• 제목/요약/키워드: Vacuum monochromator

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이차전지 양극활물질의 chemical state 측정을 위한 X0ray Induced Electron Emission Spectroscopy (XIEES)의 활용

  • 이재철;송세안;임창빈
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2000년도 제18회 학술발표회 논문개요집
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    • pp.167-167
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    • 2000
  • 전지 재료의 충방전 과정 연구에는 X-선 분말회절(x-ray powder diffraction techniques)과 중성자회절을 많이 사용하였다. 하지만 이러한 분석기술은 long-range order의 구조에 관한 정보를 제공하는데 유용하지만 atomic scale의 구조에 관한 정보를 얻기에는 한계가 있다. Li 전지에서의 전기화학적 반응에서는 cathode 물질에 포함된 전이금속의 산화, 환원 반응에 의한 Li 이온의 intercalation (charge process)과 deintercalation (discharge process) 현상이 일어난다. 이러한 충방전 과정은 알려지지 않은 다양한 형태의 위상 변화를 동반하게 되는데 x-선 이나 중성자를 이용한 powder diffraction techniques 로는 단지 정성적인 결정학적 정보를 얻을 수 있다. 따라서 최근에 원자 단위의 local structure에 관한 정보와 electrochemical state에 관한 정보를 동시에 얻을 수 있는 X-ray Absorption Fine Structure (XAFS) 분석기술을 Li 전지분석에 활용하기 시작하였다. XAFS는 하나의 x-ray 흡수원자에 대해서 주변원자들의 원자구조에 관한 정보와 구성 원소의 electrochemical state에 관한 정보를 얻을 수 있는 분석방법이다. X-ray Induced Electron Emission Spectroscopy (XIEES)는 x-ray에 의해서 방출된 전자를 검출하여 스펙트럼을 얻는 기능을 함축적으로 나타낸 것으로, x-ray를 물질 표면에 조사하여 발생하는 광전자, Auger 전자, 이차전자 등을 전자검출기(Channel Electron Multiplier: CEM)로 검출하는 기능과, 시료를 투과한 x-ray와 시료에서 발생하는 형광 x-ray를 비례계수기로 검출하는 기능을 가지고 있다. 이러한 검출 능력을 바탕으로 EXAFS, XANES, Standing Wave Technique, Elemental Composition Analysis, DXRD, Total Reflection Technique 등을 이용하여 물질을 구성하고 있는 원소의 성분, 미세원자구조, 전자구조에 관한 정보를 얻을 수 있는 새로운 spectrometer이다. 본 연구에서는 자체 개발한 XIEES의 XAFS 기능을 이용하여 여러 가지 방법으로 제조한 LiMn2-xO4와 LiMnO2, MnO2에서 Mn K-absorption edge에 대한 chemical state 변화를 측정하였다. Absorption edge에서 chemical shift를 측정하기 위해서는 방사광 가속기 수준의 에너지 분해능(~0.3eV)이 필요하다. 이번 연구에서는 SiO2(3140) monochromator를 사용하고 여기에 맞는 적절한 parameter를 적용하여 x-ray 에너지 분해능을 포항방사광가속기 수준으로 개선하였다. XIEES에서 얻은 스펙트럼과 포항방사광가속기에서 얻은 스펙트럼을 비교하였다. Chemical shift가 일어나는 경향은 두 실험 결과가 잘 일치하였다.

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Photo-induced Electrical Properties of Metal-oxide Nanocrystal Memory Devices

  • Lee, Dong-Uk;Cho, Seong-Gook;Kim, Eun-Kyu;Kim, Young-Ho
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2011년도 제41회 하계 정기 학술대회 초록집
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    • pp.254-254
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    • 2011
  • The memories with nano-particles are very attractive because they are promising candidates for low operating voltage, long retention time and fast program/erase speed. In recent, various nano-floating gate memories with metal-oxide nanocrystals embedded in organic and inorganic layers have been reported. Because of the carrier generation in semiconductor, induced photon pulse enhanced the program/erase speed of memory device. We studied photo-induced electrical properties of these metal-oxide nanocrystal memory devices. At first, 2~10-nm-thick Sn and In metals were deposited by using thermal evaporation onto Si wafer including a channel with $n^+$ poly-Si source/drain in which the length and width are 10 ${\mu}m$ each. Then, a poly-amic-acid (PAA) was spin coated on the deposited Sn film. The PAA precursor used in this study was prepared by dissolving biphenyl-tetracarboxylic dianhydride-phenylene diamine (BPDA-PDA) commercial polyamic acid in N-methyl-2-pyrrolidon (NMP). Then the samples were cured at 400$^{\circ}C$ for 1 hour in N atmosphere after drying at 135$^{\circ}C$ for 30 min through rapid thermal annealing. The deposition of aluminum layer with thickness of 200 nm was followed by using a thermal evaporator, and then the gate electrode was defined by photolithography and etching. The electrical properties were measured at room temperature using an HP4156a precision semiconductor parameter analyzer and an Agilent 81101A pulse generator. Also, the optical pulse for the study on photo-induced electrical properties was applied by Xeon lamp light source and a monochromator system.

