• Title/Summary/Keyword: Gas Electron Diffraction

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Formation of Magnesium Films on Galvanized Steel Substrates by PVD Method at Nitrogen Gas Pressures and Their Corrosion Resistances (질소가스 중 PVD법에 의해 용융아연도금 강판 상에 형성한 마그네슘 막의 내식특성)

  • Eom, Jin-Hwan;Park, Jae-Hyeok;Hwang, Seong-Hwa;Park, Jun-Mu;Yun, Yong-Seop;Lee, Myeong-Hun
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.182-182
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    • 2016
  • 철강은 기본적으로 강도가 우수하고 그 매장량이 풍부할 뿐만 아니라 대량생산이 가능하다 또한 다른 금속과 합금을 구성하여 또 다른 특성을 부여할 수 있기 때문에 현재 전 세계 금속 생산량의 95%를 차지할 정도로 많이 사용되며, 각종 산업과 기술이 발달함에 따라 그 중요도는 점점 더 커져가고 있다. 하지만 철강은 사용 환경 중 부식에 의해 그 수명과 성능이 급격히 저하되기 때문에 내식성을 향상시키기 위하여 도장이나 도금 등의 표면처리를 포함한 다양한 방법이 적용되고 있다. 그 중 철강재의 도금 표면처리방법은 주로 아연을 이용한 용융도금이나 전기도금 등과 같은 습식 프로세스가 널리 사용되고 있다. 여기서 아연은 철보다 이온화 경향은 크나 대기 환경 중 산소와 물과 반응하여 Zn(OH)2와 같은 화합물을 형성함으로써 철강재 표면상 부식인자를 차단(Barrier)함은 물론 사용 중 철 모재가 노출되는 결함이 발생하는 경우에는 철을 대신하여 희생양극(Sacrificial Anode) 역할을 하기 때문에 철의 부식방식용 금속으로 가장 많이 사용되고 있다. 한편 최근에는 철강의 사용 환경이 다양해짐은 물론 가혹해지고 있어서 이에 따른 내식성 향상이 계속해서 요구되고 있는 추세이다. 따라서 본 연구에서는 철강재의 내식성을 향상시키기 위한 일환으로 현재 많이 사용되고 있는 용융아연도금 강판 상에 아연보다 활성이 높은 마그네슘(Mg)을 건식 프로세스 방법 중에 하나인 PVD(Physical Vapour Deposition)법에 의해 코팅하는 것을 시도하였다. 일반적으로 PVD법에 의해 진공증착하는 경우에는 그 도입가스로써 불활성가스인 아르곤(Ar)을 사용하는 경우가 대부분이나 여기서는 상대적으로 비활성이면서 그 크기가 작은 질소(N2)가스를 도입하여 그 증착 막의 몰포로지는 물론 결정구조도 제어하여 그 내식특성을 향상시키고자 하였다. 본 연구에서는 철강재의 내식성을 향상시키기 위한 방법으로 마그네슘(Mg)를 PVD(Physical Vapor Deposition)법 중 진공증착법(Vacuum Deposition)을 사용하여 용융아연도금 강판 상에 마그네슘 증착 막을 형성하였다. 즉, 여기서는 진공증착 중 질소(Nitrogen, N2)가스를 도입하여 진공챔버(Vacuum Chamber)내의 진공도를 $1{\times}10^{-1}$, $1{\times}10^{-2}$, $1{\times}10^{-3}$, $1{\times}10^{-4}$로 조절하며 제작하였다. 또한 제작된 시편에 대해서는 SEM(Scanning Electron Microscope) 및 XRD(X-Ray Diffraction)을 사용하여 형성된 아연도금상 마그네슘 막의 표면 몰포로지 및 결정구조의 변화를 분석함은 물론 침지시험, 염수분무시험, 분극시험을 통해 이 막들에 대한 내식특성을 분석 평가하였다. 상기 실험결과에 의하면, 진공 가스압이 증가됨에 따라 마그네슘 막의 두께는 감소하였으며, 그 몰포로지의 단면은 주상정(Columnar)에서 입상정(Granular) 구조로 변화하며 표면의 결정립은 점점 미세화 되는 경향을 나타냈다. 이때의 표면의 결정배향성(Crystal orientation)은 표면에너지가 상대적으로 큰 면이 우세하게 나타나는 경향이 있었다. 또한 본 실험에서 형성한 진공증착 막은 비교재인 용융아연도금강판보다 우수한 내식성을 나타냈고, 본 형성 막 중에는 마그네슘 막 두께가 작음에도 불구하고 질소 가스압이 가장 큰 조건일수록 내식성이 우수한 경향을 나타냈다. 이상의 결과는 철강재의 내식성 향상을 위한 응용표면처리설계에 기초적인 지침을 제공할 수 있을 것으로 기대된다.

