• Title/Summary/Keyword: X선 흡수분광분석법

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Preparation of Poly(vinyl acetate)/Silver Hollow Microspheres via Suspension Polymerization (현탁중합에 의한 폴리(비닐 아세테이트)/은 중공 미세입자의 제조)

  • Yeum, Jeong-Hyun
    • Polymer(Korea)
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    • v.35 no.5
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    • pp.390-394
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    • 2011
  • Effects of silver nanoparticles on the polymerization rate and morphology of poly(vinyl acetate) (PVAc)/silver microspheres prepared by suspension polymerization of VAc were investigated. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction and atomic absorption spectrometry were used to characterize the morphology and properties of the PVAc/silver microspheres. Due to the change of hydrophilicity of silver nanoparticles, appearance of the microspheres having golf ball-like convave surfaces was observed. Under controlled concentration of surfactant, PVAc/silver microspheres with various hollow structures were synthesized. In the case of silver nanoparticles modified by surfactant, the polymerization rate increased slightly. PVAc/silver microspheres with a conversion up to 80% were prepared via suspension polymerization.

Mössbauer Study of Tb2Bi1GaxFe5-xO12(x=0, 1) (Tb2Bi1GaxFe5-xO12(x=0, 1)의 뫼스바우어 분광연구)

  • Park, Il-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.18 no.2
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) fabricated by sol-gel and vacuum sealed annealing process. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) have been studied by x-ray diffraction(XRD), vibrating sample magnetometer, and $M\ddot{o}ssbauer$ spectroscopy. The crystal structures were found to be a cubic garnet structure with space group Ia3d. The determined lattice constants $a_0$ of x = 0, and 1 are $12.497\AA$, and $12.465\AA$, respectively. The distribution of gallium and iron in $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ is studied by Rietveld refinement. Based on Rietveld refinement results, the terbium and bismuth ions occupy the 24c site, iron ions occupy the 24d, l6a site, and nonmagmetic gallium ions occupy the 16a site. In order to verify the magnetic site occupancy of iron and gallium, we have taken $M\ddot{o}ssbauer$ spectra for $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) at room temperature. From the results of $M\ddot{o}ssbauer$ spectra analysis, the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 60.8 % and 39.2 %, respectively, and the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 74.7 % and 25.3 %, respectively. It is noticeable that all of the nonmagnetic Ga atoms occupy the 16a site by vacuum annealing process.

Soft X-ray Synchrotron-Radiation Spectroscopy Study of [Co/Pd] Multilayers as a Function of the Pd Sublayer Thickness (Pd층의 두께 변화에 따른 [Co/Pd] 다층박막의 연엑스선 방사광 분광 연구)

  • Kim, D.H.;Lee, Eunsook;Kim, Hyun Woo;Seong, Seungho;Kang, J.-S.;Yang, Seung-Mo;Park, Hae-Soo;Hong, JinPyo
    • Journal of the Korean Magnetics Society
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    • v.26 no.4
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    • pp.124-128
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    • 2016
  • We have investigated the electronic structures of intermetallic multilayer (ML) films of [$Co(2{\AA})/Pd(x{\AA})$] (x: the thickness of the Pd sublayer; x = $1{\AA}$, $3{\AA}$, $5{\AA}$, $7{\AA}$, $9{\AA}$) by employing soft X-ray absorption spectroscopy (XAS) and soft X-ray magnetic circular dichroism (XMCD). Both Co 2p XAS and XMCD spectra are found to be similar to one another, as well as to those of Co metal, providing evidence for the metallic bonding of Co ions in [Co/Pd] ML films. By analyzing the measured Co 2p XMCD spectra, we have determined the orbital magnetic moments and the spin magnetic moments of Co ions in [$Co(2{\AA})/Pd(x{\AA})$] ML films. Based on this analysis, we have found that the orbital magnetic moments are enhanced greatly when x increases from $1{\AA}$ to $3{\AA}$, and then do not change much for $x{\geq}3{\AA}$. This finding suggests that the interface spin-orbit coupling plays an important role in determining the perpendicular magnetic anisotropy in [Co/Pd] ML films.

