• 제목/요약/키워드: Electron crystallography

검색결과 59건 처리시간 0.026초

Electronic Structure of [NiS4]- Investigated by Single-Crystal EPR and Density Functional Theory

  • Min, Su-Young;Noh, Dong-Youn;Choi, Cheol-Ho;Lee, Hong-In
    • 한국자기공명학회논문지
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    • 제16권1호
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    • pp.78-90
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    • 2012
  • To understand the electronic structure of $[NiS_4]^-$ complex ions, two complexes with such $[NiS_4]^-$ core, $FcCH=CHPymCH_3[Ni(dmit)_2]$ (Pym = pyridinium, $dmit^{2-}$ = 2-thioxo-1,3-dithiole-4,5-dithiolate) and $FcCH=CHPymCH_3[Ni(dddt)_2]{\cdot}{\frac{1}{2}}H_2O$ ($dddt^{2-}=5,6-dihydro-1,4-dithiin-2,3-dithiolato$), were synthesized to be characterized by X-ray crystallography, single crystal electron paramagnetic resonance (EPR) and density functional theory (DFT) calculation. Powder EPR spectra show narrow g-anisotropy but the anisotropy is bigger in $[Ni(dmit)_2]^-$ than in $[Ni(dddt)_2]^-$, indicating bigger spin density in Ni(III) d-orbital of $[Ni(dmit)_2]^-$ than in $[Ni(dddt)_2]^-$, which is consistent to DFT results. EPR studies of the crystals of the complexes surprisingly suggest that the $g_y$-axis of $[Ni(dddt)_2]^-$ is approximately on or perpendicular to the $[NiS_4]^-$ plane while the $g_y$-axis of $[Ni(dmit)_2]^-$ is on the plane, though DFT study of the complexes of this study and previously reported $[NiS_4]^-$ complexes indicate that the $g_y$-axis is on the $[NiS_4]^-$ plane.

수렴성전자회절에 의한 n-형 세라믹 초전도체 $Nd_{2-x}Ce_xCuO_{4-\upsilon}$의 결정구조 전이 연구 (Inestigation on the Structural Transition of n-type Ceramic Superconductor, $Nd_{2-x}Ce_xCuO_{4-\upsilon}$ System of CBED)

  • 김정식;유광수
    • 한국세라믹학회지
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    • 제34권2호
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    • pp.139-144
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    • 1997
  • 결정학적으로 T' 구조인 Nd2-xCexCuO4-$\delta$ 회토류 구리산화물 초전도체는 지금까지 매우 복잡한 미세구조를 지닌 것으로써 잘 알려져 있다. 이 구리산화물 초전도체가 초전도 특성을 띠려면, Nd3+ 이온이 Ce4+ 이온에 의해 소량 치환되고 동시에 산소환원이 필요하다. 본 연구에서는 투과전자현미경의 수렴성 전자회절(CBED)패턴을 이용하여 Nd2-xCexCuO4-$\delta$ 의 Ce 미량 첨가와 미량의 산소환원에 따른 결정구조의 전이 발생 여부에 관하여 고찰하였다. 세 가지의 서로 다른 시편 Nd2CuO3,Nd1.85Ce0.15CuO4 와Nd1.85Ce0.15CuO3.965을 고상소결에 의하여 만들어 이들 각각 시편에 대한 CBED패턴을 주사투과전자현미경(STEM)으로 관찰하였다. 그리고 실험에 의하여 얻은 이들 HOLZ선들과 컴퓨터 계산에 의해 그려진 이론적인 HOLZ선들과 비교하는 방법에 의하여 Nd1.85Ce0.15CuO4의 격자상수를 구하였다.

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$CdS/CuInSe_2$태양전지의 Window Layer로 쓰이는 CdS박막의 진공증착법에 따른 전기적.광학적 성질 (Electrical and Optical Properties of Vacuum-Evaporated CdS Films for the Window Layer of $CdS/CuInSe_2$ Solar Cells.)

  • 남희동;이병하;박성
    • 한국결정학회지
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    • 제8권2호
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    • pp.105-110
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    • 1997
  • CdS/CuInSe2 태양전지에서 창측재료로 1μm 두께의 CdS박막을 1x10-3mTorr의 진공하에서 CdS source 온도를 800-1100'C로 하고 기판의 온도를 50-200℃로하여 진공증차겁으로 제조하였다. 증착된 CdS박막의 구조적, 전기적, 광학적 특성조사는 x-ray diffractometer(XRD), scanning electron microscope(SEM), 전기비저항 측정, Hall measurement 그리고 optical transmission spectra로 행하였고, 각막들의 성분분석은 energy dispersive analysis of X-ray (EDAX)를 가하나, 광투과도는 감소하였다. 이때 증착된 CdS 박막들은 모두 hexagonal 구조를 가지고 있었으며, 결정성은 기판유리를 딸 (002)면으로 형성되었다. CdS Source 온도가 1000℃에서 증착된 CdS 박막이 0.9(S/cm)의 가장 높은 전기 전도도를 나타내었다. 또한 기판온도를 100'C로 제조한 CdS 박막이 전기비저항은 40(Ω,cm)이었고 광투과도는 80% 이상의 값을 나타내어 CdS/CuInSe2 태양전지의 창측재료로 적합했다.

