• Title/Summary/Keyword: EDS analysis

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Characteristics and Mechanisms of Phosphate Sorption by Calcined Oyster Shell (소성 굴패각에 의한 인산염의 흡착특성 및 메커니즘)

  • Park, Jong-Hwan;Heo, Jae-Young;Lee, Su-Lim;Lee, Jae-Hoon;Hwang, Se-Wook;Cho, Hyeon-Ji;Kwon, Jin-Hyeuk;Chang, Young-Ho;Seo, Dong-Cheol
    • Korean Journal of Environmental Agriculture
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    • v.40 no.1
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    • pp.40-48
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    • 2021
  • BACKGROUND: Although the calcined oyster shell can be used as a calcium-rich adsorbent for phosphate removal, information about it is limited. The purpose of this study was to evaluate the phosphate adsorption characteristics and its mechanism using calcined oyster shells. METHODS AND RESULTS: In this study, calcined oyster shell (C-OS600) was prepared by calcining oyster shells (P-OS) at 600℃ for 20 min. Phosphate adsorption by C-OS600 was performed under various environmental conditions. Phosphate adsorption by C-OS600 occurred rapidly at the beginning of the reaction, and the time to reach equilibrium was less than 1 h. The optimal isotherm and kinetic models for predicting the adsorption of phosphate by C-OS600 were the Langmuir isotherm and pseudo-second order kinetic model, respectively, and the maximum adsorption capacity derived from the Langmuir isotherm was 68.0 mg/g. The adsorption properties of phosphate by C-OS600 were dominantly influenced by the initial pH and C-OS600 dose. In addition, SEM-EDS and FTIR analysis clearly showed a difference in C-OS600 before and after phosphate adsorption, which proved that phosphate was adsorbed on the surface of C-OS600. CONCLUSION: Overall, the calcined oyster shell can be considered as an useful and effective adsorbent to treat wastewater containing phosphate.

Hot Corrosion and Thermally Grown Oxide Formation on the Coating of Used IN738LC Gas Turbine Blade (사용된 IN738LC 가스 터빈 블레이드 코팅층의 고온 부식 및 Thermally Grown Oxide 형성 거동)

  • Choe, Byung Hak;Han, Sung Hee;Kim, Dae Hyun;Ahn, Jong Kee;Lee, Jae Hyun;Choi, Kwang Su
    • Korean Journal of Materials Research
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    • v.32 no.4
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    • pp.200-209
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    • 2022
  • In this study, defects generated in the YSZ coating layer of the IN738LC turbine blade are investigated using an optical microscope and SEM/EDS. The blade YSZ coating layer is composed of a Y-Zr component top coat layer and a Co component bond coat layer. A large amount of Cr/Ni component that diffused from the base is also measured in the bond coat. The blade hot corrosion is concentrated on the surface of the concave part, accompanied by separation of the coating layer due to the concentration of combustion gas collisions here. In the top coating layer of the blade, cracks occur in the vertical and horizontal directions, along with pits in the top coating layer. Combustion gas components such as Na and S are contained inside the pits and cracks, so it is considered that the pits/cracks are caused by the corrosion of the combustion gases. Also, a thermally grown oxide (TGO) layer of several ㎛ thick composed of Al oxide is observed between the top coat and the bond coat, and a similar inner TGO with a thickness of several ㎛ is also observed between the bond coat and the matrix. A PFZ (precipitate free zone) deficient in γ' (Ni3Al) forms as a band around the TGO, in which the Al component is integrated. Although TGO can resist high temperature corrosion of the top coat, it should also be considered that if its shape is irregular and contains pore defects, it may degrade the blade high temperature creep properties. Compositional and microstructural analysis results for high-temperature corrosion and TGO defects in the blade coating layer used at high temperatures are expected to be applied to sound YSZ coating and blade design technology.