Chemical and Optical Absorption Spectroscopic Study of Colored Tourmalines (유색 전기석의 화학적 및 광학흡수 분광학적 연구)

  • Kim, Hee-Jong;Kim, Soo-Jin
    • Journal of the Mineralogical Society of Korea
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    • v.6 no.1
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    • pp.1-16
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    • 1993
  • The chemical and optical absorption spectroscopic characters of pink and colorless tourmalines from San Diego mine in California, U.S.A., blue/green tourmalines from anonymous mine, Brazil, and brownis black tourmalines from Uncheon and Haksan mines in Korea have been studied using X-ray diffractometer, electron microprobe, optical absorption spectroscopy, and heat treatment. Least-squares refinements give unit cell diminsions : a = 15.96-16.01 ${\AA}$, c = 7.15-7.16 ${\AA}$ for the brownish black tourmalines, a = 15.82 - 15.87 ${\AA}$, c = 7.09 - 7.10 ${\AA}$ for pink tourmalines, and a = 15.88 - 15.94 ${\AA}$, c = 7.12 - 7.15 ${\AA}$ for blue green tourmalines. The colors of tourmalines are responsible for the transition elements. The pink color is attributed to the $Mn^{3+}$ ions, the blue-green to $Fe^{2+}$ and $Mn^{2+}$, bluish green to $Cu^{2+}$, and the brownish black to $Fe^{2+}$, $Fe^{2+}$ - $Fe^{3+}$, and $Fe^{2+}$ - $Ti^{4+}$. The $Mn^{3+}$ ions of pink color tourmalines are stabilized in the Y sites compressed along the O(1)H-O(3)H axis by Jahn-Teller distortion. Heating removes the pink or red component from tourmalines, producing the colorless stones from the pink and red ones. The bluish green samples change into the greenish blue ones and a certain yellowish green samples change into the light green ones by heat treatment. In the elbaite-schorl series, the concentration of Fe and Mn are variable depending on the color zones. The green zone is characterrized by the high content of Fe and Mn are variable depending on the color zones. The green zone is characterized by the high content of Fe, whereas the pink zone by the high content of Mn. Mn increases in deep yellow zone compared with yellow or colorless zones.

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Crystallization and Magnetic Properties of Iron Doped La-Ba-Mn-O (Fe이 치환된 LaBaMnO계 산화물의 중성자 회절 및 Messbauer분광학연구)

  • Choi, Kang-Ryong;Kim, Sam-Jin;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.14 no.1
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    • pp.38-44
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    • 2004
  • The iron doped colossal magnetoresistance materials with La-Ba-Mn-O perovskites structure have been synthesized by chemical reaction of sol-gel methods. Their crystallographic and magnetic properties have been studied with x-ray diffraction, VSM, RBS, Mossbauer spectroscopy, and magnetoresistance measurements. The crystal structure of the La$\_$0.67/Ba$\_$0.33/Mn$\_$0.99/Fe$\_$0.01/ $O_3$ at room temperature was determined to be orthorhombic of Pnma. The lattice parameters a$\_$0/ and c$\_$0/ increased gradually, but b$\_$0/ deceased with increase of iron substitution. The magnetization and coercivity deceased, also the Curie temperature decreased from 360 K as x increased from 0.00 to 0.05. Magnetoresistence measurements were carried out, and the maximum MR ($\Delta$$\rho$/$\rho$(0)) was observed at 281 K, about 9.5 % in 10 kOe. The temperature of maximum resistance (R$\_$MAX/) decreased with increasing substitution of Fe ions and a semiconductor-metal transition temperature (T$\_$SC-M/) decreased too. This phenomena show that ferromagnetic transition temperature decreased by substituting Fe for Mn ions, it decreases double exchange interaction. This result accords with magnetic structure of neutron diffraction. Mossbauer spectra of La$\_$0.67/Ba$\_$0.33/Mn$\_$0.99/Fe$\_$0.01/ $O_3$were taken at various temperatures ranging from 15 to 350 K. With lowering temperature of the sample, two magnetic phases were increased and finally it showed the two sharp sextets of spectra at 15 K. The isomer shift at all temperature range is about 0.3 mm/s relative to Fe metal, which means that both Fe ions are Fe$\^$3+/ states.Fe$\^$3+/ states.

