• 제목/요약/키워드: In situ X-ray diffraction

검색결과 136건 처리시간 0.027초

Structural Evolution of Layered $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ upon Electrochemical Cycling in a Li Rechargeable Battery

  • 홍지현;서동화;김성욱;권혁조;박영욱;강기석
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2010년도 춘계학술발표대회
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    • pp.37.2-37.2
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    • 2010
  • Recently $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ has been consistently examined and investigated by scientists because of its high lithium storage capacity, which exceeds beyond the conventional theoretical capacity based on conventional chemical concepts. Consequently, $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ is considered as one of the most promising cathode candidates for next generation in Li rechargeable batteries. Yet the mechanism and the origin of the overcapacity have not been clarified. Previously, many authors have demonstrated simultaneous oxygen evolution during the first delithiation. However, it may only explain the high capacity of the first charge process, and not of the subsequent cycles. In this work, we report a clarified interpretation of the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$, which is the key element in understanding its anomalously high capacity. We identify how the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ occurs upon the electrochemical cycling through careful study of electrochemical profiles, ex-situ X-ray diffraction (XRD), HR-TEM, Raman spectroscopy, and first principles calculation. Moreover, we successfully separated the structural change at subsequent cycles (mainly cation rearrangement) from the first charge process (mainly oxygen evolution with Li extraction) by intentionally synthesizing sample with large particle size. Consequently, the intermediate states of structural evolution could be well resolved. All observations made through various tools lead to the result that spinel-like cation arrangement and lithium environment are created and embedded in layered framework during repeated electrochemical cycling.

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$CeO_2$의 상전이에 따른 YBCO 박막의 결정성 및 특성의 변화 (Change of crystallization and properties of YBCO thin film by phase transition of $CeO_2$)

  • 김성민;이상렬
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 1999년도 하계학술대회 논문집 D
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    • pp.1590-1592
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    • 1999
  • We have fabricated good quality superconducting $YBa_2Cu_3O_{7-{\delta}}$ thin films on Hastelloy(Ni-Cr-Mo alloys) with $CeO_2$ buffer layers by in-situ pulsed laser deposition in a multi-target processing chamber. Using one of electrical properties of YBCO superconducting which the resistance approaches to zero dramatically on transition temperature, we have researched to make power transmission line, we have deposited YBCO thin film on flexible metallic substrate. However, it is difficult to make films on flexible metallic substrates due to both interdiffusion problem between metallic substrate and superconducting layer and non-crystallization of YBCO on amorphous substrate. From early research, two ways-using textured metallic substrate and buffer layer-were proposed to overcome theses difficulties. We have chosen $CeO_2$ as a buffer layer which has cubic structure of $5.41{\AA}$ lattice parameter and only 0.2% of lattice mismatch with $3.82{\AA}$ of a-axis lattice parameter of YBCO on (110) direction of $CeO_2$. In order to enhance the crystallization of YBCO films on metallic substrates we deposited $CeO_2$ buffer layers at varying temperature $700^{\circ}C$ to $800^{\circ}C$ and $O_2$ pressure. By X-ray diffraction, we found that each domination of (200) and (111) orientations were strongly relied upon the deposition temperature in $CeO_2$ layer and the change of the domination of orientation affects the crystallization of YBCO upper layer.

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Optical sensitivity of DNA-dispersed single-walled carbon nanotubes within cement composites under mechanical load

  • Kim, Jin Hee;Rhee, Inkyu;Jung, Yong Chae;Ha, Sumin;Kim, Yoong Ahm
    • Carbon letters
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    • 제24권
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    • pp.90-96
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    • 2017
  • We demonstrated the sensitivity of optically active single-walled carbon nanotubes (SWCNTs) with a diameter below 1 nm that were homogeneously dispersed in cement composites under a mechanical load. Deoxyribonucleic acid (DNA) was selected as the dispersing agent to achieve a homogeneous dispersion of SWCNTs in an aqueous solution, and the dispersion state of the SWCNTs were characterized using various optical tools. It was found that the addition of a large amount of DNA prohibited the structural evolution of calcium hydroxide and calcium silicate hydrate. Based on the in-situ Raman and X-ray diffraction studies, it was evident that hydrophilic functional groups within the DNA strongly retarded the hydration reaction. The optimum amount of DNA with respect to the cement was found to be 0.05 wt%. The strong Raman signals coming from the SWCNTs entrapped in the cement composites enabled us to understand their dispersion state within the cement as well as their interfacial interaction. The G and G' bands of the SWCNTs sensitively varied under mechanical compression. Our results indicate that an extremely small amount of SWCNTs can be used as an optical strain sensor if they are homogeneously dispersed within cement composites.

