• Title/Summary/Keyword: Chemical structure analysis

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Surface Analysis of Modified Polymer Samples by X-Ray Photoelectron Spectroscopy and Rutherford Backscattering Spectroscopy (X-선 광전자 분광법 및 라더포드 후방산란법에 의한 개질된 고분자 시료의 표면분석)

  • Park, Sung-Woo;Kim, Dong-Hwan;Kim, Young-Man;Park, Byung-Sun;Han, Wan-Soo;Suh, Bae-Suk
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.301-313
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    • 1994
  • X-Ray Photoelectron Spectroscopy(XPS) and Rutherford Backscattering Spectroscopy(RBS) are used for the analysis of additives, examination of chemical structure and determination of identity with qualitative and quantitative analysis of surface elements, binding energy level and depth profiling in the surface. We analyzed surface of polyethylene, acrylonitrile butadien rubber, polypropylene, glass, fiber and paper treated with $XeF_2$ or C-F plasma by XPS and RBS. It was found that fluoro element was penetrated to sample surface and the distribution of surface elements are different than untreated samples.

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Chemical Structural Features of Humic-like Substances (HULIS) in Urban Atmospheric Aerosols Collected from Central Tokyo with Special Reference to Nuclear Magnetic Resonance Spectra

  • Katsumi, Naoya;Miyake, Shuhei;Okochi, Hiroshi
    • Asian Journal of Atmospheric Environment
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    • v.12 no.2
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    • pp.153-164
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    • 2018
  • We measured $^1H$ and $^{13}C$ nuclear magnetic resonance (NMR) spectra of Humic-like substances (HULIS) in urban atmospheric aerosols isolated by diethylaminoethyl (DEAE) and hydrophilic-lipophilic balance (HLB) resin to characterize their chemical structure. HULIS isolated by DEAE resin were characterized by relatively high contents of aromatic protons and relatively low contents of aliphatic protons in comparison with HULIS isolated by HLB resin, while the contents of protons bound to oxygenated aliphatic carbon atoms were similar. These results were consistent with the results of the $^{13}C$ NMR analysis and indicate that hydrophobic components were more selectively adsorbed onto HLB, while DEAE resins selectively retained aromatic carboxylic acids. Furthermore, we demonstrated that the chemical structural features of HULIS were significantly different between spring and summer samples and that these disparities were reflective of their different sources. The estimated concentrations of HULIS in spring were found to be regulated by vehicle emissions and pollen dispersion, while the behavior of HULIS in summer was similar to photochemical oxidant and nitrogen dioxide concentrations. The proportion of aliphatic protons for summer samples was higher than that for spring samples, while the proportion of aromatic protons for summer samples was lower than that for spring samples. These seasonal changes of the chemical structure may also involve in their functional expression in the atmosphere.

이차전지 양극활물질의 chemical state 측정을 위한 X0ray Induced Electron Emission Spectroscopy (XIEES)의 활용

