• Title/Summary/Keyword: -energy-dispersive x-ray-

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Preparation of Nanocrystalline ZrO2 Film by Using a Zirconium Naphthenate and Evaluation of Calcium Phosphate Forming Ability (지르코늄 나프테네이트를 이용한 나노결정질 ZrO2 박막의 제조와 칼슘 포스페이트 형성 능력의 평가)

  • Oh, Jeong-Sun;Ahn, Jun-Hyung;Yun, Yeon-Hum;Kang, Bo-An;Kim, Sang-Bok;Hwang, Kyu-Seog;Shim, Yeon-A
    • Journal of the Korean Ceramic Society
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    • v.39 no.9
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    • pp.884-889
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    • 2002
  • In order to investigate the calcium phosphate forming ability of nanocrystalline $ZrO_2$ film, we prepared $ZrO_2/Si$ structure by using a chemical solution deposition with a zirconium naphthenate as a starting material. Precursor sol was spin-coated onto the (100)Si substrate and prefired at 500$^{\circ}C$ for 10 min in air, followed by final annealing at 800$^{\circ}C$ for 30 min in air. Crystallinity of the annealed film was examined by X-ray diffraction analysis. Surface morphology and surface roughness of the film were characterized by field emission-scanning electron microscope and atomic force microscope. After annealing, nanocrystalline $ZrO_2$ grains were obtained on the surface of the film with a homogeneous interface between the film and substrate. After immersion for 1 or 5 days in a simulated body fluid, formation of calcium phosphate was observed on $ZrO_2$ film annealed at 800$^{\circ}C$ by energy dispersive X-ray spectrometer. The fourier transform infrared spectroscopy revealed that carbonate was substituted into the calcium phosphate.

A Study on the Cementation Reaction of Copper-containing Waste Etching Solution to the Shape of Iron Samples (철 샘플에 따른 구리 함유 폐에칭액의 시멘테이션 반응에 대한 연구)

  • Kim, Bo-Ram;Jang, Dae-Hwan;Kim, Dae-Weon
    • Clean Technology
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    • v.27 no.3
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    • pp.240-246
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    • 2021
  • The waste etching solution for chip on film (COF) contained about 3.5% copper, and it was recovered through cementation using iron samples. The effect of cementation with plate, chip, and powder iron samples was investigated. The molar ratio (m/r) of iron to copper was used as a variable in order to increase the recovery rate of copper. As the molar ratio increased, the copper content in the solution rapidly decreased at the beginning of the cementation reaction. Before and after the reaction, the copper content of the solution was determined by Inductively Coupled Plasma (ICP) using copper concentration according to time. After cementation at room temperature for 1 hour, the recovery rate of copper had increased the most in the iron powder sample, having the largest specific surface area of the samples, followed by the chip and plate samples. The recovered copper powder was characterized for its crystalline phase, morphology, and elemental composition by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Energy-dispersive X-ray spectroscopy (EDS), respectively. Copper and unreacted iron were present together in the iron powder samples. The optimum condition for recovering copper was obtained using iron chips with a molar ratio of iron to copper of 4 giving a recovery rate of about 98.4%.

Hydrogen Permeation Performance of Pd, Pd/Cu Membranes Manufactured through Electroless Plating (무전해 도금을 이용해 제작한 Pd, Pd/Cu 분리막의 수소 투과 성능)

  • Jeong In, Lee;Min Chang, Shin;Xuelong, Zhuang;Jae Yeon, Hwang;Chang-Hun, Jeong;Jung Hoon, Park
    • Membrane Journal
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    • v.32 no.6
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    • pp.456-464
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    • 2022
  • Hydrogen permeation performance was analyzed by manufacturing Pd and Pd-Cu membranes through electroless plating. As a support for the Pd and Pd-Cu membranes, α-Al2O3 ceramic hollow fiber were used. Pd-Cu membrane was manufactured through sequential electroless plating, and then annealing was performed at 500°C, for 18 h in a hydrogen atmosphere to make Pd and Cu alloy. After annealing, the Pd-Cu membrane confirmed that the alloy was formed through EDS (Energy Dispersive X-ray Spectroscopy) and XRD (X-ray Diffraction) analysis. In addition, the thickness of the Pd and Pd-Cu plating layers were measured to be about 3.21 and 3.72 µm, respectively, through SEM (Scanning Electron Microscope) analysis. Hydrogen permeation performance was tested for hydrogen permeation in the range of 350~450°C and 1~4 bar in hydrogen single gas and mixed gas (H2, N2). In a single hydrogen gas, Pd and Pd-Cu membranes have flux of up to 54.42 and 67.17 ml/cm2⋅ min at 450 °C and 4 bar. In the mixed gas, it was confirmed that the separation factors of 1308 and 453 were obtained under the conditions of 450 °C and 4 bar.

