• Title/Summary/Keyword: EDS Process

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Influences of Potassium Fluoride (KF) Addition on the Surface Characteristics in Plasma Electrolytic Oxidation of Marine Grade Al Alloy (해양환경용 알루미늄 합금의 플라즈마 전해 산화 시 표면 특성에 관한 불화칼륨(KF)의 영향)

  • Lee, Jung-Hyung;Kim, Seong-Jong
    • Journal of Surface Science and Engineering
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    • v.49 no.3
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    • pp.280-285
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    • 2016
  • In this study, we investigated the influences of potassium fluoride(KF) addition on the surface characteristics of plasma electrolytic oxidation(PEO) coating produced on Al alloy. The PEO of marine grade Al alloy(5083 grade) was conducted in KOH 1g/L solution adding different concentrations of KF(0, 1 and 2 g/L) under a galvanostatic regime. With KF addition, unusual behavior was observed on the voltage-time characteristic curves, which can be characterized by the following process: (i) initial rapid increase in voltage (ii) a short plateau after 1st breakdown (iii) gradual increase in voltage (iv) intermittent fluctuation of voltage after 2nd breakdown. The SEM observation revealed irregular surface morphology with KF addition, as compared with one formed without KF addition, which had a reticulate structure. The XRD analysis detected the formation of aluminium hydroxide fluoride hydrate($H_{4.76}Al_2F_{3.24}O_{3.76}$) on surface grown by PEO process with KF. Particularly, at very early stage of the process (~ 120 s), thin film was formed having nanoporous structure, and F element was confirmed on surface by EDS analysis. The thickness and surface roughness of the coating increased with increasing KF concentration. As a result, KF addition was found to be less beneficial influences on PEO of marine grade Al alloy, and therefore needs further research to improve its capability.

Characteristics of Coating Films on Hot-Dipped Aluminized Steel Formed by Plasma Electrolytic Oxidation Process at Different Current Densities (PEO 전류밀도 조건에 따른 알루미늄도금 강재상 산화코팅막의 특성)

  • Choi, In-Hye;Lee, Hoon-Seung;Lee, Myeong-Hoon
    • Journal of Surface Science and Engineering
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    • v.50 no.5
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    • pp.366-372
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    • 2017
  • Plasma electrolytic oxidation(PEO) has attracted attention as a surface treatment which has high wear resistance and corrosion resistance. PEO is generally considered as cost-effective, environmentally friendly and superior in terms of coating performance. Most of studies about the PEO processes have been applied to light metals such as Al and Mg. Because the strength of Al and Mg is weaker than that of steel, there is a limit to the application. In this study, PEO process was used to form oxide coatings on Hot dipped aluminized(HDA) steel and the characteristics of the coating film according to the PEO current density were studied. The morphology was observed by SEM and component was analyzed by using EDS. The corrosion behaviors of PEO coating films were estimated by exposing salt spray test at 5 wt.% NaCl solution and measuring polarization curves in deaerated 3 wt.% NaCl solution. With the increase of PEO process current density, the pore size of the coating surface and the thickness of coating increased. It was confirmed that no Fe component was present on the coating surface. PEO coating films obviously showed good corrosion resistance compared with HDA. It is considered that the PEO coating acts as a barrier to protect the base material from external factors causing corrosion.

A Study on Selenization of Cu-In-Ga Precursors by Cracked Selenium (Cracked Selenium을 이용한 CIGS 박막 셀렌화 공정에 관한 연구)

  • Kim, Minyoung;Kim, Girim;Kim, Jongwan;Son, Kyeongtae;Lee, Jongkwan;Lim, Donggun
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.26 no.7
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    • pp.503-509
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    • 2013
  • In this study, $Cu(In_{1-x},Ga_x)Se_2$ (CIGS) thin films were prepared on the Mo coated soda-lime glass by the DC magnetron sputtering and a subsequent selenization process. For the selenization process, selenization rapid thermal process(RTP) with cracker cell, which was helpful to smaller an atomic of Se, was adopted. To make CIGS layer, they were then annealed with the cracked Se. Based on this selenization method, we made several CIGS thin film and investigated the effects of In deposition time, and selenization time. Through x-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and atomic force microscopy (AFM), it is found that the Mo/In/CuGa structure and the high sputtering power shows the dominant chalcopyrite structure and have a uniform distribution of the grain size. The CIGS films with the In deposition time of 5 min has the best structure due to the smooth surface. And CIGS films with the selenization time of 50 min show good crystalline growth without any voids.

