• 제목/요약/키워드: X-Ray diffraction measurement

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First Example of Monometallic Palladium(II) Compound with Trans-Chelating Tridentate Ligand: Synthesis, Crystal Structure, and Characterizations

  • Tae Hwan Noh
    • Mass Spectrometry Letters
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    • 제14권3호
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    • pp.110-115
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    • 2023
  • The reaction of (COD)PdCl2 with new C3-symmetric tridentate L (COD = 1,5-cyclooctadien; L = 1,3,5-tris(picolinoyloxyethyl)cyanurate) in a mixture of acetone and dichloromethane produces single crystals consisting of unprecedented monometallacyclic [PdCl2(L)]. This cyclic compound arises from trans-chelation of two of three donating pyridyl groups of L, while the third pyridyl group remains uncoordinated. Electrospray ionization mass spectrometry (ESI-MS) data on L exhibited the major peak corresponding to [C27H24N6O9 + H+]+. Fast atom bombardment mass spectrometry (FABMS) data on [PdCl2(L)], however, showed the mass peak corresponding to the L instead of the present palladium(II) compound species, due to the insolubility and dissociation in solution. The physicochemical properties of the present palladium(II) compound were fully characterized by means of infrared (IR) and nuclear magnetic resonance (NMR) spectroscopy, thermal analysis, single-crystal X-ray diffraction (SC-XRD) measurement.

Antibacterial property and characterization of CuSn thin films deposited by RF magnetron co-sputtering method

  • 강유진;박주연;김동우;김학준;강용철
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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    • pp.360.2-360.2
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    • 2016
  • CuSn thin films were fabricated by rf magnetron co-sputtering method on the Si(100) substrate for evaluation of the antibacterial effect. The co-sputtering process was performed with different rf powers and sputtering times to regulate the thickness of the films and relative atomic ratio of Cu to Sn. The physicochemical properties of the CuSn thin films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray induced Auger electron spectroscopy (XAES), Optical microscope (OM), 4-point probe, and antibacterial test. An antibacterial test was conducted with Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) as changing contact times between CuSn fillms and bacteria suspension. We compared to the crystalline structures of films before sterilization and after sterilization by XRD measurement. The changes of oxidation states of Cu and Sn and the chemical environment of films before and after antibacterial test were investigated with high resolution XPS spectra in the regions of Cu 2p, Cu LMM, and Sn 3d. After antibacterial test, the morphology of the films was checked with an OM images. The electrical properties of the CuSn films such as surface resistance and conductivity were measured by using 4-point probe.

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중.저온형 고체 산화물 연료전지의 공기극으로 사용되는 PSCF3737 물질의 특성에 관한 연구 (Characterization of PSCF3737 for intermediate temperature solid oxide fuel cell (IT-SOFC))

  • 박광진;배중면
    • 한국신재생에너지학회:학술대회논문집
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    • 한국신재생에너지학회 2008년도 춘계학술대회 논문집
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    • pp.61-64
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    • 2008
  • $Pr_{0.3}Sr_{0.7}Co_{0.3}Fe_{0.7}O_{3-\delta}$ (PSCF3737) was prepared and characterized as a cathode material for intermediate temperature-operating solid oxide fuel cell (IT-SOFC). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), extended X-ray absorption fine structure (EXAFS), and electrical property measurement were carried out to study cathode performance of the material. XPS and EXAFS results proved that oxygen vacancy concentration was decreased and lattice constants of the perovskite structure material were increased by doping Fe up to 70 mol% at B-site of the crystal structure, which also extended the distance between oxygen and neighbor atoms. Thermal expansion coefficient (TEC) of PSCF3737 is smaller than that of $Pr_{0.3}Sr_{0.7}CoO_{3-\delta}$(PSC37) due to lower oxygen vacancy concentration. PSCF3737 showed better cathode performance than PSC37. It might be due good adhesion by a smaller difference of TEC between $Gd_{0.1}Ce_{0.9}O_2$ (CGO91) and electrode. Composite material PSCF3737-CGO91 showed better compatibility of TEC than PSCF3737. However, PSCF3737-CGO91 did not represent higher electrochemical property than PSCF3737 due to decreased reaction sites by CGO91.