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X-ray Radiography에 적합한 Double Multilayer Monochromaotr (DMM) 설계와 제작

  • 정순용;양성선;임재홍
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.118-118
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    • 2013
  • DMM은 방사광가속기의 백색광으로부터 단색광을 추출하기 위해 두 개의 다층 박막 (multilayer) 거울을 사용하는데, 첫 번째 거울은 Bragg 반사를 통해 분광을 하여 단색광을 생산하는 용도이고, 두 번째 거울은 이 단색광을 반사시켜 지면과 평행하게 출사되게 하기 위함이다. 일반적으로 사용되는 DCM (Double Crystal Monochromator)과의 차이점은, Bragg 반사를 위해 DCM에서는 결정을 사용하는 반면 DMM은 밀도차이가 많이나는 두 종류의 물질을 교대로 쌓아 올린 다층 박막을 사용한다는 것이다. 다층 박막의 주기가 곧 Bragg 반사에서의 d-spacing이 되며, X-선 분광의 목적으로 사용되는 d-spacing은 10-50 $\AA$ 사이이다. DCM이 0.01% 대의 우수한 에너지 분해능을 보이는데 비해, DMM은 1% 정도이다. 이 때문에 출사광의 밝기가 DCM에 비해 100배 밝은 특징이 있어서 에너지 분해능보다 광량이 더 중요한 응용에서 DMM이 사용된다. X-선 영상이나 방사선치료가 바로 이러한 응용에 해당한다. DMM은 포항가속기연구소와 (주) 벡트론에서 공동 설계하였으며, (주)벡트론에서 제작하였다. 그림 1에 DMM의 외형과 내부 구조를 나타내었다. Bragg 각의 조절 범위는 0.24-0.9도 이다. 입사광과 출사광의 수직 방향 offset을 10 mm로 유지하기 위해 두 번째 다층 박막이 수평방향으로 1,000 mm 가량 이동할 수 있어야 한다. 이를 위해 두 대의 고니오미터 stage를 사용하여 각각 첫 번째 및 두 번째 다층 박막의 위치와 방향을 제어한다. 첫 번째 다층 박막을 제어하는 고니오미터 stage는 하부가 전체 프레임에 고정되어 있고, 이 고니오미터의 회전축에서 Bragg 각을 조절한다. 두 번째 다층 박막을 제어하는 고니오미터 stage는 높이방향과 수평방향으로 이동이 가능하다. 다층 박막의 pitch는 고니오미터의 회전축에서 조절한다. 그리고 tilt stage를 사용하여 다층 박막의 roll을 조절한다.

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Optical Diagnostics for Pulse-discharged Plasma by Marx Generator and Its Application for Modifications of Hemoglobin and Myoglobin Proteins

  • Park, Ji Hoon;Attri, Pankaj;Hong, Young June;Park, Bong Sang;Jeon, Su Nam;Choi, Eun Ha
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.176.2-176.2
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    • 2013
  • Property of optical diagnostics for pulse-discharged plasma in liquid and its biological applications to proteins are investigated by making use of high voltage Marx generator. The Marx generator has been consisted of 5 stages, where each charging capacitor is 0.5 ${\mu}F$, to generate a high voltage pulse with rising time of $1{\mu}s$. We have applied an input voltage of 6 kV to the each capacitor of 0.5 ${\mu}F$. High voltage pulsed plasma has been generated inside a polycarbonate tube by a single-shot operation, where the breakdown voltage is measured to be 7 kV, current of 1.2 kA, and pulse width of ~ 1 ${\mu}s$ between the two electrodes of anode-cathode whose material is made of tungsten pin, which are immersed into the liquids. We have investigated the emitted hydrogen lines for optical diagnostics of high voltage pulsed plasma. The emission line of 656.3 nm from $H-{\alpha}$ and 486.1 nm from $H-{\beta}$ have been measured by a monochromator. If we assumed that the focused plasma regions satisfy the local thermodynamic equilibrium conditions, the electron temperature and density of the high voltage pulsed plasma in liquid could be obtained by the Stark broadening of optical emission spectroscopy. For the investigation of the influence of pulsed plasma on biological proteins, we have exposed it onto the proteins such as hemoglobin and myoglobin. The structural changes in these proteins and their analysis have also been obtained by circular dichroism (CD) and ultraviolet (UV) visible spectroscopy.