Photocatalytic Properties of the Ag-Doped TiO2 Prepared by Sol-Gel Process/Photodeposition (졸-겔공정/광증착법을 이용한 Ag-Doped TiO2 합성 및 광촉매 특성)

  • Kim, Byeong-Min;Kim, Jung-Sik
    • Korean Journal of Materials Research
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    • v.26 no.2
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    • pp.73-78
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    • 2016
  • $TiO_2$ nanoparticles were synthesized by a sol-gel process using titanium tetra isopropoxide as a precursor at room temperature. Ag-doped $TiO_2$ nanoparticles were prepared by photoreduction of $AgNO_3$ on $TiO_2$ under UV light irradiation and calcinated at $400^{\circ}C$. Ag-doped $TiO_2$ nanoparticles were characterized for their structural and morphological properties by X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and transmission electron microscopy (TEM). The photocatalytic properties of the $TiO_2$ and Ag-doped $TiO_2$ nanoparticles were evaluated according to the degree of photocatalytic degradation of gaseous benzene under UV and visible light irradiation. To estimate the rate of photolysis under UV (${\lambda}=365nm$) and visible (${\lambda}{\geq}410nm$) light, the residual concentration of benzene was monitored by gas chromatography (GC). Both undoped/doped nanoparticles showed about 80 % of photolysis of benzene under UV light. However, under visible light irradiation Ag-doped $TiO_2$ nanoparticles exhibited a photocatalytic reaction toward the photodegradation of benzene more efficient than that of bare $TiO_2$. The enhanced photocatalytic reaction of Ag-doped $TiO_2$ nanoparticles is attributed to the decrease in the activation energy and to the existence of Ag in the $TiO_2$ host lattice, which increases the absorption capacity in the visible region by acting as an electron trapper and promotes charge separation of the photoinduced electrons ($e^-$) and holes ($h^+$). The use of Ag-doped $TiO_2$ nanoparticles preserved the option of an environmentally benign photocatalytic reaction using visible light; These particles can be applicable to environmental cleaning applications.

Hot Corrosion Behavior of Plasma-Sprayed Partially Stabilized Zirconia Coatings in a Lithium Molten Salt (리튬용융염에서 플라즈마 용사된 부분안정화 지르코니아 코팅층의 고온부식 거동)

  • Cho, Soo-Haeng;Hong, Sun-Seok;Kang, Dae-Seong;Park, Byung-Heong;Hur, Jin-Mok;Lee, Han-Soo
    • Korean Journal of Metals and Materials
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    • v.46 no.10
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    • pp.646-651
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    • 2008
  • The electrolytic reduction of spent oxide fuel involves the liberation of oxygen in a molten LiCl electrolyte, which results in a chemically aggressive environment that is too corrosive for typical structural materials. It is essential to choose the optimum material for the process equipment handling molten salt. IN713LC is one of the candidate materials proposed for application in electrolytic reduction process. In this study, yttria-stabilized zirconia (YSZ) top coat was applied to a surface of IN713LC with an aluminized metallic bond coat by an optimized plasma spray process, and were investigated the corrosion behavior at $675^{\circ}C$ for 216 hours in the molten salt $LiCl-Li_2O$ under an oxidizing atmosphere. The as-coated and tested specimens were examined by OM, SEM/EDS and XRD, respectively. The bare superalloy reveals obvious weight loss, and the corrosion layer formed on the surface of the bare superalloy was spalled due to the rapid scale growth and thermal stress. The top coatings showed a much better hot-corrosion resistance in the presence of $LiCl-Li_2O$ molten salt when compared to those of the uncoated superalloy and the aluminized bond coatings. These coatings have been found to be beneficial for increasing to the hot-corrosion resistance of the structural materials for handling high temperature lithium molten salts.