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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.

Property Analysis of Ceramic Interconnect Prepared by Thermal Plasma Spray Coating Method for SOFC (Thermal Plasma Spray Coating 법에 의해 코팅된 SOFC용 세라믹 연결재 특성 분석)

  • Park, Kwang-Yeon;Pi, Seuk-Hoon;Lee, Jong-Won;Lee, Seung-Bok;Lim, Tak-Hyoung;Park, Seok-Joo;Song, Rak-Hyun;Shin, Dong-Ryul
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.710-714
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    • 2011
  • In present work, $La_{0.8}Ca_{0.2}CrO_{3}$(LCC), $La_{0.8}Sr_{0.2}CrO_{3}$(LSC) and $La_{0.8}Ca_{0.2}CrO_{0.9}Co_{0.1}O_{3}$(LCCC) ceramic interconnect layer for SOFC were prepared by using thermal plasma spray coating process. The LCC, LSC and LCCC powders were characterized by x-ray diffraction(XRD), scanning electron microscopy(SEM), particle counter and BET analysis. In addition, basic and essential properties such as the surface morphology, cross section, gas leak rate, and electrical conductivity of LCC, LSC, and LCCC layers coated by thermal plasma spray coating process were analyzed and discussed. Based on these experimental results, it can be concluded that the LCCC layer coated by thermal plasma spray coating process can be suitable as a ceramic interconnect of SOFC.

Synthesis of the orange color pigment in the system of TiO2-SnO-ZnO by solid state reaction (고상반응법에 의한 TiO2-SnO-ZnO의 주황 안료 합성에 관한 연구)

  • Kim, Soomin;Kim, Ungsoo;Cho, Woo Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.5
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    • pp.181-187
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    • 2016
  • In this study, new composition of orange color pigment was developed by replacing formerly used lead and chromium with environment-friendly elements. $TiO_2-SnO-ZnO$ composite was synthesized using the solid state reaction under the reducing atmosphere with the LPG and air mixture gas. The synthesized pigments were characterized by spectrophotometer, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The colorimetric analysis of pigments exhibited color values ranging from yellow to orange-red. Five different crystalline phases were formed after the heat treatment for 4 and 6 hours. The color of pigments was strongly influenced by the crystalline structure of $SnO_2$, having either cubic or tetragonal structure. The oxidation state study of elements revealed that the color of pigment is getting close to rYR with the increase of $Sn^{4+}$ ratio.