Mechanical Behavior of Directionally Solicified (Y2O3)ZrO2/Al2O3 Eurtctic Fibers

  • Park, Deok-Yong;Yang, Jenn-Ming
    • 한국세라믹학회지
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    • 제41권1호
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    • pp.1-8
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    • 2004
  • The microstructural features and mechanical behavior of directionally solidified $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fibers after extended beat treatment in oxidizing environment were investigated. The fiber was grown continuously by an Edge-defined Film-fed Growth (EFG) technique. The microstructure was characterized using X-Ray Diffraction (XRD) and Scanning Electron Microscopy(SEM). The microstructure of the fiber in the as-fabricated state consists of highly oriented colonv and fine lamellar microstructure along the fiber axis. Tensile strength of the $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fiber remained unchanged with heat treatment at temperatures between $1200^{\circ}C$ and $1500^{\circ}C$ up to 300h. The weibulls modulus remained fairly constant after extended thermal exposure. The fracture toughness and crack propagation behavior were investigated. The fracture toughness ($K_{1C}$) of the $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fiber in the as-fabricated state were measured to be 3.6 ${\pm}$ 0.5 MPa${\cdot}m^{1/2}$ by an indentation technique and 2.2 ${\pm}$ 0.2 MPa${\cdot}m^{1/2}$ by assuming elliptical flaw of a semi-infinite solid, respectively. The $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fiber showed a radial (Palmqvist) crack type and exhibited an orthotropic crack growth behavior under 100 g load.

고온-고압하에서 티탄철석에 대한 상면이 연구 (Phase Transition Study on Ilmenite under High Pressure and Temperature)

  • Kim, Young-Ho
    • 한국광물학회지
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    • 제15권3호
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    • pp.161-169
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    • 2002
  • 고온-고압 상태에서 티탄철석 ($FeTiO_3$)의 상변이에 대한 연구가 있었으나, 그 결과는 서로 일치하지 않고 있다. 특히, 티탄철석상과 페롭스카이트상의 상변이 경계는 담금방법에 의해 결정된 것으로 신뢰도에 의문이 제기되고 있다. 이러한 문제를 해결하기 위해, 고온-고압 현장상태에서 라지 볼륨 기기와 방사광을 이용하여 19 GPa와 $700^{\circ}C$의 범위에서 X선 회절실험을 시행하였다. 이러한 실험결과, 페롭스카이트상은 상온에서 16 CPa 이상의 압력에서 안정하며, 15 CPa 근처에서 $LiNbO_3$상으로 변이한다. 또한 이 두 고온-고압상은 $500^{\circ}C$에서는 순간적인 상변이를 하고 있다. $LiNbO_3$상은 각각 13 CPa 및 300'E와 10.8 GPa 및 400'E에서 티탄철석상으로 상변이 한다. 따라서 본 실험결과는 $LiNbO_3$상은 고온-고압하에서 안정 영역을 확보하고 있으며, 페롭스카이트-티탄철석상경계는 이전에 발표된 결과와는 매우 다르다는 것을 지시해주고 있다.

