• Title/Summary/Keyword: X-선 구조분석

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XRR용 두께 표준물질 제작을 위한 박막성장 및 특성평가

  • Yu, Byeong-Yun;Bin, Seok-Min;Kim, Chang-Su;O, Byeong-Seong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.141-141
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    • 2012
  • X-선 반사율 측정법(XRR)은 비파괴적인 측정방법과 수 nm의 두께를 정밀하게 측정할 수 있는 장점으로 인하여 반도체 산업현장에서 많은 관심과 연구가 이루어지고 있다. 이러한 XRR은 두께 분석 측정의 정밀도를 향상시키고 부정확한 결과를 방지하기 위하여 측정기기를 검증하고 보정할 수 있는 두께 표준물질을 필요로 하고 있다. 본 연구에서는 XRR용 두께 표준물질을 이온빔 스퍼터링 증착방법을 이용하여 제작하였다. 두께 표준물질 제작에 있어 공기 중 노출에 의해 산화가 되지 않는 산화물 박막과 산화물 기판을 선택하였다. 후보물질은 glass, sapphire, quartz, SiO2기판과 HfO2, Ta2O5, Cr2O3 산화물 타켓을 이용하여 박막을 제작하였다. 제작된 후 보물질은 교정된 XRR을 통하여 박막의 두께, 계면 및 표면 거칠기, 밀도등 박막의 구조특성분석을 하였다. Glass, quartz의 경우 기판 표면 거칠기가 좋지 않아 제작된 샘플의 X-선 반사율 곡선이 급격히 떨어지면서 측정되는 각도의 영역이 작아졌다. Sapphire로 제작한 시편은 측정된 데이터와 simulation의 curve fitting이 양호하지 않았다. 이 중 SiO2기판을 사용하고 HfO2박막을 증착한 샘플이 다른 후보물질보다 XRR curve fitting 결과가 가장 양호하여 두께 표준물질로 응용하기에 적절하였다. 그리고 AFM (Atomic Force MicroScope)을 이용하여 기판의 거칠기 및 증착한 박막표면 거칠기 측정을 하였고, TEM (Transmission Electron Microscope)으로 두께 측정을 하여 XRR로 얻은 데이터와 비교하였다. 이러한 결과를 토대로 XRR용 두께 표준물질 제작할 수 있었고, 추후 불확도 평가 및 비교실험을 통하여 제작된 XRR용 두께 표준물질을 이용할 수 있을 것으로 기대된다.

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Electrochemical Characteristics of Polyoxometalate/Polypyrrole/Carbon Cloth Electrode Synthesized by Electrochemical Deposition Method (전기화학 증착법에 의해 합성된 폴리옥소메탈레이트/폴리피롤/탄소천 전극의 전기화학적 특성)

  • Yoon, Jo Hee;Choi, Bong Gill
    • Applied Chemistry for Engineering
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    • v.27 no.4
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    • pp.421-426
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    • 2016
  • In this report, polyoxometalte (POM)-doped polypyrrole (Ppy) was deposited on surface of three-dimensional carbon cloth (CC) using an electrodeposition method and its pseudocapacitive behavior was investigated using cyclic voltammetry and galvanostatic charge-discharge. The POM-Ppy coating was thin and conformal which can be controlled by electrodeposition time. As-prepared POM-Ppy/CC was characterized using scanning electron microscope and energy-dispersive X-ray spectroscopy. The unique 3D nanocomposite structure of POM-Ppy/CC was capable of delivering excellent charge storage performances: a high areal capacitance ($561mF/cm^2$), a high rate capability (85%), and a good cycling performance (97% retention).

