• Title/Summary/Keyword: X-Ray Photoelectron Spectroscopy

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Lithium-silicate coating on Lithium Nickel Manganese Oxide (LiNi0.7Mn0.3O2) with a Layered Structure

  • Kim, Dong-jin;Yoon, Da-ye;Kim, Woo-byoung;Lee, Jae-won
    • Journal of Powder Materials
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    • v.24 no.2
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    • pp.87-95
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    • 2017
  • Lithium silicate, a lithium-ion conducting ceramic, is coated on a layer-structured lithium nickel manganese oxide ($LiNi_{0.7}Mn_{0.3}O_2$). Residual lithium compounds ($Li_2CO_3$ and LiOH) on the surface of the cathode material and $SiO_2$ derived from tetraethylorthosilicate are used as lithium and silicon sources, respectively. Powder X-ray diffraction and scanning electron microscopy with energy-dispersive spectroscopy analyses show that lithium silicate is coated uniformly on the cathode particles. Charge and discharge tests of the samples show that the coating can enhance the rate capability and cycle life performance. The improvements are attributed to the reduced interfacial resistance originating from suppression of solid-electrolyte interface (SEI) formation and dissolution of Ni and Mn due to the coating. An X-ray photoelectron spectroscopy study of the cycled electrodes shows that nickel oxide and manganese oxide particles are formed on the surface of the electrode and that greater decomposition of the electrolyte occurs for the bare sample, which confirms the assumption that SEI formation and Ni and Mn dissolution can be reduced using the coating process.

Preparation of ZnO2 Nanoparticles Using Organometallic Zinc(II) Isobutylcarbamate in Organic Solvent

  • Kim, Kyung-A;Cha, Jae-Ryung;Gong, Myoung-Seon;Kim, Jong-Gyu
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.431-435
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    • 2014
  • Zinc peroxide nanoparticles ($ZnO_2$ NPs) were prepared by reacting zinc(II) isobutylcarbamate, as an organometallic precursor, with hydrogen peroxide ($H_2O_2$) at $60^{\circ}C$. Polyethylene glycol and polyvinylpyrrolidone were used as stabilizers, which suppressed aggregation of the $ZnO_2$ NPs. Conditions such as concentrations of $H_2O_2$ and the stabilizer were systemically controlled to determine their effect on the formation of nano-sized $ZnO_2$ NPs. The formation of stable $ZnO_2$ NPs was confirmed by UV-vis, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction. The TEM images revealed that polyvinylpyrrolidone-stabilized $ZnO_2$ NPs (diameter, 10-30 nm) were well dispersed in the organic solvent. Quite pure ZnO NPs were obtained from the peroxide powder by simple heat treatment of $ZnO_2$. The transition temperature of $170^{\circ}C$ was determined by differential scanning calorimetry.

The Composition of the Rare Earth Based Conversion Coating Formed on AZ91D Magnesium Alloy

  • Chang, Menglei;Wu, Jianfeng;Chen, Dongchu;Ye, Shulin
    • Corrosion Science and Technology
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    • v.17 no.1
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    • pp.1-5
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    • 2018
  • As structural materials, magnesium (Mg) alloys have been widely used in the fields of aviation, automobiles, optical instruments, and electronic products. There are few studies on the effect of coating conditions on the compositional variation during the formation process of the conversion coatings. Rare-earth based conversion coating on AZ91 magnesium alloy was prepared in ceric sulfate and hydrogen peroxide contained solution. The element composition and valence as well as their distribution in the coating were analyzed with energy dispersive X-ray spectroscopy (EDS), Electron probe micro-analyzer (EPMA), X-ray photoelectron spectroscopy (XPS). The effect of treating process on the element composition were also studied. It was found that the conversion coating surface consists of Mg, Al, O, Ce, and the weight content of Ce in the coating was affected by the treating solution concentration and immersion time; the Ce element was distributed in the coating non-uniformly and existed in the form of $Ce^{+3}$ and $Ce^{+4}$, while the O element existed in the form of $OH^-$, $O^{2-}$, $H_2O$. Based on microscopic analysis results, the electrochemical deposition mechanism on the micro-anode and micro-cathode in the process of the coating growth was suggested.