  • 이재철;송세안;임창빈
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.167-167
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    • 2000
  • 전지 재료의 충방전 과정 연구에는 X-선 분말회절(x-ray powder diffraction techniques)과 중성자회절을 많이 사용하였다. 하지만 이러한 분석기술은 long-range order의 구조에 관한 정보를 제공하는데 유용하지만 atomic scale의 구조에 관한 정보를 얻기에는 한계가 있다. Li 전지에서의 전기화학적 반응에서는 cathode 물질에 포함된 전이금속의 산화, 환원 반응에 의한 Li 이온의 intercalation (charge process)과 deintercalation (discharge process) 현상이 일어난다. 이러한 충방전 과정은 알려지지 않은 다양한 형태의 위상 변화를 동반하게 되는데 x-선 이나 중성자를 이용한 powder diffraction techniques 로는 단지 정성적인 결정학적 정보를 얻을 수 있다. 따라서 최근에 원자 단위의 local structure에 관한 정보와 electrochemical state에 관한 정보를 동시에 얻을 수 있는 X-ray Absorption Fine Structure (XAFS) 분석기술을 Li 전지분석에 활용하기 시작하였다. XAFS는 하나의 x-ray 흡수원자에 대해서 주변원자들의 원자구조에 관한 정보와 구성 원소의 electrochemical state에 관한 정보를 얻을 수 있는 분석방법이다. X-ray Induced Electron Emission Spectroscopy (XIEES)는 x-ray에 의해서 방출된 전자를 검출하여 스펙트럼을 얻는 기능을 함축적으로 나타낸 것으로, x-ray를 물질 표면에 조사하여 발생하는 광전자, Auger 전자, 이차전자 등을 전자검출기(Channel Electron Multiplier: CEM)로 검출하는 기능과, 시료를 투과한 x-ray와 시료에서 발생하는 형광 x-ray를 비례계수기로 검출하는 기능을 가지고 있다. 이러한 검출 능력을 바탕으로 EXAFS, XANES, Standing Wave Technique, Elemental Composition Analysis, DXRD, Total Reflection Technique 등을 이용하여 물질을 구성하고 있는 원소의 성분, 미세원자구조, 전자구조에 관한 정보를 얻을 수 있는 새로운 spectrometer이다. 본 연구에서는 자체 개발한 XIEES의 XAFS 기능을 이용하여 여러 가지 방법으로 제조한 LiMn2-xO4와 LiMnO2, MnO2에서 Mn K-absorption edge에 대한 chemical state 변화를 측정하였다. Absorption edge에서 chemical shift를 측정하기 위해서는 방사광 가속기 수준의 에너지 분해능(~0.3eV)이 필요하다. 이번 연구에서는 SiO2(3140) monochromator를 사용하고 여기에 맞는 적절한 parameter를 적용하여 x-ray 에너지 분해능을 포항방사광가속기 수준으로 개선하였다. XIEES에서 얻은 스펙트럼과 포항방사광가속기에서 얻은 스펙트럼을 비교하였다. Chemical shift가 일어나는 경향은 두 실험 결과가 잘 일치하였다.

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Melt and Recrystallization Behavior of Syndiotactic Polypropylene and Isotactic Polypropylene (신디오택틱 폴리프로필렌과 아이소택틱 폴리프로필렌의 용융과 재결정화)

  • Lee, Sang-Won;Huh, Wan-Soo;Hyun, Uk;Lee, Dong-Ho;Noh, Seok-Kyun
    • Polymer(Korea)
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    • v.27 no.6
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    • pp.521-527
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    • 2003
  • It was found that polypropylene shows rearrangement of crystal structure during the melting process. For the analysis of recrystallization behavior, the change of dynamic mechanical property, crystallinity, and crystal structure were studied by DSC, FT-IR, SAXS, and DMA. Melt-recrystallization-remelting behavior of iPP was clearly observed when iPP was cooled down kom the melt more rapidly. Elastic modulus of iPP increased during the recrystallization process but crystallinity of iPP shows constant value. Furthermore, the full width of half mean of SAXS pattern decreased about 30%, and intra-lamella ordering of iPP increased during the melt process but is was not found for sPP.

Structure and Bonding of Ni(C6H4-nFn)(CO)2 (C6H4=benzyne, n=1-4) Complexes (Ni(C6H4-nFn)(CO)2 (C6H4=benzyne, n=1-4) 착물의 구조 및 화학결합)

  • Ghiasi, Reza;Hashemian, Saeedeh;Irajee, Oranoos
    • Journal of the Korean Chemical Society
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    • v.55 no.2
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    • pp.183-188
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    • 2011
  • The electronic structure and properties of Ni$(C_6H_{4-n}F_n)(CO)_2$ ($C_6H_4$=benzyne, n=1-4) complexes have been investigated using hybrid density functional B3LYP theory. Both aromatic natures and nucleus independent chemical shift (NICS) of the benzyne rings have been analyzed. Among mono-, di-, and tri-fluorinated complexes, 3-F, 3,6-F, and 4-H are the most stable isomers, respectively. NICS values calculated at the several points above the ring centers are consistent with those based on the relative energies of the complexes. The atoms in molecules (AIM) analysis indicates that Ni-C bond distance is well correlated with the electron density of a ring critical point (${\rho}_{rcp}$) in all species.