Microwave sintering of Fly Ash substituted body (석탄회가 첨가된 점토의 마이크로파를 이용한 소결)

  • 김석범;한정환;김유택
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.3
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    • pp.513-517
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    • 1998
  • Fly ashes mixed with clay as 70:30 weight percent were sintered by microwave energy and a 2.45 Ghz kitchen model microwave oven was used. Samples were sintered at $1,150^{\circ}C$ and kept at that temperature up to 50 minutes by 10 minutes intervals. Microstructures were taken by Scanning Electron Microscope (SEM) and Energy Dispersive Spectrometry (EDS) analysis of a raw fly ash was taken. X-ray diffraction analysis was done, and compressive strengths and apparent densities were measured. Pore sizes of the samples became smaller as time passed by, but compressive strengths and apparent densities did not change much. Numerical analysis on the microwave heated system was carried out in order to figure out heat transfer phenomena in the cavity.

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Chlorination of TRU/RE/SrOx in Oxide Spent Nuclear Fuel Using Ammonium Chloride as a Chlorinating Agent

  • Yoon, Dalsung;Paek, Seungwoo;Lee, Sang-Kwon;Lee, Ju Ho;Lee, Chang Hwa
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.20 no.2
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    • pp.193-207
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    • 2022
  • Thermodynamically, TRUOx, REOx, and SrOx can be chlorinated using ammonium chloride (NH4Cl) as a chlorinating agent, whereas uranium oxides (U3O8 and UO2) remain in the oxide form. In the preliminary experiments of this study, U3O8 and CeO2 are reacted separately with NH4Cl at 623 K in a sealed reactor. CeO2 is highly reactive with NH4Cl and becomes chlorinated into CeCl3. The chlorination yield ranges from 96% to 100%. By contrast, U3O8 remains as UO2 even after chlorination. We produced U/REOx- and U/SrOx-simulated fuels to understand the chlorination characteristics of the oxide compounds. Each simulated fuel is chlorinated with NH4Cl, and the products are dissolved in LiCl-KCl salt to separate the oxide compounds from the chloride salt. The oxide compounds precipitate at the bottom. The precipitate and salt phases are sampled and analyzed via X-ray diffraction, scanning electron microscope-energy dispersive spectroscopy, and inductively coupled plasma-optical emission spectroscopy. The analysis results indicate that REOx and SrOx can be easily chlorinated from the simulated fuels; however, only a few of U oxide phases is chlorinated, particularly from the U/SrOx-simulated fuels.

CORROSION BEHAVIOR OF NI-BASE ALLOYS IN SUPERCRITICAL WATER

  • Zhang, Qiang;Tang, Rui;Li, Cong;Luo, Xin;Long, Chongsheng;Yin, Kaiju
    • Nuclear Engineering and Technology
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    • v.41 no.1
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    • pp.107-112
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    • 2009
  • Corrosion of nickel-base alloys (Hastelloy C-276, Inconel 625, and Inconel X-750) in $500^{\circ}C$, 25MPa supercritical water (with 10 wppb oxygen) was investigated to evaluate the suitability of these alloys for use in supercritical water reactors. Oxide scales formed on the samples were characterized by gravimetry, scanning electron microscopy/energy dispersive spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The results indicate that, during the 1000h exposure, a dense spinel oxide layer, mainly consisting of a fine Cr-rich inner layer ($NiCr_{2}O_{4}$) underneath a coarse Fe-rich outer layer ($NiFe_{2}O_{4}$), developed on each alloy. Besides general corrosion, nodular corrosion occurred on alloy 625 possibly resulting from local attack of ${\gamma}$" clusters in the matrix. The mass gains for all alloys were small, while alloy X -750 exhibited the highest oxidation rate, probably due to the absence of Mo.

Synthesis and Characterization of Nanoporous Zirconia (나노세공 Zirconia의 합성 및 특성평가)

  • Woo, Seung-Sik;Kim, Ho-Kun
    • Journal of Powder Materials
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    • v.14 no.5
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    • pp.309-314
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    • 2007
  • Zirconia powders with nano size pores and high specific surface areas were synthesized via aqueous precipitation and hydrothermal synthetic method using $ZrOCl_28H_2O$ and $NH_4OH$ under pH=11 and ambient condition. By this reaction. zirconia hydrate $(ZrO_x(OH)_{4-2x})$ was primarily synthesized and the obtained zirconia hydrate was heat treated hydrothermally using an autoclave at various temperatures under pH=11. X-ray diffraction, Scanning electron microscopy, Energy dispersive X-ray spectroscopy, FT-IR, Raman, Particle size analysis, DTA-TG, and BET techniques were used for the characterization of the powder. The synthesized zirconia showed an amorphous phase, however, the phase was transformed to the crystalline state during the hydrothermal process. The observed crystalline phase above $160^{\circ}C$ was a mixed phase of monoclinic and tetragonal zirconia. By the BET analysis, it was found that the specific surface area was ranged in $126{\sim}276m^2/g$ and the zirconia had the cylindrical shaped pores with average diameter of $2{\sim}7nm$.