Biogenic Nano-Synthesis; towards the Efficient Production of the Biocompatible Gold Nanoparticles

  • Ghodake, Gajanan;Eom, Chi-Yong;Kim, Si-Wouk;Jin, Eon-Seon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.10
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    • pp.2771-2775
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    • 2010
  • We present a rapid biogenic method for the production of nanoscale gold particles using pear extract. The formation and stability of pear-derived gold nanoparticles (Pear-AuNPs) were monitored by ultraviolet-visible spectroscopy. Their morphology, elemental composition and crystalline phase were determined by transmission electron microscopy, energy-dispersive X-ray spectroscopy and selected area electron diffraction. The average core size of crystalline Pear-AuNPs was in the range of $10{\pm}5\;nm$ and the observed morphology was spherical. The X-ray photoelectron spectrum showed a strong peak for the pure 'Au' phase. The circular dichroism spectrum indicated the natural capping ability of the pear extract, which generated peptide-gold nanoparticles. These nanoparticles were stable in aqueous solution for two months. A cell viability assay of Pear-AuNPs showed biocompatibility with human embryonic kidney 293 cells. Accordingly, this eco-friendly process for the bio-mimetic production of Pear-AuNPs is nontoxic in nature; consequently, it will find potential application in nano-biotechnology.

Phase identification of $C_3N_4$ in CN films prepared by rf plasma chemical vapor deposition and dc magnetron sputtering

  • Fu, Dejun;Wu, Dawei;Zhang, Zhihong;Meng, Xianquan;He, Mengbing;Guo, Huaixi;Peng, Yougui;Fan, Xiangjun
    • Journal of the Korean Vacuum Society
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    • v.7 no.s1
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    • pp.140-148
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    • 1998
  • We prepared $C_3N_4$ films by rf plasma enhanced chemical vapor deposition(PCVD) and alternating $C_3N_4$/TiN composite films by dc magnetron sputtering. X-ray diffraction (XRD) and transmission electron diffraction (TED) revealed that the structure of the films is amorphous or polycrystalline, depending on deposition conditions and heat treatment. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) spectroscopy confirmed the presence of $sp_3\; and sp _2$ hybridized C atoms bonded with N atoms in the tetrahedral and hexagonal configurations, respectively. Graphite-free $C_3N_4$ films were obtained by PCVD under optimal conditions. To prepare well crystallized $C_3N_4$ films by magnetron sputtering, we introduced negatively biased gratings in the sputtering system. CN films deposited at grating voltages (Vg) lower than 400V are amorphous. Crystallites of cubic and $\beta$-$C_3N_4$ were formed at increased voltages.

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Microstructural characterization of accident tolerant fuel cladding with Cr-Al alloy coating layer after oxidation at 1200 ℃ in a steam environment

  • Park, Dong Jun;Jung, Yang Il;Park, Jung Hwan;Lee, Young Ho;Choi, Byoung Kwon;Kim, Hyun Gil
    • Nuclear Engineering and Technology
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    • v.52 no.10
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    • pp.2299-2305
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    • 2020
  • Zr alloy specimens were coated with Cr-Al alloy to enhance their resistance to oxidation. The coated samples were oxidized at 1200 ℃ in a steam environment for 300 s and showed extremely low oxidation when compared to uncoated Zr alloy specimens. The microstructure and elemental distribution of the oxides formed on the surface of Cr-Al alloys have been investigated by transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). A very thin protective layer of Cr2O3 formed on the outer surface of the Cr-Al alloy, and a thin Al2O3 layer was also observed in the Cr-Al alloy matrix, near the surface. Our results suggest that these two oxide layers near the surface confers excellent oxidation resistance to the Cr-Al alloy. Even after exposure to a high temperature of 1200 ℃, inter-diffusion between the Cr-Al alloy and the Zr alloy occurred in very few regions near the interface. Analysis of the inter-diffusion layer by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDS) measurement confirmed its identity as Cr2Zr.

Atmospheric chemical vapor deposition of graphene on molybdenum foil at different growth temperatures

  • Naghdi, Samira;Rhee, Kyong Yop;Kim, Man Tae;Jaleh, Babak;Park, Soo Jin
    • Carbon letters
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    • v.18
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    • pp.37-42
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    • 2016
  • Graphene was grown on molybdenum (Mo) foil by a chemical vapor deposition method at different growth temperatures (1000℃, 1100℃, and 1200℃). The properties of graphene were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy, and Raman spectroscopy. The results showed that the quality of the deposited graphene layer was affected by the growth temperature. XRD results showed the presence of a carbide phase on the Mo surface; the presence of carbide was more intense at 1200℃. Additionally, a higher I2D/IG ratio (0.418) was observed at 1200℃, which implies that there are fewer graphene layers at this temperature. The lowest ID/IG ratio (0.908) for the graphene layers was obtained at 1200℃, suggesting that graphene had fewer defects at this temperature. The size of the graphene domains was also calculated. We found that by increasing the growth temperature, the graphene domain size also increased.