Synthesis of Novel Platinum Precursor and Its Application to Metal Organic Chemical Vapor Deposition of Platinum Thin Films

  • Lee, Sun-Sook;Lee, Ho-Min;Park, Min-Jung;An, Ki-Seok;Kim, Jin-Kwon;Lee, Jong-Heun;Chung, Taek-Mo;Kim, Chang-Gyoun
    • Bulletin of the Korean Chemical Society
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    • v.29 no.8
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    • pp.1491-1494
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    • 2008
  • A novel platinum aminoalkoxide complex, Pt$(dmamp)_2$ has been prepared by the reaction of cis-$(py)_2PtI_2$ with two equivalents of Na(dmamp) (dmamp = 1-dimethylamino-2-methyl-2-propanolate). Single-crystal X-ray crystallographic analysis shows that the Pt(dmamp)2 complex keeps a square planar geometry with each two nitrogen atoms and two oxygen atoms having trans configuration. Platinum films have been deposited on TaN/ Ta/Si substrates by metal organic chemical vapor deposition (MOCVD) using Pt$(dmamp)_2$. As-deposited platinum thin films did not contain any appreciable amounts of impurities except a little carbon. As the deposition temperature was increased, the films resistivity and deposition rate increased. The electrical resistivity (13.6 $\mu\Omega$cm) of Pt film deposited at 400 ${^{\circ}C}$ is a little higher than the bulk value (10.5 $\mu\Omega$cm) at 293 K. The chemical composition, crystalline structure, and morphology of the deposited films were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, and atomic force microscopy.

Optimization red emission of SrMoO4: Eu3+ via hydro-thermal co-precipitation synthesis using orthogonal experiment

  • Tan, Yongjun;Luo, Xuedan;Mao, Mingfu;Shu, Dehua;Shan, Wenfei;Li, Guizhi;Guo, Dongcai
    • Current Applied Physics
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    • v.18 no.11
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    • pp.1403-1409
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    • 2018
  • In the present study, the $SrMoO_4:Eu^{3+}$ phosphors has been synthesized through hydro-thermal co-precipitation method, and single factor and orthogonal experiment method was adopted to find optimal synthesis condition. It is interesting to note that hydro-thermal temperature is a prominent effect on the luminescent intensity of $SrMoO_4:Eu^{3+}$ red phosphor, followed by co-precipitation temperature, calcining time, and the doping amount of $Eu^{3+}$. The optimal synthesis conditions were obtained: hydro-thermal temperature is $145^{\circ}C$, co-precipitation temperature is $35^{\circ}C$, the calcining time is 2.5 h, and the doping amount of activator $Eu^{3+}$ is 25%. Subsequently, the crystalline particle size, phase composition and morphology of the synthesized phosphors were evaluated by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). The results show that these phosphors possess a scheelite-type tetragonal structure, and the particle size is about $0.2{\mu}m$. Spectroscopic investigations of the synthesized phosphors are carried out with the help of photo-luminescence excitation and emission analysis. The studies reveal that $SrMoO_4:Eu^{3+}$ phosphor efficiently convert radiation of 394 nm-592 and 616 nm for red light, and the luminescence intensity of $SrMoO_4:Eu^{3+}$ phosphors is improved. $SrMoO_4:Eu^{3+}$ phosphors may be a potential application for enhancing the efficiency of white LEDs.

Development of Multi-sample Loading Device for TEM Characterization of Hydroxyapatite Nanopowder

  • Lee, Jong-Moon;Kim, Jung-Kyun;Jeong, Jong-Man;Kim, Jin-Gyu;Lee, Eunji;Kim, Youn-Joong
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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    • pp.788-792
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    • 2013
  • A shortcoming of using transmission electron microscopy (TEM) for structural analysis via electron diffraction is the relatively large error of the measurements as compared to X-ray diffraction. To reduce these errors, various internal standard methods from earlier studies have been widely used. We developed a new device to facilitate the application of internal standard methods in preparation of TEM grids used for nanopowder analysis. Through the application of a partial mask on the TEM grid, both the internal standards and the research materials can be loaded on the same grid. Through this process, we conducted a TEM analysis that compared synthetic hydroxyapatite (HAp) nanopowder to bone apatite from a bovine femur. We determined that the accuracy of the d-spacing measurements of the HAp and bone powders could be improved to better than 1% after statistical treatments of the experimental data. By applying a quarter mask, we loaded four different nanoparticles on a single TEM grid, with one section designated for the internal standard.

