• 제목/요약/키워드: X-ray Structure Analysis

검색결과 1,128건 처리시간 0.023초

Cyanide-Bridged CrIIIMnII Binuclear Complexes Based on [Mn(phen)2]2+ and Dicyanidechromate(III) Building Blocks: Syntheses, Crystal Structures, and Magnetic Properties

  • Li, Guo-Ling;Zhang, Li-Fang;Ni, Zhong-Hai;Kou, Hui-Zhong;Cui, Ai-Li
    • Bulletin of the Korean Chemical Society
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    • 제33권5호
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    • pp.1675-1680
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    • 2012
  • Three new cyanide-bridged $Cr^{III}Mn^{II}$ binuclear complexes, $[Mn(phen)_2Cl][Cr(bpmb)(CN)_2]{\cdot}H_2O$ ($\mathbf{1}$) (phen = 1,10-phenanthroline, $bpdmb^{2-}$ = 1,2-bis(pyridine-2-carboxamido)-4-methyl-benzenate), $[Mn(phen)_2Cl][Cr(bpmb)-(CN)_2]{\cdot}H_2O$ ($\mathbf{2}$) ($bpdmb^{2-}$ = 1,2-bis(pyridine-2-carboxamido)-4,5-dimethyl-benzenate), and $[Mn(phen)_2Cl]-[Cr(bpClb)(CN)_2]{\cdot}CH_3OH{\cdot}H_2O$ ($\mathbf{3}$) ($bpClb^{2-}$ = 1,2-bis(pyridine-2-carboxamido)-4-chloro-benzenate) were obtained based on $Mn(phen)_2Cl_2$ and a series of dicyanidechromate(III) building blocks. Single crystal X-ray diffraction analysis shows the structures of the three complexes are dimeric type with two different metal centers linked by a cyanide group from corresponding dicyanidechromate(III) building block. Magnetic investigations indicate the existence of relatively weak antiferromagnetic coupling between Cr(III) and Mn(II) ions with best-fit constants $J_{CrMn}=-2.78(5)cm^{-1}$ for $\mathbf{1}$, $J_{CrMn}=-3.02(2)cm^{-1}$ for $\mathbf{2}$ and $J_{CrMn}=-2.27(3)cm^{-1}$ for $\mathbf{3}$ based on the spin exchange Hamiltonian = $-2J_{CrMn}\hat{S}_{Cr}\hat{S}_{Mn}$. The magneto-structural correlation of cyanide-bridged $Cr^{III}Mn^{II}$ complexes has been discussed at last.

Synthesis and Characterization of Y2O3 Powders by a Modified Solvothermal Process

  • Jeong, Kwang-Jin;Bae, Dong-Sik
    • 한국재료학회지
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    • 제22권2호
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    • pp.78-81
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    • 2012
  • $Y_2O_3$ nanomaterials have been widely used in transparent ceramics and luminescent devices. Recently, many studies have focused on controlling the size and morphology of $Y_2O_3$ in order to obtain better material performance. $Y_2O_3$ powders were prepared under a modified solvothermal condition involving precipitation from metal nitrates with aqueous ammonium hydroxide. The powders were obtained at temperatures at $250^{\circ}C$ after a 6h process. The properties of the $Y_2O_3$ powders were studied as a function of the solvent ratio. The synthesis of $Y_2O_3$ crystalline particles is possible under a modified solvothermal condition in a water/ethylene glycol solution. Solvothermal processing condition parameters including the pH, reaction temperature and solvent ratio, have significant effects on the formation, phase component, morphology and particle size of yttria powders. Ethylene glycol is a versatile, widely used, inexpensive, and safe capping organic molecule for uniform nanoparticles besides as a solvent. The characterization of the synthesized Y2O3 powders were studied by XRD, SEM (FE-SEM) and TG/DSC. An X-ray diffraction analysis of the synthesized powders indicated the formation of the $Y_2O_3$ cubic structure upon calcination. The average crystalline sizes and distribution of the synthesized $Y_2O_3$ powders was less than 2 um and broad, respectively. The synthesized particles were spherical and hexagonal in shape. The morphology of the synthesized powders changed with the water and ethylene glycol ratio. The average size and shape of the synthesized particles could be controlled by adjusting the solvent ratio.