Nonstoichiometry and Magnetic Properties of the $Eu_{1-x}Sr_xCoO_{3-y}$ System ($Eu_{1-x}Sr_xCoO_{3-y}$계의 비화학량론과 자기적 특성)

  • Ryu, Kwang Hyun;Min, Ji Young;Yo, Chul Hyun
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.508-512
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    • 1995
  • A series of samples in the $Eu_{1-x}Sr_xCoO_{3-y}$ system has been prepared by heating the proper amount of reactant mixture to 1150$^{\circ}C$ under an ambient atmosphere, and the solid solutions are identified by X-ray powder diffraction analysis. The crystal system of samples for the compositions of x=0.00 and 0.25 are found to be orthorhombic whose local symmetry is similiar to the distorted octahedra with orthoferrite type one, whereas those of x=0.50 and 0.75 to be the cubic system, and that of x=1.00 to the orthorhombic similiar to be the brownmillerite type. The amount of $Co^{4+}$ ion (${\tau}$ value) is maximized at the composition of x=0.50, and the oxygen vacancies increase with the x value. The nonstoichiometric chemical formula of each compound could be determined from the mole ratio of $Co^{4+}$ ion and oxygen vacancies. The $Co^{3+}$ ion located in octahedral site has spin transition from low spin to high spin states with increasing temperature. Therefore, the effective magnetic moment of each samples obtained from the magnetic measurement is increased with the increasing temperature. The $EuCoO_{3.00}$ has strong antiferromagnetic interaction between the neighboring $Co^{3+}$ ions through the intermediate oxygen ions. With the increasing ${\tau}$ value, the absolute {\theta}_p$ value is decreased by the ferromagnetic interaction of $Co^{3+}-O^2-Co^{4+}$ and thus the {\theta}_p$ has positive value at x=0.50.

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Study of Iodide Adsorption on Organobentonite using X-ray Absorption Spectroscopy (X-선 흡수분광기를 이용한 유기벤토나이트의 요오드 흡착연구)

  • Yoon, Ji-Hae;Ha, Ju-Young;Hwang, Jin-Yeon;Hwang, Byoung-Hoon;Gordon E. Brown, Jr.
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.1
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    • pp.23-34
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    • 2009
  • The adsorption of iodide on untreated bentonite and bentonites modified with organic cation (i.e., hexadecylpyridinium chloride monohydrate ($HDP^+$)) was investigated, and the organobentonites were characterized using uptake measurements, ${\mu}$-XRD, and electrophoretic mobilities measurement. Uptake measurements indicate that bentonite has a high affinity for $HDP^+$. Our ${\mu}$-XRD study indicates that organobentonites significantly expanded in basal spacing and organic cations were substantially intercalated into the interlayer spaces of bentonite. The electrophoretic mobility indicates that organobentonite tht is modified with organic cations in excess of the CEC of bentonite is completely different from untreated bentonite in the surface charge distribution. We found significant differences in adsorption capacities of iodide depending on the bentonite properties as follows: iodide adsorption capacities were 439 mmol/kg for the bentonite modified with $HDP^+$ at an equivalent amount corresponding to 200% of the CEC of bentonite whereas no adsorption of iodide was observed for the untreated bentonite. The molecular environments of iodine adsorbed on organobentonites were further studied using I K-edge and $L_{III}$-edge x-ray absorption spectroscopy (XAS). The X-ray absorption near-edge structure (XANES) of iodine spectra from organobentonites was similar to that of KI reference solution. Linear combination fitting of EXAFS data suggests the fraction of iodine reacted with the organic compound increased with increasing loading of the organic compound on organobentonites. In this study, we observed significant differences in the adsorption environments of iodide depending on the modified property of bentonite and suggest that an organobentonite has potential as reactive barrier material around a nuclear waste repository containing anionic radioactive iodide.

