• Title/Summary/Keyword: Organic coatings

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Wear and corrosion coatings by MO-PACVD and dual plasma processes (MO-PACVD 및 복합 플라즈마 공정에 의한 내마모 내식성 코팅)

  • 김선규
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 1999.10a
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    • pp.3-4
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    • 1999
  • 최근 산업이 고속도화, 고능률화 및 고정멸화의 추세로 발전함에 따라 우수한 내마모성, 인성, 고온 안정성 및 내구성을 갖는 공구 및 금형을 요구하게 되었다. 그러나 이와같은 성질들은 어떤 단일 재료에서는 얻을 수 없으며 적당한 기판공구나 금혈위에 내마모성 보호피막을 coating함으로 비교적 저렴하게 얻을 수 있다. 화학증착법으로 TiC, TiN등을 증착시킬때에는 $1000^{\circ}C$정도의 반응온도가 필요하며 이러한 증착온도는 모재가 초경합금일때는 문제가 안되나 강재일 경우 모재의 연화와 칫수변화의 문제를 야기시킨다. 최근에는 플라즈마를 사용하여 증착반응온도를 $550^{\circ}C$ 이하로 낮추는 플라즈마 화학 증착볍(PACVD)이 대두되고 있다. 그러나 이 방법어서 는 뚱착하려는 금속원소가 TiCl4의 형태로 공급되고 있으므로 생성된 층이 염소를 포함하고 있다. 이 층에 잔존하는 염소는 층의 기계적 성질을 저하시키고 층내의 stress를 유발시킨다. 또한 HCI개스의 생성으로 인하여 펌프 및 장비의 부식이 촉진 된다 이러한 결점을 극복하기 위하여 금속유기화합물 전구체(metallo-organic precursor)로 $TiCl_4$를 대체하고자 하는 연구가 활발하게 진행되고 있으며 본 연구실에서 이에 대하여 연구한 결과를 소개하고자 한다. diethylamino titanium을 전구체로 사용하여 $H_2,\;N_2,\;Ar$분위기하에서 pulsed d.c.를 사용하는 MO-PACVD에 의하여 $150~250^{\circ}C$의 저온에서 Al 2024 기판에 TiCN층 형 성을 하였다. 전구체 증발온도는 $74~78^{\circ}C$의 온도범위어야 하며 고경도의 코탱층은 54% duty, 14.2kHz, 450V의 조건에서 얻어졌으며 duty, 주파수, 전압이 증가함에 따라 경도는 저하되었다. 이때의 표면 morphology를 SEM으로 조사한바 dome structure가 크게 발달되었음을 알 수 있었다. 본 실험의 온도 범위내에서 얻은 TiCN 증착반응의 활성화에너지는 7.5Kcal/mol이었다. 증착된 TiCN층은 우수한 내마모섣을 나타내었으며 스크래치테스트 결과 17N의 엄계하중을 나타내었다. 본 연구에서 변화 시킨 duty, 주파수, 전압의 범위에서는 층의 밀착력은 크게 변화하지 않았다. titanium isopropoxide를 전구체로 사용하여 Hz, Nz 분위기하에서 d.c.를 사용하는 MO-PACVD에 의하여 Ti(NCO) 코팅층을 SKDll, SKD61, SKH9 공구강에 형성시키는 공정을 개발하였다. 최적의 Ti(NCO) 코탱층을 얻기 위해 유입전구체 부피%의 양은 향착압력의 5%를 넘지 않아야 되고 수소와 젤소 가스비가 1:1일 때 가장 높은 코팅층의 경도값을 나타내었다. 수소와 질소 가스비가 3:7일 때 TiFeCr(NCO)의 복화합물 코팅층이 형성됨을 알 수 있었고 500t의 증착온도에서 얻은 Ti(NCO) 코팅층이 높은 경도값과 좋은 내식성을 나타내었다. 또한 이와같은 Ti(NCO) 코팅공정과 본 실험실에서 개발한 확산층만 형성시키는 plsma nitriding 공정을 결합하여 복합코탱층을 형성하였는데 이 복합코팅층은 고경도와 우수한 내마모성, 내식성 뿐만 아니라 10)N 이상의 뛰어난 밀착력을 나타내었다. 현재 많이 사용되고 있는 PVD법은 step coverage가 좋지 않은 점과 cost intensive p process라는 단점이 있다. MO-PACVD법은 이러한 문제를 해결할 수 있는 방법으로서 앞으로 지속적인 도전이 요구되는 분야이다.