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The New X-ray Induced Electron Emission Spectrometer

  • Yu.N.Yuryev;Park, Hyun-Min;Lee, Hwack-Ju;Kim, Ju-Hwnag;Cho, Yang-Ku;K.Yu.Pogrebitsky
    • 한국결정학회:학술대회논문집
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    • 한국결정학회 2002년도 정기총회 및 추계학술연구발표회
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    • pp.5-6
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    • 2002
  • The new spectrometer for X-ray Induced Electron Emission Spectroscopy (XIEES) .has been recently developed in KRISS in collaboration with PTI (Russia). The spectrometer allows to perform research using the XAFS, SXAFS, XANES techniques (D.C.Koningsberger and R.Prins, 1988) as well as the number of techniques from XIEES field(L.A.Bakaleinikov et all, 1992). The experiments may be carried out with registration of transmitted through the sample x-rays (to investigate bulk samples) or/and total electron yield (TEY) from the sample surface that gives the high (down to several atomic mono-layers in soft x-ray region) near surface sensitivity. The combination of these methods together give the possibility to obtain a quantitative information on elemental composition, chemical state, atomic structure for powder samples and solids, including non-crystalline materials (the long range order is not required). The optical design of spectrometer is made according to Johannesson true focusing schematics and presented on the Fig.1. Five stepping motors are used to maintain the focusing condition during the photon energy scan (crystal angle, crystal position along rail, sample goniometer rail angle, sample goniometer position along rail and sample goniometer angle relatively of rail). All movements can be done independently and simultaneously that speeds up the setting of photon energy and allows the using of crystals with different Rowland radil. At present six curved crystals with different d-values and one flat synthetic multilayer are installed on revolver-type monochromator. This arrangement allows the wide range of x-rays from 100 eV up to 25 keV to be obtained. Another 4 stepping motors set exit slit width, sample angle, channeltron position and x-ray detector position. The differential pumping allows to unite vacuum chambers of spectrometer and x-ray generator avoiding the absorption of soft x-rays on Be foil of a window and in atmosphere. Another feature of vacuum system is separation of walls of vacuum chamber (which are deformed by the atmospheric pressure) from optical elements of spectrometer. This warrantees that the optical elements are precisely positioned. The detecting system of the spectrometer consists of two proportional counters, one scintillating detector and one channeltron detector. First proportional counter can be used as I/sub 0/-detector in transmission mode or by measuring the fluorescence from exit slit edge. The last installation can be used to measure the reference data (that is necessary in XANES measurements), in this case the reference sample is installed on slit knife edge. The second proportional counter measures the intensity of x-rays transmitted through the sample. The scintillating detector is used in the same way but on the air for the hard x-rays and for alignment purposes. Total electron yield from the sample is measured by channeltron. The spectrometer is fully controlled by special software that gives the high flexibility and reliability in carrying out of the experiments. Fig.2 and fig.3 present the typical XAFS spectra measured with spectrometer.

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XAS Studies of Ion Irradaited MgO Thin Films

  • Suk, Jae-Kwon;Gautam, Sanjeev;Song, Jin-Ho;Lee, Jae-Yong;Kim, Jae-Yeoul;Kim, Joon-Kon;Song, Jong-Han;Chae, Keun-Hwa
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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    • pp.312-312
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    • 2012
  • Magnesium oxide has become focus for research activities due to its use in magnetic tunnel junctions and for understanding of do ferromagnetism. Theoretical investigations on such type of system indicate that the presence of defects greater than a threshold value is responsible for the magnetic behaviour. It has also been shown experimentally that by decreasing the film thickness and size of nanoparticles, enhancement/increase in magnetization can be achieved. Apart from the change in dimension, swift heavy ions (SHI) are well known for creating defects and modifying the properties of the materials. In the present work, we have studied the irradiation induced effects in magnesium oxide thin film deposited on quartz substrate via X-ray absorption spectroscopy (XAS). Magnesium oxide thin films of thickness 50nm were deposited on quartz substrate by using e-beam evaporation method. These films were irradiated by 200 MeV Ag15+ ion beam at fluence of $1{\times}10^{11}$, $5{\times}10^{11}$, $1{\times}10^{12}$, $3{\times}10^{12}$ and $5{\times}10^{12}ions/cm^2$ at Nuclear Science Centre, IUAC, New Delhi (India). The grain size was observed (as studied by AFM) to be decreased from 37 nm (pristine film) to 23 nm ($1{\times}10^{12}ions/cm^2$) and thereafter it increases upto a fluence of $5{\times}10^{12}ions/cm^2$. The electronic structure of the system has been investigated by X-ray absorption spectroscopy (XAS) measurements performed at the high energy spherical grating monochromator 20A1 XAS (HSGM) beamline in the National Synchrotron Radiation Research Center (NSRRC), Taiwan. Oxides of light elements like MgO/ZnO possess many unique physical properties with potentials for novel application in various fields. These irradiated thin films are also studied with different polarization (left and right circularly polarized) of incident x-ray beam at 05B3 EPU- Soft x-ray scattering beamline of NSRRC. The detailed analysis of observed results in the wake of existing theories is discussed.

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