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The Morphology and Crystallography of Isothermal Martensite in Yttria Stabilized Zirconia

  • Pee, Jae-Hwan;Choi, Eui-Seok;Hayakawa, Motozo
    • 한국세라믹학회지
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    • 제43권2호
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    • pp.69-73
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    • 2006
  • A full retention of the tetragonal phase with coarse grains $(50\~60\;{\mu}m)$ was possible with the specimen $ZrO_2-1.9\;mol\%\;Y_2O_3$. In these coarse grains, $\{101\}_t$ annealing twins were frequently observed, although they do not exist in the usual fine grained specimens. The morphology and growth rate of the isothermally formed individual products are studied at an optical microscopic level. The habit planes of both products are also identified by performing two-surface trace analysis on the grains whose orientations are determined by the Electron Back Scattering Pattern (EBSP) method. The morphologies of isothermal martensite were well-defined thin plates and lenticular types. The growth rate in their longitudinal directions was quite slow and temperature-dependent. A two-surface trace analysis, incorporated with the EBSP method, identified the habit planes near $\{013\}_c$, in agreement with previous reports obtained from TEM works.

Doping-Concentration and Annealing Effects on Photoluminescence Profile of Eu(III)-doped CeO2 nanorods

  • Lee, Juheon;Park, Yohan;Joo, Sang Woo;Sohn, Youngku
    • Bulletin of the Korean Chemical Society
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    • 제35권11호
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    • pp.3319-3325
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    • 2014
  • Eu(III)-doped $CeO_2$ nanorods were prepared by a co-precipitation method at room temperature, and their photoluminescence profiles were examined with different Eu(III)-doping concentrations and thermal annealing temperatures. Scanning electron microscopy, X-ray diffraction crystallography and UV-Vis absorption spectroscopy were employed to examine the morphology, crystal structure and photon absorption profiles of the nanorods, respectively. Additionally, their 2D and 3D-photoluminescence profile maps were obtained to fully understand the photoluminescence mechanism. We found that the magnetic dipole $^5D_0{\rightarrow}^7F_1$ and the electric dipole $^5D_0{\rightarrow}^7F_2$ transitions of Eu(III) were highly dependent on the doping concentration, annealing temperature and excitation wavelength, which was explained by the presence of different Eu(III)-doping sites (with and without an inversion center) in the $CeO_2$ host with a cubic crystal structure.

내열금속 기판위에 다이아몬드 박막의 증착과 특성분석 (Vapor Phase Deposition and Characterization of Diamond Thin Films on Refractory Metals)

  • 홍성현;형준호
    • 한국결정학회지
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    • 제5권1호
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    • pp.39-50
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    • 1994
  • Hot Tungsten Filament법에 의해 실리콘(Si), 몰리브데늄(Mo), 타이타늄(Ti), 텅스텐(W) 기판 위에 다이아몬드 박막을 증착시시키고 SEM, X선 회절분석 및 Raman spectroscopy로 분석하였다. 증착시간에 따른 증착실험의 결과로부터 내열금속위에 증착한 다이아몬드박막의 경우에는 먼저 탄화물 층이 형성되고, 그 이후에 다이아몬드가 핵형성되어 성장함을 알 수 있었다. 내열금속에 증착한 다이아몬드 박막은 5기판 위에 증착한 것과 비교할 때, 핵이 많이 형성되었고 facet이 잘 발달된 입자가 적었다. 5기판 뿐만 아니라 내열금속 기판 위에 다이아몬드막을 증착시킬 경우, 다이아몬드의 Raman 피크는 천연 다이아몬드에 비해 높은 주파수쪽으로 이동되었다. 이와같은 Raman 피크의 이동은 다이아몬드와 기판 사이의 열충격보다는 완충층의 역활을 하는 탄화물과 다이아몬드 사이의 열충격을 고려할 때 효과적으로 설명이 가능하였다. 생성된 탄화물의 형태와 다이아몬드 사이에 열충격이 가장 큰 Mo기판의 경우, 다이아몬드 Rarirm 피크의 이동이 가장 크게 나타났으며 Ti, W, Si기판의 순서로 이동이 적게 관찰되었다.