Feasibility Evaluation for Remediation of Groundwater Contaminated with Heavy Metal using Calcium Polysulfide in Homogeneous media (균질한 매질 내 Calcium polysulfide 주입에 따른 고농도 중금속 오염 지하수 정화 타당성 검토)

  • Hyeon Woo Go;Jin Chul Joo;Kyoungphile Nam;Hee Sun Moon;Sung Hee Yoon;Dong Hwi Lee;So Ye Jang
    • Journal of Soil and Groundwater Environment
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    • v.28 no.1
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    • pp.1-14
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    • 2023
  • In this study, column tests using relatively uniform Jumunjin sand media were conducted to evaluate the feasibility of calcium polysulfide (CaSx, CPS) in removing high concentration of Zn2+ in groundwater. The injected CPS solution reacted rapidly with Zn2+ in artificial groundwater and effectively reduced Zn2+ by more than 99% through metal sulfide precipitation. Since the density (d = 1.27 g/cm3 ) of CPS solution was greater than that of water, CPS solution settled down rapidly while capturing Zn2+ and formed stable CPS layer similar to dense nonaqueous phase liquid. Mass balance analysis on Zn2+ in CPS solution suggested that CPS solution effectively reacted with Zn2+ to form metal sulfide precipitates except for high groundwater seepage velocity of 400 cm/d. With greater groundwater seepage velocity, injected CPS did not completely dissolve at the CPS-water interface, but a partially-misible CPS layer continuously moved and reacted with Zn2++ in the direction of groundwater flow. Since hydraulic conductivity (Kh) decreased slightly due to the generated metal precipitates in the inter-pores of media, injection of CPS solution should be optimized to prevent clogging. As evidenced by both XRF and SEM/EDS results, ZnS precipitates were clearly observed through the reaction between the CPS solution and Zn2+. Further study is warranted to evaluate the feasibility of CPS to remove high-concentration heavy metalcontaminated groundwater in complex and heterogeneous media.

Phase evaluation of Fe/Co pigments coated porcelain by rietveld refinement (리트벨트 정밀화법에 의한 Fe/Co 안료가 코팅된 도자기의 상분석)

  • Nam-Heun Kim;Kyung-Nam Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.5
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    • pp.174-180
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    • 2023
  • Porcelain (white ware, celadon ware) coated with a ferrous sulfate and ferrous/cobalt sulfate was sintered at 1250℃. The specimens were investigated by HR-XRD, FE-SEM, HR-EDS, and UV-vis spectrophotometer. Through X-ray rietveld quantitative analysis, quartz and mullite were found to be the main phases for white ware, and mullite and plagioclase were found to be the main phases for celadon ware. When the pigment of ferrous/cobalt sulfate was applied, were identified as an andradite phase for celadon ware and a spinel phase for the white ware, and the amorphous phase, respectively. The L* value, which was the brightness of the specimen, was 72.01, 60.92 for white ware and celadon ware, respectively. The ferrous and ferrous/cobalt pigment coated porcelain had L* values of 44.89, 52.27 for white ware and celadon ware, respectively; with a* values of 2.12, 1.40, an d at b* values of 1.45 and 13.79. As for the color of the specimens, it was found that the L* value was greatly affected by the white ware, and the b* value differed greatly depending on the clay. It was thought to be closely related to the production of the secondary phase such as Fe2O3 and andradite phase produced in the surface layer.

Scientific Analysis and Conservation Treatment on the Buddhist Scriptures of Paper Relics Excavated from Sum Tolgoi, Mongolia (몽골 숨 톨고이 출토 지류 유물의 과학적 분석 및 보존처리)

  • Bae, Su Bin;Yang, Min Jeong;Kwon, Yun Mi;Yoo, Ji Hyun;Jeong, Hee Won
    • Journal of Conservation Science
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    • v.37 no.6
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    • pp.723-737
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    • 2021
  • This study analyzed the composition and structure of materials with Buddhist paper scriptures excavated from architectural sites in 'Sum Tolgoi' of the 17th century and carried out conservation treatment base on the result of the analysis. The scriptures were covered in dust and foreign sub stances, and were so crumpled that it was impossible to identify the form. The damage, loss, and discoloration have been identified. Buddhist scriptures written in Tibetan used indigo and ink sticks on paper as a result of UV-Vis analysis, and ink sticks as black character materials from scriptures written ancient Mongolian. SEM-EDS and Micro-XRF analyses revealed that the outlines were drawn with red lines using a mix of Minium (Pb3O4) and Cinnabar (HgS), or Cinnabar (HgS) alone, and the contents of the scriptures were written with silver paint. Silver chloride (AgCl) and Calcium (Ca) were identified in the silver paint component of the characters, while Calcium and Orpiment (As2S3) were identified in the yellow lines. Concerning the paper ground, Buddhist scriptures written in ancient Mongolian were characterized by herbal plant fiber and bast fiber, and those written in Tibetan, by bast fiber. Radiocarbon dating indicates that the paper for the scriptures was produced between the 15th and 17th centuries. Conservation treatment of the scriptures was carried out based on the experiment on the production of pre-coated paper and how to coat that to prevent the second damage due to the deformation and fragility of the excavated paper. The scriptures were preserved and mounted, and a neutral box was made to identify the contents of the scriptures recorded on both sides after the treatment. This conservation treatment is the result of a study that applied new conservation treatment materials and methods according to the principle of conservation treatment reversibility.