Dry Etching of $Al_2O_3$ Thin Film in Inductively Coupled Plasma

  • Xue, Yang;Um, Doo-Seung;Kim, Chang-Il
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2009년도 추계학술대회 논문집
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    • pp.67-67
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    • 2009
  • Due to the scaling down of the dielectrics thickness, the leakage currents arising from electron tunneling through the dielectrics has become the major technical barrier. Thus, much works has focused on the development of high k dielectrics in both cases of memories and CMOS fields. Among the high-k materials, $Al_2O_3$ considered as good candidate has been attracting much attentions, which own some good properties as high dielectric constant k value (~9), a high bandgap (~2eV) and elevated crystallization temperature, etc. Due to the easy control of ion energy and flux, low ownership and simple structure of the inductively coupled plasma (ICP), we chose it for high-density plasma in our study. And the $BCl_3$ was included in the gas due to the effective extraction of oxygen in the form of BClxOy compound. In this study, the etch characteristic of ALD deposited $Al_2O_3$ thin film was investigated in $BCl_3/N_2$ plasma. The experiment were performed by comparing etch rates and selectivity of $Al_2O_3$ over $SiO_2$ as functions of the input plasma parameters such as gas mixing ratio, DC-bias voltage and RF power and process pressure. The maximum etch rate was obtained under 15 mTorr process perssure, 700 W RF power, $BCl_3$(6 sccm)/$N_2$(14 sccm) plasma, and the highest etch selectivity was 1.9. We used the x-ray photoelectron spectroscopy (XPS) to investigate the chemical reactions on the etched surface. The Auger electron spectroscopy (AES) was used for elemental analysis of etched surface.

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Raney Ni-Zn-Fe 전극의 산소발생 반응 특성에 미치는 도금변수의 영향 (Effect of Electroplating Parameters on Oxygen Evolution Reaction Characteristics of Raney Ni-Zn-Fe Electrode)

  • 채재병;김종원;배기광;박주식;정성욱;정광진;김영호;강경수
    • 한국수소및신에너지학회논문집
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    • 제31권1호
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    • pp.23-32
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    • 2020
  • The intermittent characteristics of renewable energy complicates the process of balancing supply with demand. Electrolysis technology can provide flexibility to grid management by converting electricity to hydrogen. Alkaline electrolysis has been recognized as established technology and utilized in industry for over 100 years. However, high overpotential of oxygen evolution reaction in alkaline water electrolysis reduces the overall efficiency and therefore requires the development of anode catalyst. In this study, Raney Ni-Zn-Fe electrode was prepared by electroplating and the electrode characteristics was studied by varying electroplating parameters like electrodeposition time, current density and substrate. The prepared Raney Ni-Zn-Fe electrode was electrochemically evaluated using linear sweep voltammetry. Physical and chemical analysis were conducted by scanning electron microscope, energy dispersive spectrometer, and X-ray diffraction. The plating time did not changed the morphology and composition of the electrode surface and showed a little effect on overpotential reduction. As the plating current density increased, Fe content on the surface increased and cauliflower-like structure appeared on the electrode surface. In particular, the overpotential of the electrode, which was prepared at the plating current density of 320 mA/㎠, has showed the lowest value of 268 mV at 50 mA/㎠. There was no distinguishable overpotential difference between the type of substrate for the electrodes prepared at 80 mA/㎠.

우럭 껍질 젤라틴 복합필름의 특성 (Characterization of Rockfish Skin Gelatin Composite Films)

  • 백송이;김혜리;송경빈
    • 한국식품영양과학회지
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    • 제46권3호
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    • pp.394-399
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    • 2017
  • 플라스틱 포장 폐기물로 인한 환경오염을 해결하기 위한 대안으로 생분해성 필름이 많이 연구되어 왔다. 본 연구에서는 우럭 껍질 젤라틴(RFG)과 nano-clay(Cloisite $Na^+$, 10A)의 복합필름의 특성에 관하여 연구하였다. 우럭 껍질로부터 젤라틴을 추출하여 sorbitol을 가소제로서 첨가한 단백질 필름을 제조하였고, 제조된 RFG 필름의 tensile strength(TS), water vapor permeability(WVP), water solubility(WS)는 각각 15.0 MPa, $2.70{\times}10^{-9}g\;m/m^2\;s\;Pa$, 53.8%였다. RFG에 nano-clay를 첨가한 복합필름은 TS가 증가하고 WVP와 WS는 감소하였다. XRD 분석과 SEM 측정 결과를 통하여 RFG/nano-clay 복합필름 내부에 박리형 구조를 형성함을 확인할 수 있었다. 결론적으로 본 연구 결과 RFG/nano-clay 복합필름은 생분해성 포장재로 적용될 수 있음을 시사한다.