Effect of Precipitator and Quantity on the Formation of Fe3(PO4)2 (Fe3(PO4)2 생성에 미치는 침전제와 첨가량의 영향)

  • An, Suk-Jin;Lee, Sun-Young;Oh, Kyoung-Hwan;Suhr, Dong-Soo
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.587-591
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    • 2011
  • The effect of the precipitator (NaOH, $NH_4OH$) and the amount of the precipitator (150, 200, 250, 300 ml) on the formation of $Fe_3(PO_4)_2$, which is the precursor used for cathode material $LiFePO_4$ in Li-ion rechargeable batteries was investigated by the co-precipitation method. A pure precursor of olivine $LiFePO_4$ was successfully prepared with coprecipitation from an aqueous solution containing trivalent iron ions. The acid solution was prepared by mixing 150 ml $FeSO_4$(1M) and 100 ml $H_3PO_4$(1M). The concentration of the NaOH and $NH_4OH$ solution was 1 M. The reaction temperature (25$^{\circ}C$) and reaction time (30 min) were fixed. Nitrogen gas (500 ml/min) was flowed during the reaction to prevent oxidation of $Fe^{2+}$. Single phase $Fe_3(PO_4)_2$ was formed when 150, 200, 250 and 300 ml NaOH solutions were added and 150, 200 ml $NH_4OH$ solutions were added. However, $Fe_3(PO_4)_2$ and $NH_4FePO_4$ were formed when 250 and 300 ml $NH_4OH$ was added. The morphology of the $Fe_3(PO_4)_2$ changed according to the pH. Plate-like lenticular shaped $Fe_3(PO_4)_2$ formed in the acidic solution below pH 5 and plate-like rhombus shaped $Fe_3(PO_4)_2$ formed around pH 9. For the $NH_4OH$, the pH value after 30 min reaction was higher with the same amount of additions of NaOH and $NH_4OH$. It is believed that the formation mechanism of $Fe_3(PO_4)_2$ is quite different between NaOH and $NH_4OH$. Further investigation on this mechanism is needed. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and the pH value was measured by pH-Meter.

Preparation of Pd Coated Hollow Fiber-Type La0.1Sr0.9Co0.2Fe0.8O3-δ Catalyst and Study on Removal Characteristics of Minute Oxygen (Pd 코팅 된 중공사형 La0.1Sr0.9Co0.2Fe0.8O3-δ 촉매의 제조 및 미량 산소 제거 특성 연구)

  • Jeong, Byeong Jun;Lee, Hong Ju;Kim, Min Kwang;Lee, Seung Hwan;Park, Jung Hoon
    • Korean Chemical Engineering Research
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    • v.57 no.6
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    • pp.774-780
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    • 2019
  • An efficient Pd-coated $La_{0.1}Sr_{0.9}Co_{0.2}Fe_{0.8}O_{3-{\delta}}$ (LSCF-1928) catalyst for total oxidation of methane under landfill gas at low tmeperature has been developed. Synergism was observed between Pd coating and LSCF-1928 substrate. When Pd coating on LSCF-1928, we used electroless plating method and conformed characteristic of catalyst through TPR(Temperature Programmed Reduction) analysis, XRD(X-ray Diffraction) analysis, SEM(Scanning Electron Microscope). The results demonstrated that the Pd coated LSCF-1928 catalysts showed higher performance than non-Pd LSCF-1928. Pd coated LSCF-1928 had low total oxidation temperature of methane (< $475^{\circ}C$) which is lower than total oxidation temperature of methane about non-Pd LSCF-1928 catalysts (= $475^{\circ}C$). Also, $O_2$ conversion rate was higher than non-Pd LSCF-1928 at same temperature.

Study on the Fuel Decomposition Characteristics and Coke Formation by Type of Endothermic Fuel and Method of Catalyst Molding (흡열연료 종류와 촉매 성형 방법에 따른 분해특성과 코크 생성에 관한 연구)