A Deep Investigation of the Thermal Decomposition Process of Supported Silver Catalysts

  • Jiang, Jun;Xu, Tianhao;Li, Yaping;Lei, Xiaodong;Zhang, Hui;Evans, D.G.;Sun, Xiaoming;Duan, Xue
    • Bulletin of the Korean Chemical Society
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    • 제35권6호
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    • pp.1832-1836
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    • 2014
  • A deep understanding of the metallic silver catalysts formation process on oxide support and the formation mechanism is of great scientific and practical meaning for exploring better catalyst preparing procedures. Herein the thermal decomposition process of supported silver catalyst with silver oxalate as the silver precursor in the presence of ethylenediamine and ethanolamine is carefully investigated by employing a variety of characterization techniques including thermal analysis, in situ diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, and X-ray diffraction. The formation mechanism of supported silver particles was revealed. Results showed that formation of metallic silver begins at about $100^{\circ}C$ and activation process is essentially complete below $145^{\circ}C$. Formation of silver was accompanied by decomposition of oxalate group and removal of organic amines. Catalytic performance tests using the epoxidation of ethylene as a probe reaction showed that rapid activation (for 5 minutes) at a relatively low temperature ($170^{\circ}C$) afforded materials with optimum catalytic performance, since higher activation temperatures and/or longer activation times resulted in sintering of the silver particles.

Analysis of Photoluminescence for N-doped and undoped p-type ZnO Thin Films Fabricated by RF Magnetron Sputtering Method

  • Liu, Yan-Yan;Jin, Hu-Jie;Park, Choon-Bae;Hoang, Geun C.
    • Transactions on Electrical and Electronic Materials
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    • 제10권1호
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    • pp.24-27
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    • 2009
  • N-doped ZnO thin films were deposited on n-type Si(100) and homo-buffer layer, and undoped ZnO thin film was also deposited on homo-buffer layer by RF magnetron sputtering method. After deposition, all films were in-situ annealed at $800^{\circ}C$ for 5 minutes in ambient of $O_2$ with pressure of 10Torr. X -ray diffraction shows that the homo-buffer layer is beneficial to the crystalline of N-doped ZnO thin films and all films have preferable c-axis orientation. Atomic force microscopy shows that undoped ZnO thin film grown on homo-buffer layer has an evident improvement of smoothness compared with N-dope ZnO thin films. Hall-effect measurements show that all ZnO films annealed at $800^{\circ}C$ possess p-type conductivities. The undoped ZnO film has the highest carrier concentration of $1.145{\times}10^{17}cm{-3}$. The photoluminescence spectra show the emissions related to FE, DAP and many defects such as $V_{Zn}$, $Zn_O$, $O_i$ and $O_{Zn}$. The p-type defects ($O_i$, $V_{Zn}$, and $O_{Zn}$) are dominant. The undoped ZnO thin film has a better p-type conductivity compared with N-doped ZnO thin film.

유기금속화학증착법으로 유리기판 위에 성장된 산화아연 하이브리드 구조의 광학적 전기적 특성 (Optical and Electrical Properties of ZnO Hybrid Structure Grown on Glass Substrate by Metal Organic Chemical Vapor Deposition)

  • 김대식;강병훈;이창민;변동진
    • 한국재료학회지
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    • 제24권10호
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    • pp.543-549
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    • 2014
  • A zinc oxide (ZnO) hybrid structure was successfully fabricated on a glass substrate by metal organic chemical vapor deposition (MOCVD). In-situ growth of a multi-dimensional ZnO hybrid structure was achieved by adjusting the growth temperature to determine the morphologies of either film or nanorods without any catalysts such as Au, Cu, Co, or Sn. The ZnO hybrid structure was composed of one-dimensional (1D) nanorods grown continuously on the two-dimensional (2D) ZnO film. The ZnO film of 2D mode was grown at a relatively low temperature, whereas the ZnO nanorods of 1D mode were grown at a higher temperature. The change of the morphologies of these materials led to improvements of the electrical and optical properties. The ZnO hybrid structure was characterized using various analytical tools. Scanning electron microscopy (SEM) was used to determine the surface morphology of the nanorods, which had grown well on the thin film. The structural characteristics of the polycrystalline ZnO hybrid grown on amorphous glass substrate were investigated by X-ray diffraction (XRD). Hall-effect measurement and a four-point probe were used to characterize the electrical properties. The hybrid structure was shown to be very effective at improving the electrical and the optical properties, decreasing the sheet resistance and the reflectance, and increasing the transmittance via refractive index (RI) engineering. The ZnO hybrid structure grown by MOCVD is very promising for opto-electronic devices as Photoconductive UV Detectors, anti-reflection coatings (ARC), and transparent conductive oxides (TCO).