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A Study on the Preparation of Aluina & Titania Sols for Coatings (코팅용 알루미타, 티타니아솔 제조에 관한 연구)

  • Kim, Chu-Hui;Choe, Hyeong-Su;Jo, Yeong-Sang;Im, Jong-Ju
    • Korean Journal of Materials Research
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    • v.4 no.3
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    • pp.319-328
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    • 1994
  • Aluminium and titanium precursors containing $\beta$-diketonate ligands were used for the synthesis of polymeric sols of alumina and titania by sol-gel methods. To prepare polymeric sols by solgel processing, we synthesized modified precursors having chelating organic ligands. With these precursors it was found to be possible to control both hydrolysis and polycondensation reaction rates which resulted in ultrafine particles few nms of average size. The optimum molar ratio of acid to alkoxide for alumina sol was 0.3-0.4 and that of water to alkoxide &as 1. On the other hand, the corresponding ratios for titania sol were found be 0.25-0.20 and 1 respectively. Dynamic light scattering measurements indicated that the average particle size in both sols was in the order of few nms. SEM photographs were taken to observe crack-free and smooth surfaces of coated membranes after sintering at $450^{\circ}C$. Alumina coated membrane on a slide glass had about 4-4.5$\mu \textrm{m}$, thickness and titania coated one had 2-2.5$\mu \textrm{m}$, thickness. And according to TEM photographs, the grain size of titania was smaller than 30nm and that of alumina was in the range of few $\AA$s to 2nms. An X-ray diffraction study revealed that alumina was $\gamma$ phase and titania was anatase crystal.

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Effects of Passivation Thin Films by Spray Coatings on Properties of Flexible CIGS Solar Cells (스프레이코팅법에 의한 패시베이션 박막이 플렉시블 CIGS 태양전지의 특성에 미치는 영향)

  • Lee, Sang Hee;Park, Byung Min;Kim, Ki Hong;Chang, Young Chul;Pyee, Jaeho;Chang, Ho Jung
    • Journal of the Microelectronics and Packaging Society
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    • v.23 no.3
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    • pp.57-61
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    • 2016
  • In order to protect the solar cells from the moisture and oxygen, we evaluated the electrical and optical properties for the $Cu(In,Ga)Se_2$ (CIGS) solar cells which were prepared by the spray coating method. Generally, the EVA (ethylene-vinyl acetate) films are laminated to protect the CIGS flexible solar cells, which results in a high cost process due to complicated devices. In this study, we tried to prepare the protection layers of the flexible CIGS flexible solar cells by using spray coating method instead of conventional laminating films in order to reduce the device weight as well as the process time. The CIGS solar cells with spray coating method showed an enhanced efficiency than the before treated sample (2.77% to 2.93%) and relatively proper water vapor transmission rate of the solar cells about 62.891 gm/[$m^2-day$].