  • Lee, Tae Ho;Kang, Saetbyeol;Kim, Sung Hyun
    • Korean Chemical Engineering Research
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    • v.57 no.5
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    • pp.611-619
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    • 2019
  • This study was carried out to investigate fuel decomposition characteristics and coke formation according to types of endothermic fuels and methods of catalyst molding. Methylcyclohexane (MCH), n-dodecane, and exo-tetrahydrodipentadiene (exo-THDCP) were used as the endothermic fuels. As a catalyst, USY720 supported with platinum was used. It was manufactured by only using pressure to disk-type, or pelletized with a binder and a silica solution. The characteristics of the catalysts according to the molding method were analyzed by X-ray diffraction analysis, scanning electron microscopy, nitrogen adsorption-desorption isotherm, and ammonia temperature programmed desorption analysis. The reaction was carried out under conditions of high temperature and high pressure ($500^{\circ}C$, 50 bar) in which the fuel could exist in a supercritical state. The product was analyzed by gas chromatograph/mass spectrometer and the coke produced by the catalyst was analyzed by thermogravimetric analyzer. After the reaction, the composition of the products varied greatly depending on the structure of the fuel. In addition, the crystallinity and surface properties of the catalysts were not changed by the method of catalyst molding, but the changes of the acid sites and the pore characteristics were observed, which resulted in changes in the amount and composition of products and coke.

Geotechnical Engineering Characteristics of Ulleung Basin Sediment, East Sea (동해, 울릉 분지 심해토의 지반공학특성)

  • Lee, Chang-Ho;Yun, Tae-Sup;J.C., Santamarina;Bahk, Jang-Jun;Lee, Jong-Sub
    • Journal of the Korean Geotechnical Society
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    • v.25 no.6
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    • pp.17-29
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    • 2009
  • There has been an increase in the investigation of deep sea sediments with a consequent increase in the amount of energy required to undertake these investigations. The geotechnical characteristics of Ulleung Basin sediment are explored by using depressurized specimens following methane production tests carried out on pressured core samples obtained at 2,100 m water depth and 110 m below sea floor. Geotechnical index tests, X-ray diffraction, and scanning electron microscope are conducted to identify the geotechnical index parameters, clay mineralogy, chemical composition, and microstructure of the sediments. Compressibility, and elastic and electromagnetic wave parameters are investigated for two samples by using a multi sensing instrumented oedometer cell. The strength chatracteristics are obtained by the direct shear tests. The dominant clay minerals are mostly kaolinite, illite, chlorite, and calcite. The SEM shows a well-developed flocculated structure of the microfossil. Void ratio, electrical resistivity, real permittivity, conductivity, and shear wave velocity show bi-linear behavior with the effective vertical stress: as the vertical effective stress increases. The friction angle obtained by the direct shear test is about $21^{\circ}$, which is similar to the value observed in the Ulleung Basin sediments. This study shows that the understanding of the behavior acting on the diatomaceous marine sediment is important because it often maintains the useful energy resources such as gas hydrate and so will be the new engineering field in the next generation.

Research on the Production of CO2 Absorbent Using Railway Tie Concrete Waste (콘크리트 철도 침목 폐기물을 활용한 CO2 포집제 제조 연구)

  • Gyubin Lee;Jae-Young Lee;Hyung-Jun Jang;Sangwon Ko;Hye-Jin Hong
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.11 no.3
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    • pp.260-266
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    • 2023
  • In recent years, excessive emissions of carbon dioxide(CO2) have become the cause of global climate change. Consequently, there has been significant research activity aimed at both removing and utilizing CO2. This study assesses the potential utilization of railway tie concrete waste, generated from railway infrastructure, as a CO2 absorption material and investigates the physicochemical properties before and after CO2 absorption to understand the CO2 removal mechanisms. Railway tie concrete waste primarily consists of Si(26.60 %) and contains 9.82 % of Ca. Compared to samples of Cement and Normal concrete waste, it demonstrated superior potential for use as a CO2 absorption material, with approximately 98 % of the Ca content participating in CO2 absorption reactions. Through Thermogravimetric Analysis(TGA) and X-ray Diffraction(XRD) analysis, it was confirmed that the carbonate reaction, where the Ca in railway tie concrete waste converts into CaCO3 through reaction with CO2 gas, is the primary mechanism for CO2 removal. Furthermore, Scanning Electron Microscopy(SEM) analysis revealed the formation of numerous CaCO3 particles with sizes less than 0.1 ㎛ after the CO2 absorption reaction. This transformation of large internal voids in the CO2 absorption material into mesopores resulted in an increase in the specific surface area of the material.