Identification of Sorption Characteristics of Cesium for the Improved Coal Mine Drainage Treated Sludge (CMDS) by the Addition of Na and S (석탄광산배수처리슬러지에 Na와 S를 첨가하여 개량한 흡착제의 세슘 흡착 특성 규명)

  • Soyoung Jeon;Danu Kim;Jeonghyeon Byeon;Daehyun Shin;Minjune Yang;Minhee Lee
    • Economic and Environmental Geology
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    • v.56 no.2
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    • pp.125-138
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    • 2023
  • Most of previous cesium (Cs) sorbents have limitations on the treatment in the large-scale water system having low Cs concentration and high ion strength. In this study, the new Cs sorbent that is eco-friendly and has a high Cs removal efficiency was developed by improving the coal mine drainage treated sludge (hereafter 'CMDS') with the addition of Na and S. The sludge produced through the treatment process for the mine drainage originating from the abandoned coal mine was used as the primary material for developing the new Cs sorbent because of its high Ca and Fe contents. The CMDS was improved by adding Na and S during the heat treatment process (hereafter 'Na-S-CMDS' for the developed sorbent in this study). Laboratory experiments and the sorption model studies were performed to evaluate the Cs sorption capacity and to understand the Cs sorption mechanisms of the Na-S-CMDS. The physicochemical and mineralogical properties of the Na-S-CMDS were also investigated through various analyses, such as XRF, XRD, SEM/EDS, XPS, etc. From results of batch sorption experiments, the Na-S-CMDS showed the fast sorption rate (in equilibrium within few hours) and the very high Cs removal efficiency (> 90.0%) even at the low Cs concentration in solution (< 0.5 mg/L). The experimental results were well fitted to the Langmuir isotherm model, suggesting the mostly monolayer coverage sorption of the Cs on the Na-S-CMDS. The Cs sorption kinetic model studies supported that the Cs sorption tendency of the Na-S-CMDS was similar to the pseudo-second-order model curve and more complicated chemical sorption process could occur rather than the simple physical adsorption. Results of XRF and XRD analyses for the Na-S-CMDS after the Cs sorption showed that the Na content clearly decreased in the Na-S-CMDS and the erdite (NaFeS2·2(H2O)) was disappeared, suggesting that the active ion exchange between Na+ and Cs+ occurred on the Na-S-CMDS during the Cs sorption process. From results of the XPS analysis, the strong interaction between Cs and S in Na-S-CMDS was investigated and the high Cs sorption capacity was resulted from the binding between Cs and S (or S-complex). Results from this study supported that the Na-S-CMDS has an outstanding potential to remove the Cs from radioactive contaminated water systems such as seawater and groundwater, which have high ion strength but low Cs concentration.

The Study on Material Characteristics of Slags Excavated from Iron Making Site (제철 유적 출토 철재(鐵滓)의 재료학적 특성 연구)

