  • Rock properties and the effects of chemicals that were used for conservation were studied for effective conservation treatment of Seated Buddha rock carving, which is composed of grayish white tuff, at Golguram Hermitage, Gyeongju. The rocks contain 3-5% montmorillonite, a swelling mineral and reacting with water, the d spacing of swelling minerals was increased (1.54-2.69%). On the one hand, the physical properties of the rock samples, such as surface hardness, water absorption rate, and porosity improved after the application of ethyl silicate-based stone strengthener. On the other, the interlayer of swelling minerals decreased and greater the of swelling mineral content, the greater is the extent of swelling (4.23-12.12%). When the ethyl silicate-based stone strengthener was applied after pretreatment with a swelling inhibitor, the physical properties were similar to those of the stone strengthener alone. There was no interlayer spacing change of swelling minerals due to swelling inhibition treatment; however, when the stone strengthener was applied after the swelling inhibitor, interlayer changes were similar to those when only the stone strengthener was treated (4.10-11.85%). Though the peak intensity of swelling minerals in X-ray diffraction pattern decreased, the effect of the swelling inhibitor was almost negligible. Therefore, it is not appropriate to use ethyl silicate-based stone strengthener for Golgulam rock containing swelling minerals and supplementing them with a swelling inhibition system is not effective. Because weathering rapidly progresses when swelling minerals contact moisture, for now, measures to prevent water contact, such as expansion of the canopy, are needed in the lower and side parts of the carving.

Formation of Environment Friendly Electrodeposition Films by CO2 Gas Dissolved in Seawater and Their Corrosion Resistance (해수 중 CO2 기체의 유입에 의한 환경 친화적인 전착 코팅막의 형성과 그 내식특성)

  • Lee, Sung-Joon;Kim, Hye-Min;Lee, Seul-Gee;Moon, Kyung-Man;Lee, Myeong-Hoon
    • Journal of the Korean institute of surface engineering
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    • v.47 no.1
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    • pp.39-47
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    • 2014
  • The peculiar feature of cathodic protection in seawater has the capability to form mineral calcareous deposits such as magnesium and calcium on metal surfaces. It is assumed that $OH^-$ ions are generated close to the metal surface as a result of cathodic protection and generated $OH^-$ ions increases the pH of the metal/seawater interface outlined as the following formulae. (1) $O_2+2H_2O+4e{\rightarrow}4OH^-$, or (2) $2H_2O+2e{\rightarrow}H_2+2OH^-$. And high pH causes precipitation of $Mg(OH)_2$ and $CaCO_3$ in accordance with the following formulae. (1) $Mg^{2+}+2OH^-{\rightarrow}Mg(OH)_2$, (2) $Ca^{2+}+CO{_3}^{2-}{\rightarrow}CaCO_3$. The focus of this study was to increase the amount of $CO{_3}^{2-}$ with the injection of $CO_2$ gas to the solution for accelerating process of the following formulae. (1) $H_2O+CO_2{\rightarrow}H_2CO_3$, (2) $HCO^{3-}{\rightarrow}{H^+}+CO{_3}^{2-}$. Electrodeposit films were formed by an electro-deposition technique on steel substrates in solutions of both natural seawater and natural seawater dissolved $CO_2$ gas with different current densities, over different time periods. The contents of films were investigated by scanning electron microscopy(SEM) and X-ray diffraction(XRD). The adhesion and corrosion resistance of the coating films were evaluated by anodic polarization. From an experimental result, only $CaCO_3$ were found in solution where injected $CO_2$ gas regardless of current density. In case of injecting the $CO_2$ gas, weight gain of electrodeposits films hugely increased and it had appropriate physical properties.