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$Bi_{12}GeO_{20}$단결정 육성 및 표면탄성파 소자 제조 (Growth of Optical Quality $Bi_{12}GeO_{20}$ Crystals and Preparation of SAW-Filter)

  • 이태근;정수진
    • 한국결정학회지
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    • 제2권2호
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    • pp.32-40
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    • 1991
  • The effects of compositional variation, rotation speel and pulling rate on the growth of optical quality Bi120e02(1 crystals were examined. It was found to flatten the shape of crystal-melt interface for yowing a single crystals less than about 30mm in diameter at the rotation speed of 50rpm. Diameter of crystals with flat interface was increased as the pulling rate. The precipitation of Bi40e3012 phase set limits to pulling rate of BGO crystals. Precipitate-free BGO crystals were grown under pulling rate of 2mm l hr which released the stress resulted from too hi어 Pulling rate, and from 6. IBi203·GeO2 batch composition obtained by addition of 0.1 mole Bi203 into Bi-deficient melts to fill up the deficiency resulted from gradual volatilization of Bi2O). The pale-yellow colored crystals had good quality in that dislocation density was less than 103pits/cm, and it also exhibited transmittance of 70% and optical activity of 23°/mm. and SAW velosity was measured 1700m/sec on 111 cut 110 propagating BGO crystals. The SAW filter with electrode thickness of 9.8um was fabricated by using the electron beam and dry etching technique, it makes Bi12GeO20 devices intersting for color TV IF with half device size.

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Use of Molecular Replacement to Determine the Phases of Crystal Structure of Taq DNA Polymerase

  • Kim, Young-Soo;Suh, Se-Won
    • BMB Reports
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    • 제29권1호
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    • pp.38-44
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    • 1996
  • Taq DNA polymerase from Thermus aquaticus has been shown to be very useful in the polymerase chain reaction method, which is being used for amplifying DNA. Not only does Taq DNA polymerase have high commercial value commercial value for the polymerase chain reaction application, but it is also important in studying DNA replication, because it is apparently an homologue to E. coli DNA polymerase I, which has long been used for DNA replication study (Lawyer et ai., 1993). The crystal structure determination of Taq DNA polymerase was initiated. An X-ray diffraction pattern breaks down a crystal structure into discrete sine waves in a Fourier series. The original shape of a crystal object in terms of electron density may be represented as the sum of those sine waves with varying amplitudes and phases in three dimensions. The molecular replacement method was initially employed to provide phase information for the structure of Taq DNA polymerase. The rotation search using the program MERLOT resulted in a solution peak with 5.4 r.m.s. PC-refinement of the X-PLOR program verified the result and also optimized the orientation angles. Next, the translation search using the X-PLOR program resulted in a unique solution peak with 7.35 r.m.s. In addition, the translation search indicated $P3_121$ to be the true space group out of two possible ones. The phase information from the molecular replacement was useful in the MIR phasing experiment.

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Synthesis and Characterization of Nickel(II) Tetraaza Macrocyclic Complex with 1,1-Cyclohexanediacetate Ligand

  • Lim, In-Taek;Kim, Chong-Hyeak;Choi, Ki-Young
    • 대한화학회지
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    • 제62권6호
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    • pp.427-432
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    • 2018
  • The reaction of [$[Ni(L)]Cl_2{\cdot}2H_2O$ (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[$14,4,0^{1.18},0^{7.12}$]docosane) with 1,1-cyclohexanediacetic acid ($H_2cda$) yields mononuclear nickel(II) complex, [$Ni(L)(Hcda^-)_2$] (1). This complex has been characterized by X-ray crystallography, electronic absorption, cyclic voltammetry and thermogravimetric analyzer. The crystal structure of 1 exhibits a distorted octahedral geometry with four nitrogen atoms of the macrocycle and two 1,1-cyclohexanediacetate ligands. It crystallizes in the triclinic system P-1 with a = 11.3918(7), b = 12.6196(8), $c=12.8700(8){\AA}$, $V=1579.9(2){\AA}^3$, Z = 2. Electronic spectrum of 1 also reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes one wave of a one-electron transfer corresponding to $Ni^{II}/Ni^{III}$ process. TGA curve for 1 shows three-step weight loss. The electronic spectra, electrochemical and TGA behavior of the complex are significantly affected by the nature of the axial $Hcda^-$ ligand.

The LaserFIB: new application opportunities combining a high-performance FIB-SEM with femtosecond laser processing in an integrated second chamber

  • Ben Tordoff;Cheryl Hartfield;Andrew J. Holwell;Stephan Hiller;Marcus Kaestner;Stephen Kelly;Jaehan Lee;Sascha Muller;Fabian Perez-Willard;Tobias Volkenandt;Robin White;Thomas Rodgers
    • Applied Microscopy
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    • 제50권
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    • pp.24.1-24.11
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    • 2020
  • The development of the femtosecond laser (fs laser) with its ability to provide extremely rapid athermal ablation of materials has initiated a renaissance in materials science. Sample milling rates for the fs laser are orders of magnitude greater than that of traditional focused ion beam (FIB) sources currently used. In combination with minimal surface post-processing requirements, this technology is proving to be a game changer for materials research. The development of a femtosecond laser attached to a focused ion beam scanning electron microscope (LaserFIB) enables numerous new capabilities, including access to deeply buried structures as well as the production of extremely large trenches, cross sections, pillars and TEM H-bars, all while preserving microstructure and avoiding or reducing FIB polishing. Several high impact applications are now possible due to this technology in the fields of crystallography, electronics, mechanical engineering, battery research and materials sample preparation. This review article summarizes the current opportunities for this new technology focusing on the materials science megatrends of engineering materials, energy materials and electronics.