Comparative Tooth Morphology and Qualitative Analysis on the Enamel Surface using Energy Dispersive X-ray Spectroscopy in the White-Toothed Shrew Crocidura lasiura and C. suaveolens and the Red-Toothed Shrew Sorex caecutiens from Korea (한국 땃쥐속 우수리땃쥐 Crocidura lasiura와 작은땃쥐 C. suaveolens, 뒤쥐속 뒤쥐 Sorex caecutiens의 치아형태와 Energy Dispersive X-ray Spectroscopy를 이용한 법랑질 표면의 정성적 분석 비교)

  • Jeong, Soon-Jeong
    • Journal of dental hygiene science
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    • v.13 no.2
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    • pp.203-212
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    • 2013
  • The tooth morphology and qualitative mineral contents on enamel surface using energy dispersive X-ray spectroscopy, (EDX) were examined in the white-toothed shrew (genus Crocidura ) Crocidura lasiura and C. suaveolens and the red-toothed shrew (genus Sorex) Sorex caecutiens. In the case of C. lasiura and C. suaveolens, dental formula was found I 3/1 C1/1 P1/1 M3/3=28. The upper 1st and 2nd molars had an unequal W-shape formed by 5 cusps on the crown. The 3rd molar was found one-third the size of those of 1st and 2nd molars. The upper 1st incisor had two different sized hook-shapes and the lower 1st incisor was even. In the case of S. caecutiens, dental formula was found to be I3/1 C1/1 P3/1 M3/3=32. The upper 1st and 2nd molars had an equal W-shape on crown. The upper 3rd molar was half the size of those of the other molars. The upper 1st incisor possessed two similar sized hook-shapes and the lower 1st incisor had an uneven and serrated form. A comparison with the dental and cranial measurements revealed C. lasiura to be the largest of the three species (p<0.001) and C. suaveolens and S. caecutiens were similar in size (p>0.05). A qualitative analysis of mineral contents on enamel surface of the lower 1st incisor and lower 1st molar using EDX revealed C, O, P, Ca and Cu in all specimens and Pb was detected in several enamel specimens. No significant differences in the mineral contents (% weight) were observed among the three species (p>0.05). Fe was only detected on enamel surface of S. caecutiens with red pigmented teeth. Therefore, Fe is responsible for the red tip of the teeth. These results suggest that tooth morphological characteristics including the color of the tooth tip might be used as the key classifying species belonging to Crocidura and Sorex.

The Analysis of CdS and CdTe Thin Film at the Processes of Manufacturing CdTe Solar Cells (CdTe 태양전지 제조 공정에 따라 변화하는 CdS와 CdTe 박막의 물성 변화 분석)

  • Chun, Seungju;Jung, Younghun;Choi, Suyoung;Tark, Sung Ju;Kim, Jihyun;Kim, Donghwan
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.106.2-106.2
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    • 2011
  • 다층 박막 구조로 이루어진 CdS/CdTe 태양전지의 경우, 각각의 박막이 다양한 제조 공정을 거치면서 물성특성의 변화를 겪게 된다. 각각의 박막이 고온의 열처리 공정과, $CdCl_2$ 용액 처리 및 후면 산화막 제거 공정 등을 거치게 되면서 겪게 되는 물성 변화 분석을 살펴보고자 한다. 각각의 박막 제조 방식은 일반적으로 사용되는 방식으로, CdS의 경우는 용액성장법(Chemical Bath Deposition, CBD), CdTe의 경우는 근접승화법(Closed Space Sublimaition, CSS)을 사용했으며, X-Ray Diffractometer (XRD), Raman spectroscopy, Field Emission Scanning Electron Microscope (FE-SEM), Energy Dispersive Spectroscopy (EDS), X-ray Photoelectron Spectroscopy (XPS) 등을 이용하여 분석하였다. 각각의 셀 제조 공정을 거치면서 CdS, CdTe 박막들은 결정, 광 특성, 성분 변화를 보였다.

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Evolution pathway of CZTSe nanoparticles synthesized by microwave-assisted chemical synthesis

  • Reyes, Odin;Sanchez, Monica F.;Pal, Mou;Llorca, Jordi;Sebastian, P.J.
    • Advances in nano research
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    • v.5 no.3
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    • pp.203-214
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    • 2017
  • In this study we present the reaction mechanism of $Cu_2ZnSnSe_4$ (CZTSe) nanoparticles synthesized by microwave-assisted chemical synthesis. We performed reactions every 10 minutes in order to identify different phases during quaternary CZTSe formation. The powder samples were analyzed by x-ray diffraction (XRD), Raman spectroscopy, energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The results showed that in the first minutes copper phases are predominant, then copper and tin secondary phases react to form ternary phase. The quaternary phase is formed at 50 minutes while ternary and secondary phases are consumed. At 60 minutes pure quaternary CZTSe phase is present. After 60 minutes the quaternary phase decomposes in the previous ternary and secondary phases, which indicates that 60 minutes is ideal reaction time. The EDS analysis of pure quaternary nanocrystals (CZTSe) showed stoichiometric relations similar to the reported research in the literature, which falls in the range of Cu/(Zn+Sn): 0.8-1.0, Zn/Sn: 1.0-1.20. In conclusion, the evolution pathway of CZTSe synthesized by this novel method is similar to other synthesis methods reported before. Nanoparticles synthesized in this study present desirable properties in order to use them in solar cell and photoelectrochemical cell applications.