수퍼커패시터 전극을 위한 폴리아닐린/TiO2 복합체의 제조 및 전기화학적 성질 (Preparation and Electrochemical Properties of PANI/TiO2 Composites for Supercapacitor Electrodes)

  • 박수근;김광만;이영기;정용주;김석
    • Korean Chemical Engineering Research
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    • 제50권1호
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    • pp.50-54
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    • 2012
  • 본 연구는 커패시터 전극 응용을 위한 복합체 전극에 관련된 것으로 PANI와 PANI/$TiO_2$로 구성된 수퍼커패시터 전극을 제조하여 cyclic voltammetry(CV)를 이용하여 6 M KOH 수용액에서 축전량(capacitance) 특성을 조사하였다. PANI/$TiO_2$ 복합체는 간단한 in-situ 방법을 통해 다양한 비율로 합성되었다. PANI/$TiO_2$ 복합체의 형태학(morphology)적 특징을 파악하기 위해서 주사전자현미경(SEM)과 투과전자현미경(TEM)을 통해 분석하였고, X선 회절 분석기(XRD)를 이용하여 복합체의 결정화도와 담지된 $TiO_2$의 입자크기를 확인하였다. 전기화학적 시험 결과, 아닐린 대비 $TiO_2$의 주입량이 10 wt%일 때 가장 우수한 축전량(626 $Fg^{-1}$)을 나타냈고 높은 주사속도인 100 $mVs^{-1}$에서 286 $Fg^{-1}$의 비축전량을 나타내었다. 이는 폴리아닐린(PANI) 매트릭스(matrix)에 균일하게 담지된 $TiO_2$(~6.5 nm)가 효과적인 연결 구조를 형성하여 전하이동현상이 증가하고, 축전이 가능한 반응면적이 증가한 것과 관련있다고 판단된다.

중금속 흡착을 위한 원위치 피복소재로서 천연제올라이트의 양이온교환용량에 따른 적용성 평가 (Applicability of Natural Zeolite with Different Cation Exchange Capacity as In-situ Capping Materials for Adsorbing Heavy Metals)

  • 강구;신원호;홍성구;김영기;박성직
    • 대한환경공학회지
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    • 제39권2호
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    • pp.51-58
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    • 2017
  • 본 연구에서는 오염퇴적물의 원위치 피복을 위한 소재의 적용성 평가를 위해 양이온교환용량이 다른 제올라이트의 중금속 흡착특성을 평가하였다. 실험을 위해 양이온교환용량이 높은 제올라이트(HCzeo, 163.74 cmol/kg), 중간 값의 양이온교환용량의 제올라이트(MCzeo, 127.20 cmol/kg), 양이온교환용량이 낮은 제올라이트(LCzeo, 70.62 cmol/kg)를 사용하였다. 비표면적을 측정한 결과 HCzeo ($59.43m^2/g$) > MCzeo ($52.10m^2/g$) > LCzeo ($10.12m^2/g$)순으로 높은 결과를 나타내었다. 광물학적 조성 분석을 위해 XRD 측정결과 LCzeo는 quartz와 albite로 구성되었고 MCzeo와 HCzeo의 구성광물은 quartz, albite와 더불어 clinoptilolite, heulandite, mordenite도 측정되었다. HCzeo, MCzeo, LCzeo를 이용한 Cd, Cu, Ni, Zn의 동역학적 흡착실험 결과 실험 6시간대에 흡착 평형에 도달하였다. 평형흡착실험 결과 Cd과 Zn의 흡착은 제올라이트의 양이온교환용량에 따라 증가하였지만 Cu와 Ni의 흡착은 양이온교환용량에 따라 증가하는 경향을 보이지 않았다. 이에 따라 오염퇴적물의 원위치 피복적용에 있어 Cd과 Zn으로 오염된 지역은 양이온교환용량이 높은 제올라이트의 피복적용이 효과적이지만 Cu와 Ni로 오염된 지역의 경우 가격이 저렴한 양이온교환용량이 낮은 제올라이트를 적용하여도 무방할 것으로 판단된다.