Effect of Deposition Parameter and Mixing Process of Raw Materials on the Phase and Structure of Ytterbium Silicate Environmental Barrier Coatings by Suspension Plasma Spray Method (서스펜션 플라즈마 스프레이 코팅법으로 제조된 Ytterbium Silicate 환경차폐코팅의 상형성 및 구조에 미치는 증착인자 및 원료혼합 공정의 영향)

  • Ryu, Ho-lim;Choi, Seon-A;Lee, Sung-Min;Han, Yoon-Soo;Choi, Kyun;Nahm, Sahn;Oh, Yoon-Suk
    • Journal of Powder Materials
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    • v.24 no.6
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    • pp.437-443
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    • 2017
  • SiC-based composite materials with light weight, high durability, and high-temperature stability have been actively studied for use in aerospace and defense applications. Moreover, environmental barrier coating (EBC) technologies using oxide-based ceramic materials have been studied to prevent chemical deterioration at a high temperature of $1300^{\circ}C$ or higher. In this study, an ytterbium silicate material, which has recently been actively studied as an environmental barrier coating because of its high-temperature chemical stability, is fabricated on a sintered SiC substrate. $Yb_2O_3$ and $SiO_2$ are used as the raw starting materials to form ytterbium disilicate ($Yb_2Si_2O_7$). Suspension plasma spraying is applied as the coating method. The effect of the mixing method on the particle size and distribution, which affect the coating formation behavior, is investigated using a scanning electron microscope (SEM), an energy dispersive spectrometer (EDS), and X-ray diffraction (XRD) analysis. It is found that the originally designed compounds are not effectively formed because of the refinement and vaporization of the raw material particles, i.e., $SiO_2$, and the formation of a porous coating structure. By changing the coating parameters such as the deposition distance, it is found that a denser coating structure can be formed at a closer deposition distance.

Development and Characterization of Horse Bone-derived Natural Calcium Phosphate Powders

  • Jang, Kyoung-Je;Cho, Woo Jae;Seonwoo, Hoon;Kim, Jangho;Lim, Ki Taek;Chung, Pill-Hoon;Chung, Jong Hoon
    • Journal of Biosystems Engineering
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    • v.39 no.2
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    • pp.122-133
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    • 2014
  • Purpose: This study was to develop an effective process for fabricating biocompatible calcium phosphate powders (CPPs) using horse bones, and to investigate the characteristics of them. Methods: The characteristics of horse bone powders (HBPs) were investigated according to the different osseous tissue types (compact bone and cancellous bone), bone types (spine and tibia), pretreatment methods (cold water, $H_2O_2$, and hot water), sintering time (4, 8 and 12h), and sintering temperature (600, 900, 1100 and $1300^{\circ}C$). In addition, the grinding methods were compared based on the wet grinding (ball mill) and dry grinding (blade grinder) method to make it as powders. Finally, their cytotoxicity and cell viability were checked. Results: Regardless of the types of osseous tissues and bones, HBPs were well fabricated as biocompatible CPPs. It was also found that the pretreatment methods did not influence on the resultants, showing well-fabricated HBPs. Considering the processing time, the hot water method was the most suitable compared to other pretreatment methods. Further, 12h-sintering time was sufficient to remove residual organic compounds. The sintering temperatures greatly affected the properties of bone powders fabricated. The x-ray diffraction (XRD) peak of horse bone sintered at $600^{\circ}C$ was most closed to that of hydroxyapatite (HA). Our bioactivity study demonstrated that the HBPs fabricated by sintering horse bones at $1300^{\circ}C$ showed the best performance in terms of cell viability whereas the HBPs $1100^{\circ}C$ showed the cytotoxicity. Conclusions: Using various types of horse bone tissues, biocompatible CPPs were successfully developed. We conclude that the HBPs may have a great potential as biomaterials for various biological applications including bone tissue engineering.