Study on the screening method for determination of heavy metals in cellular phone for the restrictions on the use of certain hazardous substances (RoHS) (유해물질 규제법(RoHS)에 따른 휴대폰 내의 중금속 함유량 측정을 위한 스크리닝법 연구)

  • Kim, Y.H.;Lee, J.S.;Lim, H.B.
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.1-14
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    • 2010
  • It is of importance that all countries in worldwide, including EU and China, have adopted the Restrictions on the use of certain Hazardous Substances (RoHS) for all electronics. IEC62321 document, which was published by the International Electronics Committee (IEC) can have conflicts with the standards in the market. On the contrary Publicly Accessible Specification (PAS) for sampling published by IEC TC111 can be adopted for complementary application. In this work, we tried to find a route to disassemble and disjoint cellular phone sample, based on PAS and compare the screening methods available in the market. For this work, the cellular phone produced in 2001, before the regulation was born, was chosen for better detection. Although X-ray Fluorescence (XRF) showed excellent performance for screening, fast and easy handling, it can give information on the surface, not the bulk, and have some limitations due to significant matrix interference and lack of variety of standards for quantification. It means that screening with XRF sometimes requires supplementary tool. There are several techniques available in the market of analytical instruments. Laser ablation (LA) ICP-MS, energy dispersive (ED) XRF and scanning electron microscope (SEM)-energy dispersive X-ray (EDX) were demonstrated for screening a cellular phone. For quantitative determination, graphite furnace atomic absorption spectrometry (GF-AAS) was employed. Experimental results for Pb in a battery showed large difference in analytical results in between XRF and GF-AAS, i.e., 0.92% and 5.67%, respectively. In addition, the standard deviation of XRF was extremely large in the range of 23-168%, compared with that in the range of 1.9-92.3% for LA-ICP-MS. In conclusion, GF-AAS was required for quantitative analysis although EDX was used for screening. In this work, it was proved that LA-ICP-MS can be used as a screening method for fast analysis to determine hazardous elements in electrical products.

Comparative Studies on Mechanism of Photocatalytic Degradation of Rhodamine B with Sulfide Catalysts under Visible Light Irradiation (가시광선하에서 황화물계 광촉매를 이용한 로다민 B의 광분해 반응기구에 대한 비교 연구)

  • Lee, Sung Hyun;Jeong, Young Jae;Lee, Jong Min;Kim, Dae Sung;Bae, Eun Ji;Hong, Seong Soo;Lee, Gun Dae
    • Clean Technology
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    • v.25 no.1
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    • pp.46-55
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    • 2019
  • CdS and CdZnS/ZnO materials were prepared using precipitation method and used as photocatalysts for the photocatalytic degradation of rhodamine B (RhB) under visible light irradiation. The prepared photocatalysts were also characterized by XRD and UV-vis DRS. The results indicated that the photocatalysts with intended crystalline structures were successfully obtained and both the CdS and CdZnS/ZnO can absorb visible light as well as UV. The photocatalytic activities were examined with the addition of scavenger for various active chemical species and the difference of reaction mechanisms over the catalysts were discussed. The $CH_3OH$, KI and p-benzoquinone were used as scavengers for ${\cdot}OH$ radical, photogenerated positive hole and ${\cdot}O_2{^-}$ radical, respectively. The CdS and CdZnS/ZnO showed different photocatalytic degradation mechanisms of RhB. It can be postulated that ${\cdot}O_2{^-}$ radical is the main active species for the reaction over CdS photocatalyst, while the photogenerated positive hole for CdZnS/ZnO photocatalyst. As a result, the predominant reaction pathways over CdS and CdZnS/ZnO photocatalysts were found to be the dealkylation of chromophore skeleton and the cleavage of the conjugated chromophore structure, respectively. The above results may be mainly ascribed to the difference of band edge potential of conduction and valence bands in CdS, CdZnS and ZnO semiconductors and the redox potentials for formation of active chemical species.