  • Kang, Yoon-Hee;Cho, Nam-Chul;Song, Hyeon-Jeong;Go, Hyeong-Sun
    • Journal of Conservation Science
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    • v.26 no.2
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    • pp.171-182
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    • 2010
  • The slag excavated from Gyesil-ri in Gongju, Yeonje-ri in Cheongwon and Beopcheonsaji (temple) site in Wonju are analyzed by X-ray Fluorescence Analyzer, metallurgical microscope, SEM-EDS etc., for chemical composition and microstructure to figure out the raw material and the iron manufacturing technique. First of all, as a result of principal component analysis, the total Fe-content of slag from Gyesil-ri is 39 to 44% and the modified rate is 15 to 21%, which is common in ancient iron slag. Yeonje-ri site is found the ancient iron-smelting furnace. The total Fe-content of slag from Yeonje-ri is 41 to 43% and modified rate is 18~30%, which is also the general value in the ancient slag. However only slag is excavated in the residential area at Beopcheonsaji site and there is no iron making relic. In addition, the result of principal component analysis contains that the total Fe-content of Beopcheonsaji site is 52 to 57%, and modified rate is 8 to 14%. It shows that the total Fe-content of Beopcheonsaji site is higher than relic from Gyesil-ri and Yeonje-ri and the modified rate is lower than other sites. This results mean that recollecting rate of Fe in Beopcheonsaji site is lower than other sites. Also, as a result of minor elements analysis, the slag from Gyesil-ri has the higher level of Ti, V and Zr than other sites and the microstructure are observed as magnetite and ulvospinel, so that the raw material of slag is iron sand. But the slag from Yeonje-ri and Beopcheonsaji site are identified to use iron ore. As a result of microstructure observation, fayalite, gray-columnar crystal, is found in the slag from Yeonje-ri and big wustite as main phase is observed in the slag from Beopcheonsaji site. This study show that the slag from Yeonje-ri is made of smelt ash produced during smelting works and the slag from Beopcheonsaji site is made of forging ash produced during forging work concerning the excavated location and the microstructure.

Study on Iron-making and Manufacturing Technology of Iron Swords with Ring Pommel Excavated in Ipbuk-dong, Suwon (수원 입북동 출토 철제환두도의 제철과 제작기술 연구)

  • Kim, Soo-Ki
    • Journal of Conservation Science
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    • v.32 no.4
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    • pp.579-588
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    • 2016
  • This study analyzed nonmetallic inclusions in iron swords with a ring pommel excavated in the Ipbuk-dong, Suwon. Scanning electron microscopy with energy dispersive spectroscopy(SEM-EDS) was used to estimate the iron-making temperature, and we compared the oxide with $SiO_2$ to investigate the heat-treatment technology in the production of iron swords with a ring pommel by investigating the artificial insertion of a slag former and the metallurgical structure. From the wustite observed in most of the specimens, it is judged that these swords were produced by heating and forging iron smelted at a low temperature using the solid reduction method. In addition, judging from the partial presence of $P_2O_5$, it is assumed that they were smelted directly with natural ore, not calcined. From the ratios of $CaO/SiO_2$ and $TiO_2/SiO_2$, it is judged that the raw material for iron-making was iron ore and that a calcareous slag former was not artificially inserted. The structure of the blade part on the front end was pure iron. From the high carbon content of the blade part on the ring pommel and the formation of a martensitic structure and pearlite colony, it is judged that they were tempered after carburizing and that the back, handle part, and ring pommel were unintentionally carburized. Judging from the structure of these specimens, it was noted that they were produced by applying artificial partial heat-treatment technology. This study attempted to present a more scientific analysis by using the method of interpretation through component analysis of nonmetallic inclusions appearing in one relic by the ratio of the oxide divided by $SiO_2$. It is judged that reinterpreting the arguments by the results of the existing analysis and research in this way can obtain different interpretations.

A Study of the Material Properties of Steel Used to Repair the Stupa of State Preceptor Jigwang from Beopcheonsa Temple, Wonju in 1957 (1957년 원주 법천사지 지광국사탑 수리에 사용된 철물(鐵物)의 재료학적 특성 연구)

  • You, Harim;Lee, Jaesung;Lee, Taejong;Park, Heejeoung
    • Korean Journal of Heritage: History & Science
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    • v.53 no.4
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    • pp.100-117
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    • 2020
  • National Treasure no. 101, the stupa of State Preceptor Jigwang from the Beopcheonsa Temple Site in Wonju has been transferred from place to place and reassembled several times since it was built. In particular, overall dismantling and repair was carried out in 1957 to restore parts damaged by bombing during the Korean War. Documented information on the repair process and materials used at that time does not exist. However, various types of metal materials used for this stupa have been identified during conservation work. Besides clamps anchor bolts, 9mm-thick circular rebars were mainly used for joining the parts of this stupa, while circular rebars and wires of various thicknesses were used for joining the parts with mortar restoration materials. Although deformed bars are typically used for stone pagodas classified as architectural structures, smooth circular rebars were used in this case. In terms of restoration using mortar, material shapes were transformed, bound alternately, and twisted irregularly to improve bonding strength and coherence in order to insert restoration materials and to bolster structural weaknesses. In addition, metallographic analysis showed the material to be hypo-eutectoid steel with low carbon content. Many non-metallic inclusions in the shape of drops of different sizes were included, which do not affect the whole elemental composition due to the very small quantities involved. Qualitative and EPMA analysis of Mn and S, which were not identified by SEM-EDS area analysis, established an even distribution of MnS in crystal grains of the microstructure, regardless of the shape of the samples. It is presumed that secondary homogenization and softening might have been conducted after manufacturing to facilitate the working process. Furthermore, in consideration of properties indicating that the thinner the steel is, the less carbon content contained and the greater the elasticity and elongation, it is judged that restoration work was ordered.