Effects of Annealing on Ni/Au Ohmic Contact to Nonpolar p-type GaN

  • Lee, Dong-Min;Kim, Jae-Gwan;Yang, Su-Hwan;Kim, Jun-Yeong;Lee, Seong-Nam;Lee, Ji-Myeon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.358-359
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    • 2012
  • 최근 분극 특성이 상이한 무분극 GaN 에피성장에 관한 심도 있는 연구와 함께 전자-전공 캐리어의 주입 및 캐리어의 거동, 방출되는 편광 특성 및 다양한 물리적 특성들에 대해 보고되고 있으며, 광학적 특성 및 물리적 특성의 확보를 위한 많은 연구가 활발히 진행 중이다 [1]. GaN의 ohmic 접촉(ohmic contact)의 형성은 발광 다이오드(light emitting diode), 레이저 다이오드(Laser), 태양전지(solar cell)와 같은 고신뢰도, 고효율 광전자 소자를 제조하기 위해서는 매우 중요하다 [2]. 그러나 이와 함께 병행 되어야 할 무분극 p-GaN 의 ohmic contact에 관한 연구는 많이 이루어지고 있지 않는 실정이다. 따라서 본 논문에서는 r-plane 사파이어 기판 상에 성장된 p-GaN에서의 ohmic 접촉 형성 연구를 위하여 Ni/Au ohmic 전극의 접촉저항 특성을 연구하였다. 본 실험에서는 성장된 a-plane GaN의 Hole농도가 $3.09{\times}1017cm3$ 인 시편을 사용하였다. E-beam evaporation 장비를 이용하여 Ni/Au를 각각 20 nm 그리고80 nm 증착 하였으며 비접촉저항을 측정하기 위해 Circle-Transfer Length Method (C-TLM) 패턴을 사용하였다. 샘플은 RTA (Rapid Thermal Annealing)를 사용하여 $300^{\circ}C$에서 $700^{\circ}C$까지 온도를 변화시키며 전기적 특성을 비교하여 그림 1(a) 나타내었다. 그림에서 알 수 있듯이 $400^{\circ}C$에서 가장 낮은 비접촉저항 값인 $6.95{\times}10-3{\Omega}cm2$를 얻을 수 있음을 발견하였다. 이 때의 I-V curve 도 그림1(b)에 나타낸 바와 같이 열처리에 의해 크게 향상됨을 알 수 있다. 그러나, $500^{\circ}C$ 이상 온도를 증가시키면 다시 비접촉 저항이 증가하는 것을 관찰하였다. XRD (x-Ray Diffraction) 분석을 통하여 $400^{\circ}C$ 이상열처리 온도가 증가하면 금속 표면에 $NiO_2$가 형성되며, 이에 따라 오믹특성이 저하 된다고 사료된다. 또한 $Ni_3N$의 존재를 확인 하였으며 이는 nonpolar surface의 특성으로 인해 nitrogen out diffusion 현상이 동시에 발생하여 계면에는 dopant로 작용하는 질소 공공을 남기고 표면에 $Ni_3N$을 형성하여 ohmic contact의 특성이 저하되기 때문인 것으로 사료된다.

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Copper Film Growth by Chemical Vapor Deposition: Influence of the Seeding Layer (ICB seeding에 의한 CVD Cu 박막의 증착 및 특성 분석)

  • Yoon, Kyoung-Ryul;Choi, Doo-Jin;Kim, Seok;Kim, Ki-Hwan;Koh, Seok-Keun
    • Korean Journal of Materials Research
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    • v.6 no.7
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    • pp.723-732
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    • 1996
  • Cu films were deposited by chemical wapor deposition on the as-received substrates (TiN/Si) and three kinds of Cu-seeded substrates (Cu/TiN/Si) which had seeding layer in the thick ness of 5 ${\AA}$ and 130 ${\AA}$ coated by ICB(Ionized Cluster Beam) method. The effect of Cu seeding layers on the growth rate, crystallinity, grain size uniformity and film adhesion strength of final CVD-Cu films was investigated by scanning eletron microscopy(SEM), X-ray diffractometry and scratch test. The growth rate was found to incresase somewhat in the case of ICB-seeding. The XRD patterns of the Cu films on the as-received substrate and ICB Cu-seeded substrates exhibited the diffraction peaks corresponding to FCC phase, but the peak intensity ratio($I_{111}/I_{200}$) of Cu films deposited on the ICB Cu-seeded substrates increased compared with that of Cu films on the as-received substrate. The resistivity of final Cu film on 40 ${\AA}$ seeded substrate was observed as the lowest value, 2.42 $\mu\Omega\cdot$cm compared with other Cu films. In adhesion test, as the seeding thickness increased from zero to 130 ${\AA}$, the adhesion strength increased from 21N to 27N.

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