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습식 산화법으로 성장된 산화구리입자를 이용한 방열 컴파운드 제조 및 특성 연구 (Characterizations of Thermal Compound Using CuO Particles Grown by Wet Oxidation Method)

  • 이동우;엄창현;주제욱
    • 한국재료학회지
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    • 제27권4호
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    • pp.221-228
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    • 2017
  • Various morphologies of copper oxide (CuO) have been considered to be of both fundamental and practical importance in the field of electronic materials. In this study, using Cu ($0.1{\mu}m$ and $7{\mu}m$) particles, flake-type CuO particles were grown via a wet oxidation method for 5min and 60min at $75^{\circ}C$. Using the prepared CuO, AlN, and silicone base as reagents, thermal interface material (TIM) compounds were synthesized using a high speed paste mixer. The properties of the thermal compounds prepared using the CuO particles were observed by thermal conductivity and breakdown voltage measurement. Most importantly, the volume of thermal compounds created using CuO particles grown from $0.1{\mu}m$ Cu particles increased by 192.5 % and 125 % depending on the growth time. The composition of CuO was confirmed by X-ray diffraction (XRD) analysis; cross sections of the grown CuO particles were observed using focused ion beam (FIB), field emission scanning electron microscopy (FE-SEM), and energy dispersive analysis by X-ray (EDAX). In addition, the thermal compound dispersion of the Cu and Al elements were observed by X-ray elemental mapping.

$H_2SO_4$-Intercalated Graphite Fiber의 Deintercalation에 관한 연구 (Study on the Deintercalation of $H_2SO_4$--Intercalated Graphite Fiber)

  • 김인기;최상흘;고영신
    • 한국세라믹학회지
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    • 제30권10호
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    • pp.797-802
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    • 1993
  • Graphite fiber intercalated compound was deintercalated at $25^{\circ}C$, 65% of humidity and its deintercalated compound was discussed, based on the X-ray diffraction analysis, electrical resistivity measurement, and UV/VIS spectrometer measurements. During deintercalation, the structure was changed in orderlongrightarrowdisorderlongrightarroworder, and resistivity was decreased in the disorder state of the structure, which reflectance minimum of the UV/VIS spectrum ranged from 660 to 750nm (1.88~1.65eV).

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토기의 소성온도에 따른 미세조직 비교연구 (Microsturucture of pottery by the measurement of firing temperature)

  • 홍종욱;정광룡
    • 보존과학연구
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    • 통권15호
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    • pp.1-20
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    • 1994
  • A typology was established for 15 pottery artefacts at Chejuisland. Conjectured methods of manufacture were confirmed by radiography X-ray diffraction. Scanning electron microscopy etc. The compositions and mineralogy of $500^{\circ}C$ to $1200^{\circ}C$ was measured and compared with those of microstructure. The mechanism of sintering was impurity-initiated, liquid-phase sintering. The making, firing, and sometimes exploding of the figurines may have been the prime function of the pottery at this site rather than being manufactured as permanent, portable object.

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슬래그-석고계 수화반응에 대한 기초 연구 (A Study on Hydration of Slag-Gypsum System)

  • 지정식;최상흘
    • 한국세라믹학회지
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    • 제15권4호
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    • pp.205-212
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    • 1978
  • The hydration reaction of the slag-gypsum system was studied by X-ray diffraction, differential thermal analysis, optical icroscopic observation, and measurement of heat liberation of hydration. 1. Domestic granulated slag was almost noncrystalized state, and its mineral compositions calculated were 46.53% of gehlenite, 28.14% of akermanite, and 19.04% of wollastonite. 2. The slag quenched with water at relatively high temperature had better reactivity. 3. The production of ettringite, CSH gel and AH3 gel were stimulated by effect of $Ca(OH)_2$, $Mg(OH)_2$ and calcined dolomite as activators, and the strength of hardened body would be developed by forming compacted microstructure.