A safe and cost-effective PMMA carbon source for MgB2

  • Ranot, Mahipal;Jang, S.H.;Shinde, K.P.;Sinha, B.B.;Bhardwaj, A.;Oh, Y.S.;Kang, S.H.;Chung, K.C.
    • 한국초전도ㆍ저온공학회논문지
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    • 제19권1호
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    • pp.47-50
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    • 2017
  • Carbon is proven to be very effective in pinning the magnetic vortices and improving the superconducting performance of $MgB_2$ at high fields. In this work, we have used polymethyl methacrylate (PMMA) polymer as a safe and cost effective carbon source. The effects of molecular weight of PMMA on crystal structure, microstructure as well as on superconducting properties of $MgB_2$ were studied. X-ray diffraction analysis revealed that there is a noticeable shift in (100) and (110) Bragg reflections towards higher angles, while no shift was observed in (002) reflections for $MgB_2$ doped with different molecular weights of PMMA. This indicates that carbon could be substituted in the boron honeycomb layers without affecting the interlayer interactions. As compared to undoped $MgB_2$, substantial enhancement in $J_c(H)$ properties was obtained for PMMA-doped $MgB_2$ samples both at 5 K and 20 K. The enhancement could be attributed to the effective carbon substitution for boron and the refinement of crystallite size by PMMA doping.

유도 열플라즈마를 이용한 카본나노시트 합성 (Synthesis of carbon nanosheets using RF thermal plasma)

  • 이승용;고상민;구상만;황광택;한규성;김진호
    • 한국결정성장학회지
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    • 제24권5호
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    • pp.207-212
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    • 2014
  • 2차원 흑연구조를 갖는 카본나노시트는 큰 비표면적과 우수한 전기적, 화학적 및 기계적 물성으로 인하여 미래소재로 각광받고 있다. 경제적이고 쉬운 카본나노시트의 양산공정개발을 위해 본 연구에서는 메테인($CH_4$)과 프로페인($C_3H_8$) 가스를 이용한 유도 열플라즈마 공정을 통해 기상 합성하여 카본나노시트 분말을 합성하였다. 유도 열플라즈마를 이용한 카본나노시트 합성은 촉매나 증착공정 없이 진행되었으며, 합성된 카본나노시트의 물성을 TEM, Raman, XRD, BET로 분석하였다. 메테인과 프로페인으로부터 합성된 카본 나노시트는 각각 5~6개의 그래핀 층과 15~16개의 그래핀 층으로 이루어진 분말로 합성되었으며 분말의 크기는 약 100 nm임을 확인할 수 있었다.

증착온도를 달리하여 제조한 Zn0.8Co0.2O 박막의 미세조직 및 자기 특성 (Microstructure and Magnetic Properties of Pulsed DC Magnetron Sputtered Zn0.8Co0.2O Film Deposited at Various Substrate Temperatures)

  • 강영훈;김봉석;태원필;김기출;서수정;박태석;김용성
    • 한국세라믹학회지
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    • 제43권2호
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    • pp.79-84
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    • 2006
  • We studied the microstructure and magnetic property of the pulsed DC magnetron sputtered $Zn_{\0.8}Co_{0.2}O$ film as a function of substrate temperatures. The X-ray patterns of the $Zn_{\0.8}Co_{0.2}O$ film showed a strong (002) preferential orientation at $500^{\circ}C$. The films with a crystallite size of 23-35 nm were grown in the form of nano-sized structure and this tendency was remarkable with increasing substrate temperature. The UV-visible result showed that the $Zn_{\0.8}Co_{0.2}O$ film prepared above $300^{\circ}C$ has a high optical transmittance of over $80\%$ in the visible region. The absorption bands were observed due to sp-d interchange action by $Co^{2+}$ complex ion and dd transition in the region from 500 to 700nm. The resistivity of the film was below $10^{-1}\;\Omega-cm\;above\;300^{\circ}C$. The AGM analysis results for the all films showed the magnetic hysteresis curves of ferromagnetic nature. The low electrical resistivity and room temperature ferromagnetism of ZnCoO thin films 'deposited above $300^{\circ}C$ suggested the possibility for the application to Diluted Magnetic Semiconductors (DMSs).