A Study on Practicality of Condition Monitoring Method of Accelerated Thermal Aging CSPE (가속열화 된 CSPE 상태감시법 유효성 평가)

  • Lee, Jung-Hoon;Goo, Cheol-Soo;Kim, In-Yong;Shin, Yong-Deok
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.60 no.11
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    • pp.2088-2092
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    • 2011
  • The accelerated thermal aging of CSPE(chloro sulfonate polyethylene) of test cables were carried out for the period equal to 10, 20 and 30 years in air at $100^{\circ}C$, respectively. The CSPE cables(TAIHAN electric wire Co. Ltd) which installed in nuclear power plant for three years were used as starting materials. Condition monitering methods of the accelerated thermal aging of CSPE cables were estimated through indenter modulus and OIT(oxidation induction time) of IEC 62582, and those were newly estimated through volume electrical resistivity, ultrasound reflection time, density, FE-SEM(field emission scanning electron microscopy), XPS(x-ray photoelectron spectroscopy), EDS(energy dispersive spectroscopy), and WD-XRF(wavelength dispersive x-ray fluorescence). A new condition monitoring methods of the accelerated thermal aging of CSPE cables were generally coincident with trend of indenter modulus expect EDS, XPS and XRF. A volume electrical resistivity among new condition monitoring methods of the accelerated thermal aging of CSPE cables is excellent. It is considered that life-time of CSPE cable can be predicted through volume electrical resistivity, if CSPE jacket was aged for period such as more than 20 years.

Synthesis of direct-patternable ZnO film incorporating Pt Nanoparticles

  • Choi, Yong-June;Park, Hyeong-Ho;Reddy, A.Sivasankar;Park, Hyung-Ho
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.11a
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    • pp.369-369
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    • 2007
  • ZnO film has been investigated during several decades because it has excellent optical property like a transmittance among the range of visible light for using transparent conducting oxide (TCO) films. But ZnO film has not enough conductivity for applying to TCO devices. Therefore we synthesized platinum nanoparticles and they incorporated into ZnO due to improve the electrical property of ZnO film by sol-gel synthesis method. Also, we fabricated photosensitive ZnO thin film containing Pt nanoparticles by sol-gel process and spin-coating for using photochemical solution deposition. Photosensitive ZnO film could carry out the direct-pattern which allow the etching process to be convenient. The optical and electrical properties of ZnO film with or without various atomic percent of Pt nanoparticles annealed at various temperatures were investigated by using UV-Vis spectroscopy and 4-point probe method, respectively. We characterized the ZnO thin film containing Pt nanoparticles using X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy.

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Sputtering effect on chemical state changes in amorphous Ga-In-Zn-O thin film

  • Lee, Mi-Ji;Gang, Se-Jun;Baek, Jae-Yun;Kim, Hyeong-Do;Jeong, Jae-Gwan;Lee, Jae-Cheol;Lee, Jae-Hak;Sin, Hyeon-Jun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.134-134
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    • 2010
  • Ga-In-Zn-O 물질은 비정질상태에서 높은 전하 운동성을 가지고 있으며 차세대 투명전극 thin film transistor 대안 소재로 각광받고 있다. 그런데 이 물질은 ion sputtering에 따라 전기적인 특성에 큰 변화가 관찰되고 있으며, 이는 표면에서의 화학적 상태가 전기적 특성을 좌우할 것이라는 것을 의미한다. 또한 보다 안정적이고 신뢰적인 소자를 구현하기 위해서는 ion sputtering에 의한 표면에서의 화학적 특성 변화를 이해하는 것이 매우 중요하다는 것을 의미한다. 본 연구에서는 $Ga_2O_3:In_2O_3$:ZnO의 비율이 각각 1:1:1, 2:2:1, 3:2:1 그리고 4:2:1인 시료를 $Ne^+$이온을 이용하여 sputtering하면서 표면에 민감한 분광분석 기법인 x-ray photoelectron spectroscopy와 x-ray absorption spectroscopy를 이용하여 분광정보의 변화들을 연구하였다. 실험에 의하면, Ga 3d의 양에 비해서 In 4d, Zn 3d의 양은 sputtering 시간에 따라서 각 각 양이 줄어들었으며, 전체적으로 보다 산화가가 높은 경향을 보였으며, valence band maximum 근처에 subgap state를 형성하는 것을 관찰하였다. 또한 sputtering을 계속하는 경우 In 3d, In 4d, 및 Fermi energy 근처에 metallic state가 형성되는 것을 관찰하였다. 이러한 subgap state와 metallic state의 관측은 각기 sputtering에 따라서, 아직 명확하지는 않지만, surface state의 형성 및/혹은 oxygen interstitial의 형성 그리고 metallic In의 형성 및/혹은 oxygen defect의 형성이 이루어지는 것을 의미한다.

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