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기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화 (Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders)

  • 이충효;전성용;김지순
    • 한국결정성장학회지
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    • 제14권4호
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    • pp.129-134
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    • 2004
  • 본 연구에서는 기계적 합금화(MA)에 의한 고상-기상반응에 있어서 질소원자가 V-Fe계 합금의 비정질화에 미치는 영향을 조사하였다. 유성형 볼밀을 사용하여 $V_{70}Fe_{30}$혼합분말을 질소가스 분위기 중 MA 처리하였다. 그 결과 160시간 MA 처리에 의하여 비정질상이 생성됨을 알 수 있었다. 160시간 동안 MA 처리한 ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ 분말시료의 열분석 결과 약 $600^{\circ}C$에 비정질상의 결정화에 의한 발열 peak가 관찰되었다. 또한 bcc 결정에서 비정질상으로의 구조변화 과정을 X선 및 중성자 회절법을 통하여 조사하였으며, 특히 중성자회절에서는 V원자의 중성자에 대한 간섭성 핵산란진폭이 매우 작은 특징을 이용하였다. 그 결과, 이 합금계에서의 비정질화는 모든 결정구조에서 전형적으로 존재하는 8면체 unit가 우선적으로 붕괴되어 4면체 unit로 변환되어 가는 과정임을 알 수 있었다. 또한 중성자 회절에 의한 구조해석 결과 질소원자는 V원자로 이루어진 다면체의 중심에 위치하고 있음을 알 수 있었다.

Two-Facing-Targets (TFT) 스퍼터링장치를 이용하여 증착한 AlN박막의 잔류응력 측정 (Measurement of Residual Stress of AlN Thin Films Deposited by Two-Facing-Targets (TFT) Sputtering System)

  • 한창석;권용준
    • 한국재료학회지
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    • 제31권12호
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    • pp.697-703
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    • 2021
  • Aluminum nitride having a dense hexagonal structure is used as a high-temperature material because of its excellent heat resistance and high mechanical strength; its excellent piezoelectric properties are also attracting attention. The structure and residual stress of AlN thin films formed on glass substrate using TFT sputtering system are examined by XRD. The deposition conditions are nitrogen gas pressures of 1 × 10-2, 6 × 10-3, and 3 × 10-3, substrate temperature of 523 K, and sputtering time of 120 min. The structure of the AlN thin film is columnar, having a c-axis, i.e., a <00·1> orientation, which is the normal direction of the glass substrate. An X-ray stress measurement method for crystalline thin films with orientation properties such as columnar structure is proposed and applied to the residual stress measurement of AlN thin films with orientation <00·1>. Strength of diffraction lines other than 00·2 diffraction is very weak. As a result of stress measurement using AlN powder sample as a comparative standard sample, tensile residual stress is obtained when the nitrogen gas pressure is low, but the gas pressure increases as the residual stress is shifts toward compression. At low gas pressure, the unit cell expands due to the incorporation of excess nitrogen atoms.

Au-Te 과 n-GaAs 의 접촉저항 특성 (The characteristics of the specific contact resistance of Au-Te to n-GaAs)

  • 정성훈;송복식;문동찬;김선태
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 1995년도 추계학술대회 논문집
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    • pp.63-66
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    • 1995
  • The ohmic characterization of Au/Te/Au/n-GaAs structure is investigated by the application of x-ray diffraction, scanning electron microscopy, Auger electron spectroscopy, the specific contact resistance and I-V measurement. Increasing the annealing temperature, the results of XRD measurement show the sharpening of the Au-Ga peak and the increasing of the intensity of Au peak due to the crystallization. At 400$^{\circ}C$, which is the ohmic onset point, Ga$_2$Te$_3$peak gets evident and GaAs regrowth peak appears for the samples annealed at 500$^{\circ}C$. The variation of shottky contact to ohmic contact is confirmed by the I-V curve transition. The specific contact resistance of 3.8x10$\^$-5/$\Omega$-$\textrm{cm}^2$ is obtained for the sample annealed at 500$^{\circ}C$ and above 600$^{\circ}C$ the specific contact resistance increased due to the decomposition of GaAs substrate.

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