Stable Defect Structure of La2O3-Modified BaTiO3 (La$_2O_3$-변형 BaTi$O_3$의 안정한 결함구조)

  • Kim, Jeong Su;Park, Hyu Beom;An, Tae Ho;Kim, Si Jung
    • Journal of the Korean Chemical Society
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    • v.38 no.4
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    • pp.309-318
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    • 1994
  • The stable defect structure and the single phase region of La$_2O_3$-modified BaTi$O_3$ have been studied by X-ray diffractometer and scanning electron microscope. The stable defect structure of La$_2O_3$-modified BaTi$O_3$ has been identified as [($Ba^x_{Ba})_{1-2x}(La{\cdot}_{Ba})_{2x}][Ti^x_{Ti})_{1-x/2}(V""_{Ti})_{x/2}]O_3$ which consists of La$^{3+}$ ion substitution for Ba$^{3+}$ ion in the lattice structure and the formation of Ti vacancies for the charge compensation. When 3 mol% of La$_2O_3{\cdot}3/2TiO_3$ was added to BaTi$O_3$, the unit cell structure was transformed from tetragonal to cubic and the solubility limit was about 14 mol%. When La$_2O_3{\cdot}3/2TiO_2$ was added above this solubility limit, the second phase, La$_4Ba_2Ti_5O_{18}$, was formed. In the La$_2O_3$-modified BaTi$O_3$, it was found by the liquid phase sintering process that the sinterability was decreased by excess BaO but increased by excess Ti$O_2$.

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Structural and thermal analysis of electrochemically Li intercalated synthetic graphite (전기 화학적으로 리튬이 층간 삽입된 인조흑연의 구조와 열적 특성 분석)

  • Oh, Won-Chun
    • Analytical Science and Technology
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    • v.14 no.3
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    • pp.197-202
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    • 2001
  • The characteristics of the electrochemically Li intercalated synthetic graphite were determined from the studies with XRD method, DSC and solid $^7Li-NMR$ spectrophotometric analysis. From the results of X-ray diffraction method, it was found that the compounds in the stage 1 structure were predominantly formed. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From these results, it was found that exothermic and endothermic reactions of lithium intercalated into synthetic graphite are related to thermal stability of lithium ion between carbon graphene layers. From the $^7Li-NMR$ data, scientific observation found that bands are shift toward higher frequencies with increasing lithium concentration because non-occupied electron shells of Li increased in charge carrier density. Line widths of the Li intercalated synthetic graphite compounds decreased slowly because of non-homogeneous local magnetic order and the random electron spin direction for substituted Li.

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The Analysis of Energy Character and Synthesis of Lithium-Carbon Intercalation Compounds (리튬-탄소층간화합물의 합성과 에너지 특성의 분석)

  • 오원춘;백대진;고영신
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.3 no.2
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    • pp.167-175
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    • 1993
  • Lithium-Carbon Intercalation Compounds(Li-CICs) have been synthesized from various carbon ma-terials by use of the modified stainless steel two-bulbs methods. These compounds had various colours by structural character of starting materials. The synthesized Li-CICs were identified to stage formation process by X-ray diffraction data. At these results, well-oriented natural graphite and graphite fiber are formed lower stages(Stage 1, Stage 2), but poor-oriented carbon fiber and petroleum cokes are also formed higher stages(Stage 3, Stage 4, Stage 5). And when we compared with measured d value and calculated d value, these values agreed with each other. But poor-oriented carbon materials are some difference from them. The stage stability and energy stage of Li-CICs were obtained by UV/VIS Spectrophotometric data. X-ray diffraction and UV/VIS Spectrophotometric data suggested that well-oriented carbon materials has distingushible curve between energy and reflectance. In these results, we know that many charge carriers between carbon layers are related to concentration of intercalants. And then, this paper also provides information on high efficiency energy storing materials at intercalation process of Li-CICs.