Tuning of the Interparticle interactions in ultrafine ferrihydrite nanoparticles

  • Knyazev, Yuriy V.;Balaev, Dmitry A.;Yaroslavtsev, Roman N.;Krasikov, Aleksandr A.;Velikanov, Dmitry A.;Mikhlin, Yuriy L.;Volochaev, Mikhail N.;Bayukov, Oleg A.;Stolyar, Sergei V.;Iskhakov, Rauf S.
    • Advances in nano research
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    • v.12 no.6
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    • pp.605-616
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    • 2022
  • We prepared two samples of ultrafine ferrihydrite (FH) nanoparticle ensembles of quite a different origin. First is the biosynthesized sample (as a product of the vital activity of bacteria Klebsiella oxytoca (hereinafter marked as FH-bact) with a natural organic coating and negligible magnetic interparticle interactions. And the second one is the chemically synthesized ferrihydrite (hereinafter FH-chem) without any coating and high level of the interparticle interactions. The interparticle magnetic interactions have been tuned by modifying the nanoparticle surface in both samples. The coating of the FH-bact sample has been partially removed by annealing at 150℃ for 24 h (hereinafter FH-annealed). The FH-chem sample, vice versa, has been coated (1.0 g) with biocompatible polysaccharide (arabinogalactan) in an ultrasonic bath for 10 min (hereinafter FH-coated). The changes in the surface properties of nanoparticles have been controlled by XPS. According to the electron microscopy data, the modification of the nanoparticle surface does not drastically change the particle shape and size. A change in the average nanoparticle size in sample FH-annealed to 3.3 nm relative to the value in the other samples (2.6 nm) has only been observed. The estimated particle coating thickness is about 0.2-0.3 nm for samples FH-bact and FH-coated and 0.1 nm for sample FH-annealed. Mössbauer and magnetization measurements are definitely shown that the drastic change in the blocking temperature is caused by the interparticle interactions. The experimental temperature dependences of the hyperfine field hf>(T) for samples FH-bact and FH-coated have not revealed the effect of interparticle interactions. Otherwise, the interparticle interaction energy Eint estimated from the hf>(T) for samples FH-chem and FH-annealed has been found to be 121kB and 259kB, respectively.

Adsorption and Transfer of Trace Elements in Repellent Soils (토양 소수성에 따른 미량원소의 흡착 및 이동)

  • Choi, Jun-Yong;Lee, Sang-Soo;Ok, Yong-Sik;Chun, So-Ul;Joo, Young-Kyoo
    • Korean Journal of Soil Science and Fertilizer
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    • v.45 no.2
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    • pp.204-208
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    • 2012
  • Water repellency which affects infiltration, evaporation, erosion and other water transfer mechanisms through soil has been observed under several natural conditions. Water repellency is thought to be caused by hydrophobic organic compounds, which are present as coatings on soil particles or as an interstitial matter between soil particles. This study was conducted to evaluate the characteristics of the water repellent soil and transport characteristics of trace elements within this soil. Capillary height of the water repellent soil was measured. Batch and column studies were accompanied to identify sorption and transport mechanism of trace elements such as $Cu^{2+}$, $Mn^{2+}$, $Fe^{2+}$, $Zn^{2+}$ and $Mo^{5+}$. Difference of sorption capacity between common and repellent soils was observed depended on the degree of repellency. In the column study, the desorption of trace elements and the spatial concentration distribution as a function of time were evaluated. The capillary height was in the repellency order of 0% > 15% > 40% > 70% > 100%. No water was absorbed in soil indicating >70% repellency. Using trace elements, $Fe^{2+}$ and $Mo^{5+}$ showed higher sorption capacity in the repellent soil than in non-repellent soil. The sorption performance of $Fe^{2+}$ was found to be in the repellency order of 40% > 15% > 0%. Our results found that transfer of $Mo^{5+}$ had similar sorption tendency in soils having 0%, 15% and 40% repellency at the beginning, however, the higher desorption capacity was observed as time passes in the repellent soil compared to in non-repellent soils.

Sorption of Arsenite Using Nanosized Mackinawite (FeS)-Coated Silica Sand (나노 크기 매킨나와이트로 코팅된 규사를 이용한 아비산염의 흡착)