Structural and Magnetic Properties of the Brownmillerite $Ca_2Al_xFe_{2-x}O_5$ System

  • 김귀야;로권선;여철현
    • Bulletin of the Korean Chemical Society
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    • v.16 no.10
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    • pp.934-938
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    • 1995
  • A series of solid solutions in the Ca2AlxFe2-xO5 (x=0.00, 0.50, 0.66, 1.00 and 1.34) system with brownmillerite structure has been synthesized at 1100 ℃ under an atmospheric air pressure. The solid solutions are analysed by powder x-ray diffraction analysis, Mohr salt titration, thermal analysis, and Mossbauer spectroscopic analysis. The x-ray diffraction analysis assigns the compositions of x=0.00 and 0.50 to the space group Pcmn and those of x=0.66, 1.00, and 1.34 to the Ibm2. Mo&ssbauer spectra have shown the coordination state and disordering of Al3+ and Fe3+ ions. The substituting preference of Al3+ ions for the tetrahedral site decreases with increasing x value. Magnetic susceptibility of the system has been measured in the temperature range of 5 K to 900 K. The solid solutions of the compositions of x=0.00, 0.50 and 0.66 have shown a thermal hysteresis and the thermoremanent magnetization gap decreases with increasing x value in the above systems. However the compositions of x=1.00 and 1.34 do not show the hysteresis. The exchange integral is calculated from Fe3+ ion occupancy ratio. The integral decreases with x value and thus the magnetic transition temperature decreases with the increasing x value.

Short-term Changes of Community Structure of Phytoplankton in Summer Around Namhae Island of Korea (여름철 남해도 연안 식물플랑크톤 군집 구조의 단기 변화)

  • Im, Wol Ae;Gang, Chang Geun;Kim, Suk Yang;Lee, Sam Geun;Kim, Hak Gyun;Jeong, Ik Gyo
    • ALGAE
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    • v.18 no.1
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    • pp.49-58
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    • 2003
  • The short-term dynamics of the summer phytoplankton community structure were investigated in coastal waters around Namhae Island, the Southern Sea of Korea. The study was based on a comprehensive survey constituting 39 collections from 13 stations on July 18-22, August 1-2, 14-16 and 27-30, respectively. The community structure was analysed using cluster analysis and important environmental correlates of the assemblage structure were identified with canonical correspondence analysis (CCA). Water temperature, salinity, NO₂, NO₃, NH₄, PO₄, chlorophyll a and transparency were measured as physico-chemical environmental factors which may be associated with the phytoplankton community structure. Variations of salinity and concentrations of NO₃ and chlorophyll a were not significant. In addition to warmer water temperature, concentrations of NO₂, NO₄and PO₄ decreased at the beginning of August. And transparency was deeper and water column became very unstable after the middle of August. A wide taxonomic diversity was encountered during the survey, including a total of 121 taxa which was composed of 72 diatoms, 48 dinoflagellates and 1 euglenoid species. Cluster analysis showed that the Phytoplankton community could be divided into 4 distinct groups, indicating rapid changes of the community in the short course of this survey. These phytoplankton groups also showed distinctive dispersion patterns in 2-dimensional canonical space, indicating distinct groupings for stations at each survey. Dominant taxa of diatoms (Chaetoceros curvisetus, Chaetoceros spp., Leptocylindrus danicus, Leptocylindrus mediteraneus, Skeletonema costanum, and Pseudo-nitzschia pungen) clustered in region of CCA space corresponding to stations surveyed at the middle of July. Dominant taxa of dinoflagellates were tightly associated with stations surveyed at the middle (Karenia breve) and end (Cochlodinium polykrikoides and Polykrikos schwartzii) of August. The CCA also showed that the phytoplankton community compositions were highly associated with water temperature, transparency, NO₂, NH₄ and PO₄, suggesting that gradients in physical and nutrient conditions affect short-term changes in phytoplankton composition.