• Title/Summary/Keyword: 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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    • v.14 no.3
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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

  • Gang, Yu-Jin;Park, Ju-Yeon;Kim, Dong-U;Kim, Hak-Jun;Gang, Yong-Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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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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Characterization of PSCF3737 for intermediate temperature solid oxide fuel cell (IT-SOFC) (중.저온형 고체 산화물 연료전지의 공기극으로 사용되는 PSCF3737 물질의 특성에 관한 연구)

  • Park, Kwang-Jin;Bae, Joong-Myeon
    • 한국신재생에너지학회:학술대회논문집
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    • 2008.05a
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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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Characterizations of Thermal Compound Using CuO Particles Grown by Wet Oxidation Method (습식 산화법으로 성장된 산화구리입자를 이용한 방열 컴파운드 제조 및 특성 연구)

  • Lee, Dong Woo;Um, Chang Hyun;Chu, Jae Uk
    • Korean Journal of Materials Research
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    • v.27 no.4
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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.

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

  • 김인기;최상흘;고영신
    • Journal of the Korean Ceramic Society
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    • v.30 no.10
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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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Microsturucture of pottery by the measurement of firing temperature (토기의 소성온도에 따른 미세조직 비교연구)

  • Hong, Jong-Ouk;Jung, Kwang-Yong
    • 보존과학연구
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    • s.15
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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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A Study on Hydration of Slag-Gypsum System (슬래그-석고계 수화반응에 대한 기초 연구)

  • 지정식;최상흘
    • Journal of the Korean Ceramic Society
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    • v.15 no.4
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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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Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders (기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화)

  • 이충효;전성용;김지순
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.4
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    • pp.129-134
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    • 2004
  • In this study, we investigated the effect of a nitrogen atom on the amorphization of V-Fe alloy through solid-gas reaction during mechanical alloying (MA). MA by planetary ball mill of $V_{70}Fe_{30}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed after 160 hours of ball milling in this case. The DSC spectrum for the mechanically alloyed ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ powders exhibits a sharp exothermic peak due to crystallization at about $600^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was also observed through X-ray and neutron diffractions. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is selectively situated at a center of the polyhedron formed by V atoms.

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

  • Han, Chang-Suk;Kwon, Yong-Jun
    • Korean Journal of Materials Research
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    • v.31 no.12
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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.

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

  • 정성훈;송복식;문동찬;김선태
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1995.11a
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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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