Study on the Microstructure Evolution during Extrusion of Zn-Al-Mg alloy (Zn-Al-Mg 합금의 압출 시 미세조직 변화에 관한 연구)

  • W. G. Seo;K. Thool;H. N. Lee;D. J. Yang;S. G. Park;S. H. Choi
    • Transactions of Materials Processing
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    • v.32 no.6
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    • pp.344-351
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    • 2023
  • The use of Zn-Al-Mg alloy coatings for enhancing the corrosion resistance of steel sheets is gaining prominence over traditional Zn coatings. There is a growing demand for the development of thermal spray wires made from Zn-Al-Mg alloys, as a replacement for the existing wires produced using Al and Zn. This is particularly crucial to secure corrosion resistance and durability in the damaged areas of coated steel sheets caused by deformation and welding. This study focuses on the casting and extrusion processes of Zn-2Al-1Mg alloy for the fabrication of such spray wires and analyzes the changes in microstructure during the extrusion process. The Zn-2Al-1Mg alloy, cast in molds, was subjected to a heat treatment at 250 ℃ for 3 hours prior to extrusion. The extrusion process was carried out by heating both the material and the mold up to 300 ℃. Microstructural analysis was conducted using FE-SEM and EDS to differentiate each phase. The mechanical properties of the cast specimen were evaluated through compression tests at temperatures ranging from 200 to 300 ℃, with strain rates of 0.1 to 5 sec-1. Vickers hardness testing was utilized to assess the inhomogeneity of mechanical properties in the radial direction of the extruded material. Finite Element Analysis (FEA) was employed to understand the inhomogeneity in stress and strain distribution during extrusion, which aids in understanding the impact of heterogeneous deformation on the microstructure during the process.

Nano particle size control of Pt/C catalysts manufactured by the polyol process for fuel cell application (폴리올법으로 제조된 Pt/C 촉매의 연료전지 적용을 위한 나노 입자 크기제어)

  • Joon Heo;Hyukjun Youn;Ji-Hun Choi;Chae Lin Moon;Soon-Mok Choi
    • Journal of Surface Science and Engineering
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    • v.56 no.6
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    • pp.437-442
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    • 2023
  • This research aims to enhance the efficiency of Pt/C catalysts due to the limited availability and high cost of platinum in contemporary fuel cell catalysts. Nano-sized platinum particles were distributed onto a carbon-based support via the polyol process, utilizing the metal precursor H2PtCl6·6H2O. Key parameters such as pH, temperature, and RPM were carefully regulated. The findings revealed variations in the particle size, distribution, and dispersion of nano-sized Pt particles, influenced by temperature and pH. Following sodium hydroxide treatment, heat treatment procedures were systematically executed at diverse temperatures, specifically 120, 140, and 160 ℃. Notably, the thermal treatment at 140 ℃ facilitated the production of Pt/C catalysts characterized by the smallest platinum particle size, measuring at 1.49 nm. Comparative evaluations between the commercially available Pt/C catalysts and those synthesized in this study were meticulously conducted through cyclic voltammetry, X-ray diffraction (XRD), and field-emission scanning electron microscopy-energy dispersive X-ray spectroscopy (FE-SEM EDS) methodologies. The catalyst synthesized at 160 ℃ demonstrated superior electrochemical performance; however, it is imperative to underscore the necessity for further optimization studies to refine its efficacy.

Study on the Room Temperature Degreasing Conditions of Steel Sheet for Electrogalvanizing (전기아연도금용 강판의 상온 탈지 조건 연구)

  • Tae-Yeon Park;Chae-Won Kim;Su-Mi Yang;Hee-Jun Hong;In-Chul Choi
    • Journal of the Korean Society for Heat Treatment
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    • v.37 no.1
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    • pp.16-22
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    • 2024
  • The conventional degreasing process involves removing oil and contaminants at temperatures above 80℃, resulting in excessive energy consumption, increased process costs, and environmental issues. In this study, we aimed to find the optimal degreasing conditions for the pre-treatment process of electro-galvanizing cold-rolled steel sheets, conducted efficiently at room temperature without the need for a separate heating device. To achieve this, we developed a room temperature degreasing solution and a brush-type degreasing tool, aiming to reduce energy consumption and normalize the decrease in degreasing efficiency caused by temperature reduction. Alkaline degreasing solution were prepared using KOH, SiO2, NaOH, Na2CO3, and Sodium Lauryl Sulfate, with KOH and NaOH as the main components. To enhance the degreasing performance at room temperature, we manufactured additives including sodium oleate, sodium stearate, sodium palmitate, sodium lauryl sulfate, ammonium lauryl sulfate, silicone emulsion, and EDTA-Na. Room temperature additives were added to the alkaline degreasing solution in quantities ranging from 0.1 to 20 wt.%, and the uniformity of degreasing and the adhesion of the galvanized layer were evaluated through Dyne Test, T-bending Test, OM, SEM, and EDS analyses. The results indicated that the optimal degreasing solution composition consisted of NaOH (30 g/L), Na2CO3 (30 g/L), SLS (6 g/L), and room temperature additives (≤1 wt%).