Research of Diffusion Bonding of Tungsten/Copper and Their Properties under High Heat Flux

  • Li, Jun;Yang, Jianfeng
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.14-14
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    • 2011
  • W (tungsten)-alloys will be the most promising plasma facing armor materials in highly loaded plasma interactive components of the next step fusion reactors due to its high melting point, high sputtering resistance and low deuterium/tritium retention. The bonding technology of tungsten to Cu alloy was one of the key issues. In this paper, W/CuCrZr diffusion bonding has been performed successfully by inserting pure metal interlay. The joint microstructure, interfacial elements migration and phase composition were analyzed by SEM, EDS, XRD, and the joint shear strength and micro-hardness were investigated. The mock-ups were fabricated successfully with diffusion bonding and the cladding technology respectively, and the high heat flux test and thermal fatigue test were carried out under actively cooling condition. When Ni foil was used for the bonding of tungsten to CuCrZr, two reaction layers, Ni4W and Ni(W) layer, appeared between the tungsten and Ni interlayer with the optimized condition. Even though Ni4W is hard and brittle, and the strength of the joint was oppositely increased (217 MPa) due primarily to extremely small thicknesses (2~3 ${\mu}m$). When Ti foil was selected as the interlayer, the Ti foil diffused quickly with Cu and was transformed into liquid phase at $1,000^{\circ}C$. Almost all of the liquid was extruded out of the interface zone under bonding pressure, and an extremely thin residual layer (1~2 ${\mu}m$) of the liquid phase was retained between the tungsten and CuCrZr, which shear strength exceeded 160 MPa. When Ni/Ti/Ni multiple interlayers were used for bonding of tungsten to CuCrZr, a large number of intermetallic compound ($Ni_4W/NiTi_2/NiTi/Ni_3T$) were formed for the interdiffusion among W, Ni and Ti. Therefore, the shear strength of the joint was low and just about 85 MPa. The residual stresses in the clad samples with flat, arc, rectangle and trapezoid interface were estimated by Finite Element Analysis. The simulation results show that the flat clad sample was subjected maximum residual stress at the edge of the interface, which could be cracked at the edge and propagated along the interface. As for the rectangle and trapezoid interface, the residual stresses of the interface were lower than that of the flat interface, and the interface of the arc clad sample have lowest residual stress and all of the residual stress with arc interface were divided into different grooved zones, so the probabilities of cracking and propagation were lower than other interfaces. The residual stresses of the mock-ups under high heat flux of 10 $MW/m^2$ were estimated by Finite Element Analysis. The tungsten of the flat interfaces was subjected to tensile stresses (positive $S_x$), and the CuCrZr was subjected to compressive stresses (negative $S_x$). If the interface have a little microcrack, the tungsten of joint was more liable to propagate than the CuCrZr due to the brittle of the tungsten. However, when the flat interface was substituted by arc interfaces, the periodical residual stresses in the joining region were either released or formed a stress field prohibiting the growth or nucleation of the interfacial cracks. Thermal fatigue tests were performed on the mock-ups of flat and arc interface under the heat flux of 10 $MW/m^2$ with the cooling water velocity of 10 m/s. After thermal cycle experiments, a large number of microcracks appeared at the tungsten substrate due to large radial tensile stress on the flat mock-up. The defects would largely affect the heat transfer capability and the structure reliability of the mock-up. As for the arc mock-up, even though some microcracks were found at the interface of the regions, all microcracks with arc interface were divided into different arc-grooved zones, so the propagation of microcracks is difficult.

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