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The Jahn-Teller Effect in the Iron Copper Spinel $CuFe_{2}O_{4}$ (철, 구리 스피넬 $CuFe_{2}O_{4}$의 Jahn-Teller 효과에 관한 연구)

  • 서정철;이민용
    • Journal of the Korean Magnetics Society
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    • v.5 no.2
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    • pp.123-127
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    • 1995
  • $CuFe_{2}O_{4}$ was accomplished by chemical rrethod and the crystallographic and magnetic properties have been studied by $M\"{o}ssbauer$ spectroscopy and X-ray diffraction. The slowly cooled sample is found to have a tetragonal spinel structure with the lattice constant $a=8.26{\pm}0.05{\AA},\;c=8.75{{\pm}}0.05{\AA}$. The $M\"{o}ssbauer$ spectra between the room temperature to the Curie temperature show that the $Cu_{2+}$ ions at octahedral site have the Jahn-Teller effect and the sample exhibits a structural phase transition near 630K due to the Jahn-Teller effect. The Curie temperature is found to be 690K and it is lower than that of ceramic method.

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RF 마그네트론 스퍼터링 방법으로 증착된 CdS박막의 기판 온도와 열처리 온도 변화에 따른 구조적 및 광학적 특성

  • Im, Jeong-U;Kim, Myeong-Seop;Yu, Jae-Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.399-399
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    • 2012
  • II-V 족 화합물 반도체인 황화카드뮴(CdS)은 상온에서 2.42 eV의 밴드갭을 갖는 직접 천이형 물질로서 CdTe 또는 $CuInSe_2$와 같은 박막형 태양전지의 투과층(window layer)으로 널리 사용되고 있다. CdS 박막은 전자빔 증착법(e-beam evaporation), 화학용액증착법(chemical bath deposition), 열분해법(spray pyrolysis), 스퍼터링법(sputtering) 등으로 제작되고 있다. 이 중 스퍼터링법의 경우, 다른 증착법에 비해 조작이 간단하고 넓은 면적에서 균일한 박막을 증착할 수 있을 뿐만 아니라, 박막두께 조절이 용이하다. 따라서 본 실험에서는 RF 마그네트론 스퍼터링법으로 증착된 CdS 박막의 기판온도 및 열처리 온도변화에 따른 구조적 및 광학적 특성을 조사하였다. 기판은 RCA 기법으로 세정된 Corning Eagle 2000 유리 기판을 사용하였다. 박막 공정은 초기 진공 $1{\times}10^{-6}Torr$ 상태에서 20 sccm의 Ar 가스를 주입하고 100 W의 RF 파워, 7 mTorr의 공정 압력에서 기판 온도를 $200^{\circ}C$부터 $500^{\circ}C$까지 변화시키면서 수행하였다. 증착된 CdS 박막은 질소 분위기의 가열로(furnace)를 이용해 $300-500^{\circ}C$ 온도에서 30분간 열처리되었다. 시료들의 표면 형상은 scanning electron microscope를 사용하여 관찰하였으며, UV-vis-NIR spectrophotometer를 사용하여 400-1,000 nm 파장영역에서의 투과율을 측정하였다. 그리고 X-선 회절분석(X-Ray Diffraction)으로 결정구조를 조사하고 결정립 크기를 산출하였다.

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A Study on $Ni_{0.8}Cd_{0.2}Fe_2O_4$ by Mossbauer spectroscopy (Mossbauer 분광법을 이용한 $Ni_{0.8}Cd_{0.2}Fe_2O_4$)

  • Baek, Seung-Do
    • Korean Journal of Materials Research
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    • v.6 no.11
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    • pp.1107-1112
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    • 1996
  • Ni를 Cd로 대치시켜 세라믹 소결법으로 합성한 Ni0.8Cd0.2Fe2O4 의 X-ray 회절선을 측정하여 구조를 확인하고, 형성된 결정체의 격자 상수를 조사하였다. 이 시료의 Mossbauer 스펙트럼을 80K-900K의 온도 영역에서 측정 분석하여 Mossbauer parameter의 온도 의존성과 Fe 이온에 대한 자료를 얻고, 이 자료를 토대로 Ni0.8Cd0.2Fe2O4 의 자기 전이 현상과 Curied 온도 Tc와 격자 비열 및 Debye 온도와 같은 물성을 조사하였다.

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