Hydrophilic Modification of Porous Polyvinylidene Fluoride Membrane by Pre-irradiating Electron Beam (전자빔 전조사를 이용한 Polyvinylidene Fluoride 다공막의 친수화 개질)

  • Choi, Yong-Jin;Lee, Sung-Won;Seo, Bong-Kuk;Kim, Min
    • Membrane Journal
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    • v.21 no.2
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    • pp.118-126
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    • 2011
  • A method of light pre-irradiation, one of methods modifying hydrophobic surface to hydrophilic surface in a membrane, was proposed to overcome the drawback of previous methods such as blending, chemical treatment and post-irradiation, Process of membrane preparation in the study was comprised of 4 parts as follows: firstly process of precursor preparation to introduce hydrophilic nature under atmosphere and aqueous vapor by irradiating electron beam (EB), secondly process of dope solution preparation to cast on non-woven fabrics, thirdly process of casting to prepare membrane and finally process of coagulation in non-solvent to form porous structure. The merit of this method might show simple process as well as homogenous modification compared to previous methods. To carry it out, precursor was prepared by irradiating EB to powder PVDF at 75~125 K Gray dose. Precursor prepared was analyzed by FTIR, EDS and DSC to confirm the introduction of hydrophilic function and its mechanism. From their results, it was inferred I conformed that hydrophilic function was hydroxy1 and it was introduced by dehydrozenation. Hydrophilicity of membranes prepared was evaluated by contact angle (pristine PVDF : $62^{\circ}$, 125 K Gray-PVDF$13^{\circ}$). Porosity was evaluated by mercury intrusion method, simultaneously morpholoy and surface pore size were observed by SEM phothographs. The result showed the trend that more dose of EB led to smaller pore size and to lower porosity (pristine PVDF : 82%, 125 K Gray-PVDF : 63%). Trend of water permeability was similar to result above (pristine PVDF : 892 LMH, 125 K Gray-PVDF : 355 LMH).

Characterization and Formation Mechanism of Zr-Cu and Zr-Cu-Al Metallic Glass Thin Film by Sputtering Process

  • Lee, Chang-Hun;Sun, Ju-Hyun;Moon, Kyoung-Il;Shin, Seung-Yong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.271-272
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    • 2012
  • Bulk Metallic Glasses (BMGs or amorphous alloy) exhibit high strength and good corrosion resistance. Applications of thin films and micro parts of BMGs have been used a lot since its inception in the research of BMGs. However, Application and fabrication of BMGs are limited to make structural materials. Thin films of BMGs which is sputtered on the surface of structural materials by sputtering process is used to improve limits about application of BMGs. In order to investigate the difference of properties between designed alloys and thin films, we identified that thin films deposited on the surface that have the characteristic of the amorphous films and the composition of designed alloys. Zr-Cu (Cu=30, 35, 38, 40, 50 at.%) and Zr-Cu-Al (Al=10 at.% fixed, Cu=26, 30, 34, 38 at.%) alloys were fabricated with Zr (99.7% purity), Cu (99.997% purity), and Al (99.99% purity) as melting 5 times by arc melting method before rods 2mm in diameter was manufactured. In order to analyze GFA (Glass Forming Ability), rods were observed by Optical Microscopy and SEM and $T_g$, $T_x$, ($T_x$ is crystallization temperature and $T_g$ is the glass transition temperature) and Tm were measured by DTA and DSC. Powder was manufactured by Gas Atomizer and target was sintered using powder in large supercooled liquid region ($=T_x-T_g$) by SPS(Spark Plasma Sintering). Amorphous foil was prepared by RSP process with 5 gram alloy button. The composition of the foil and sputtered thin film was analyzed by EDS and EPMA. In the result of DSC curve, binary alloys ($Zr_{62}Cu_{38}$, $Zr_{60}Cu_{40}$, $Zr_{50}Cu_{50}$) and ternary alloys ($Zr_{64}Al_{10}Cu_{26}$, $Zr_{56}Al_{10}Cu_{34}$, $Zr_{52}Al_{10}Cu_{38}$) have $T_g$ except for $Zr_{70}Cu_{30}$ and $Zr_{60}Al_{10}Cu_{30}$. The compositions with $T_g$ made into powders. Figure shows XRD data of thin film showed similar hollow peak.

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