이온교환수지 촉매를 이용한 옥탄가 향상제인 TAME 합성반응의 연구 (A Study over Catalytic Behavior Octane Enhancer, TAME Synthesis with Ion Exchange Resin Catalysts)

  • 박진화
    • 공업화학
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    • 제7권5호
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    • pp.832-842
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    • 1996
  • 성질이 서로 다른 그물 구조형 이온교환수지인 Amberlyst-15, Amberlyst-15(wet)와 Amberlyst XN-1010을 가지고 고정층 상압 유통식 반응장치에서 옥탄가 향상제인 TAME 합성반응을 행하였다. Amberlyst-15가 Amberlyst-15(wet)와 Amberlyst XN-1010에 비해 활성이 좋았는데 그 이유는 겔형 미세입자 내부 활성점의 반응참여 정도가 크기 때문으로 생각되며, TAME 합성반응의 최적 조건들은, 반응온도=$135^{\circ}C$, 반응물 몰비(MeOH/I.A.A.)=1.0~4.0, W/F=2.0~4.0 gr.-cat. hr/gr.-mole일 때이었다. X-ray 회절 분석결과 $2{\theta}=20$에서 styrene divinyl benzene이 가교결합을 나타냈으며, DSC 분석결과 열적 안정성의 순서로는 Amberlyst-15, Amberlyst-15(wet) 및 Amberlyst XN-1010이였다. 본 실험에서 구한 TAME 합성의 겉보기 활성화 에너지 값은 Amberlyst-15:Ea=12.36 kcal/mole, Amberlyst-15(wet):Ea=12.46 kcal/mole 및 Amberlyst XN-1010:Ea=14.72 kcal/mole이였다.

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건축용 내화 재료로서의 포비성 알칼리 규산염의 특성에 관한 연구 (Properties of Intumescence Alkali Silicates for Building Fire-Resistant)

  • 강현주;강승민;송명신;김영식;박종헌
    • 공업화학
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    • 제20권4호
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    • pp.416-422
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    • 2009
  • 강구조 건축물은 화재시 화염을 차단하기 위한 목적으로 내화재료를 사용하고 있다. 일반적으로 모든 건축 구조용 재료는 시간이 경과할수록 초기의 성능이 열화되기 때문에 이들의 유지관리가 필요하다. 내화 피복재는 건축물의 화재에 대한 내구성능은 내화피복재에 의존하기 때문에 건축물에서 매우 중요한 재료라 할 수 있다. 본 연구에서는 내화피복재로서의 알칼리 규산염의 합성 및 합성한 알칼리 규산염의 물성에 대해 연구하였는데, 알칼리 규산염의 종류로는 potassium silicate, sodium silicate, lithium silicate으로 하였으며, 기본적으로 몰 비율의 변화를 주어 합성하였다. 합성한 알칼리 규산염의 내화특성을 확인하기 위하여 용해도 포비도, 열 분석, 결정학적 분석, 차열성능 및 차염성능에 대해 시험하였다. 연구결과, 합성한 알칼리 규산염의 용해도, 포비도는 칼륨 실리케이트, 소디움 실리케이트, 리튬실리케이트의 순서로 나타났으며, 열분석에 의한 무게 손실은 소디움 실리케이트와 리튬 실리케이트가 칼륨 실리케이트 보다 큰 것으로 나타났다. 또한 화재 시 가장 중요한 차열성능과 차염성능에 대해KS 기준을 만족하는 것은 소디움 실리케이트 3.3 몰 배합으로 나타났는데, 내화피복재로서 우수한 성능을 발휘하였다.