  • Lee, Seungyeol;Kang, Jung Chun;Park, Minji;Yang, Kyounghee;Jeong, Hoon Young
    • Journal of the Mineralogical Society of Korea
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    • v.25 no.4
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    • pp.185-195
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    • 2012
  • Due to the high reduction and sorption capacity as well as the large specific surface area, nanosized mackinawite (FeS) is useful in reductively transforming chlorinated organic pollutants and sequestering toxic metals and metalloids. Due to the dynamic nature in its colloid stability, however, nanosized FeS may be washed out with the groundwater flow or result in aquifer clogging via particle aggregation. Thus, these nanoparticles should be modified such as to be built into permeable reactive barriers. This study employed coating methods in efforts to facilitate the installation of permeable reactive barriers of nanosized mackinawite. In applying the methods, nanosized mackinawite was coated on non-treated silica sand (NTS) and chemically treated silica sand (CTS). For both silica sands, the maximum coating of mackinawite occurred around pH 5.4, the condition of which was governed by (1) the solubility of mackinawite and (2) the surface charge of both silica and mackinawite. Under this pH condition, the maximum coating by NTS and CTS were found to be 0.101 mmol FeS/g and 0.043 mmol FeS/g respectively, with such elevated coatings by NTS likely linked with impurities (e.g., iron oxides) on its surface. Arsenite sorption experiments were performed under anoxic conditions using uncoated silica sands and those coated with mackinawite at the optimal pH to compare their reactivity. At pH 7, the relative sorption efficiency between uncoated NTS and coated NTS changed with the initial concentration of arsenite. At the lower initial concentration, uncoated NTS showed the higher sorption efficiency, whereas at the higher concentration, coated NTS exhibited the higher sorption efficiency. This could be attributed to different sorption mechanisms as a function of arsenite concentration: the surface complexation of arsenite with the iron oxide impurity on silica sand at the low concentration and the precipitation as arsenic sulfides by reaction with mackinawite coating at the high concentration. Compared to coated NTS, coated CTS showed the lower arsenite removal at pH 7 due to its relatively lower mackinawite coating. Taken together, our results indicate that NTS is a more effective material than CTS for the coating of nanosized mackinawite.

Electrochemical Characterization of Anti-Corrosion Film Coated Metal Conditioner Surfaces for Tungsten CMP Applications (텅스텐 화학적-기계적 연마 공정에서 부식방지막이 증착된 금속 컨디셔너 표면의 전기화학적 특성평가)

  • Cho, Byoung-Jun;Kwon, Tae-Young;Kim, Hyuk-Min;Venkatesh, Prasanna;Park, Moon-Seok;Park, Jin-Goo
    • Journal of the Microelectronics and Packaging Society
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    • v.19 no.1
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    • pp.61-66
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    • 2012
  • Chemical Mechanical Planarization (CMP) is a polishing process used in the microelectronic fabrication industries to achieve a globally planar wafer surface for the manufacturing of integrated circuits. Pad conditioning plays an important role in the CMP process to maintain a material removal rate (MRR) and its uniformity. For metal CMP process, highly acidic slurry containing strong oxidizer is being used. It would affect the conditioner surface which normally made of metal such as Nickel and its alloy. If conditioner surface is corroded, diamonds on the conditioner surface would be fallen out from the surface. Because of this phenomenon, not only life time of conditioners is decreased, but also more scratches are generated. To protect the conditioners from corrosion, thin organic film deposition on the metal surface is suggested without requiring current conditioner manufacturing process. To prepare the anti-corrosion film on metal conditioner surface, vapor SAM (self-assembled monolayer) and FC (Fluorocarbon) -CVD (SRN-504, Sorona, Korea) films were prepared on both nickel and nickel alloy surfaces. Vapor SAM method was used for SAM deposition using both Dodecanethiol (DT) and Perfluoroctyltrichloro silane (FOTS). FC films were prepared in different thickness of 10 nm, 50 nm and 100 nm on conditioner surfaces. Electrochemical analysis such as potentiodynamic polarization and impedance, and contact angle measurements were carried out to evaluate the coating characteristics. Impedance data was analyzed by an electrical equivalent circuit model. The observed contact angle is higher than 90o after thin film deposition, which confirms that the coatings deposited on the surfaces are densely packed. The results of potentiodynamic polarization and the impedance show that modified surfaces have better performance than bare metal surfaces which could be applied to increase the life time and reliability of conditioner during W CMP.