PREPARATION OF AMORPHOUS CARBON NITRIDE FILMS AND DLC FILMS BY SHIELDED ARC ION PLATING AND THEIR TRIBOLOGICAL PROPERTIES

  • Takai, Osamu
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2000.11a
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    • pp.3-4
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    • 2000
  • Many researchers are interested in the synthesis and characterization of carbon nitride and diamond-like carbon (DLq because they show excellent mechanical properties such as low friction and high wear resistance and excellent electrical properties such as controllable electical resistivity and good field electron emission. We have deposited amorphous carbon nitride (a-C:N) thin films and DLC thin films by shielded arc ion plating (SAIP) and evaluated the structural and tribological properties. The application of appropriate negative bias on substrates is effective to increase the film hardness and wear resistance. This paper reports on the deposition and tribological OLC films in relation to the substrate bias voltage (Vs). films are compared with those of the OLC films. A high purity sintered graphite target was mounted on a cathode as a carbon source. Nitrogen or argon was introduced into a deposition chamber through each mass flow controller. After the initiation of an arc plasma at 60 A and 1 Pa, the target surface was heated and evaporated by the plasma. Carbon atoms and clusters evaporated from the target were ionized partially and reacted with activated nitrogen species, and a carbon nitride film was deposited onto a Si (100) substrate when we used nitrogen as a reactant gas. The surface of the growing film also reacted with activated nitrogen species. Carbon macropartic1es (0.1 -100 maicro-m) evaporated from the target at the same time were not ionized and did not react fully with nitrogen species. These macroparticles interfered with the formation of the carbon nitride film. Therefore we set a shielding plate made of stainless steel between the target and the substrate to trap the macropartic1es. This shielding method is very effective to prepare smooth a-CN films. We, therefore, call this method "shielded arc ion plating (SAIP)". For the deposition of DLC films we used argon instead of nitrogen. Films of about 150 nm in thickness were deposited onto Si substrates. Their structures, chemical compositions and chemical bonding states were analyzed by using X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and infrared spectroscopy. Hardness of the films was measured with a nanointender interfaced with an atomic force microscope (AFM). A Berkovich-type diamond tip whose radius was less than 100 nm was used for the measurement. A force-displacement curve of each film was measured at a peak load force of 250 maicro-N. Load, hold and unload times for each indentation were 2.5, 0 and 2.5 s, respectively. Hardness of each film was determined from five force-displacement curves. Wear resistance of the films was analyzed as follows. First, each film surface was scanned with the diamond tip at a constant load force of 20 maicro-N. The tip scanning was repeated 30 times in a 1 urn-square region with 512 lines at a scanning rate of 2 um/ s. After this tip-scanning, the film surface was observed in the AFM mode at a constant force of 5 maicro-N with the same Berkovich-type tip. The hardness of a-CN films was less dependent on Vs. The hardness of the film deposited at Vs=O V in a nitrogen plasma was about 10 GPa and almost similar to that of Si. It slightly increased to 12 - 15 GPa when a bias voltage of -100 - -500 V was applied to the substrate with showing its maximum at Vs=-300 V. The film deposited at Vs=O V was least wear resistant which was consistent with its lowest hardness. The biased films became more wear resistant. Particularly the film deposited at Vs=-300 V showed remarkable wear resistance. Its wear depth was too shallow to be measured with AFM. On the other hand, the DLC film, deposited at Vs=-l00 V in an argon plasma, whose hardness was 35 GPa was obviously worn under the same wear test conditions. The a-C:N films show higher wear resistance than DLC films and are useful for wear resistant coatings on various mechanical and electronic parts.nic parts.

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