• Title/Summary/Keyword: X-선 구조분석

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The Crystal Structure of Tris(ethylenediamine)nickel(II)-dichromate, $[Ni(C_2N_2H_8)_3]\cdotCr_2O_7$ ($[Ni(C_2N_2H_8)_3]\cdotCr_2O_7$의 결정구조)

  • Kim, Se-Hwan;Kim, Seung-Bin;Nam, Gung-Hae
    • Korean Journal of Crystallography
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    • v.7 no.1
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    • pp.36-43
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    • 1996
  • The crystal structure Tris(ethylenediamine)nickel(II)Dichromate has been determined by X-ray crystallography. Crystal data: a=8.268(2), b=13.865(2), c=14.921(2)Å, γ=102.04(2)°, V=1672.9(5)Å3, Z=4, Monocline, P21/b (space group No.=14), Dcalc=1.806 gcm-3, μ=24.05 cm-0.1. The intensity data were collected with Mo-Kα radiation(λ=0.7107Å) on an automatic four-circle diffractometer with a graphite monochromator. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were R=0.045, Rw=0.051, Rall=0.059 and S=2.171for 2248 observed reflections. The two carbon atoms of a ring of Ni(en)-ion were split into crossed four atoms. In consideration of α- and β-angles of two rings of a disordered ethylenediamine of Nien3-ion and the hydrogen bonds between Ni(en)3-cation and Cr2O7-anion, the configuration of Ni(en)3-ion is assumed to be disordered with Λδδδ and Λδδλ.

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A study of semi-quantification of the Friedel's salt using the X-ray diffraction method in concrete (콘크리트 내 Friedel염의 XRD를 이용한 반정량적 측정기법에 관한 연구)

  • Lee, Ho-Jae;Lee, Jang-Hwa;Kim, Do-Gyeum
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.33-38
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    • 2012
  • Despite the importance of chloride binding, it is very difficult to measure the binding capacity, in particular, for the concrete body in an existing structure: in fact, the measurement procedure for chloride binding is much influenced by the environmental condition such as temperature, fineness of sample and pore water extraction techniques. The present study concerns the quantification of the binding capacity of chloride ions in concrete using the X-ray diffraction (XRD) technique. Once the binding isotherm of chlorides was determined by the Langmuir isotherm, as a function of the W/C, curing age and binder type, the generation of bound chlorides (i.e. Friedel's salt) was simultaneously ensured by the XRD technique. The amount of bound chloride was then determined by analyzing the peak intensity for the bound chlorides in the XRD curve. It was found that an increase in the curing age and a decrease in the W/C resulted in an increase in the binding capacity.

Growth and Magnetic Properties of $Y_{3-x}La_xFe_5O_{12}(0.0{\le}X{\le}1.0)$ Powders and Thin Films by a Sol-Gel Method (Sol-Gel 법에 의한 $Y_{3-x}La_xFe_5O_{12}(0.0{\le}X{\le}1.0)$ 분말과 박막의 합성 및 자기적 특성에 관한 연구)

  • 엄영랑;김철성;임연수;이재광
    • Journal of the Korean Magnetics Society
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    • v.8 no.6
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    • pp.350-356
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    • 1998
  • $Y_{3-x}La_xFe_5O_{12}$ (x=0.0, 0.25, 0.5, 0.75, 1.0) powders and thin films were fabricated by a sol-gel method and their magnetic properties and crystal structure were investigated by using X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), and Mossbauer spectroscopy. XRD and Mossbauer spectroscopy measurements show that garnet powders annealed at 900 $^{\circ}C$ for 8 hours were single-phased and that thin films fired at 800 $^{\circ}C$ for 2 hours were crystallized without any preferred direction. X-ray diffraction patterns of $Y_{3-x}La_xFe_5O_{12}$ powders annealed at 1000 $^{\circ}C$ had only peaks of the garnet structure in case of x$\leq$0.75 but those of $Y_2LaFe_5O_{12}$ powders consisted of peaks from garnets and $LaFeO_3$. Mossbauer sepectra of garnet powders grown by the sol-gel method had a similar shape of those of powders grown by a conventional ceramic method. Grain sizes of garnet powders were 200~300 nm and the averaged surface roughness was 3.17 nm. Results of VSM measurements show the powders and thin films had soft magnetic properties and that the garnet powders had the largest saturation magnetization, 30 emu/g, and the lowest coercivity, 52 Oe.

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A Study on Nonstoichiometry and Physical Properties of the Mixed Valency $Sr_{1+x}Dy_{1-x}FeO_{4-y}$Ferrite System (혼합원자가 $Sr_{1+x}Dy_{1-x}FeO_{4-y}$훼라이트계의 비화학양론과 물성 연구)

  • Chul Hyun Yo;Eun Seok Lee;Woong Bum Pyon;Moo Sil Pyon
    • Journal of the Korean Chemical Society
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    • v.32 no.1
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    • pp.3-8
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    • 1988
  • Nonstoichiometric solid solutions of the $Sr_{1+x}Dy_{1-x}FeO_{4-y}$ system (x = 0. 00, 0. 25, 0. 50, 0. 75 and 1. 00) with layered $K-2NiF_4$ type structure were prepared at 1200$^{\circ}$C under atmospheric pressure. X-ray powder diffraction spectra show that the crystallographic phases of the samples are tetragonal within the x range. Nonstoichiometric chemical formulas have been determined by Mohr salt analysis and it shows that the amount of $Fe^{4+}$ ion or ${\tau}$ value increases with increasing x. Electrical conductivities of the samples which were measured in the temperature range of $-100{\sim}200^{\circ}$C under atmospheric air pressure are varied within the semiconductivity range of $l0^{-8}{\sim}10^{-2}(ohm^{-1}{\cdot}cm^{-1}$) and the activation energies are also varied from 0.02 to 0.08 eV. Mixed valency state of $Fe^{3+}$ and $Fe^{4+}$ in the sample of $Sr_{1.00}Dy_{1.00}FeO_{4.04}$ was identified again by Mossbauer spectrum at 200K.

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Neutron Capture Resonance Energy Identification of Indium by Time-of-Flight Method (중성자 비행시간법을 이용한 인듐의 공명에너지 동정에 관한 연구)

  • Lee, Sam-Yol
    • Journal of the Korean Society of Radiology
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    • v.6 no.5
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    • pp.403-408
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    • 2012
  • Prompt gamma ray from the natural Indium sample was measured by using an assembly of BGO($Bi_4Ge_3O_{12}$) scintillation detectors in the neutron energy region from 1 to 300 eV. The assembly was composed of pieces of BGO. The spectrometer was composed geometrically as total energy absorption detector. 46-MeV electron linear accelerator which is located at Research Reactor Institute, Kyoto University used for neutron sources from photonuclear reaction. The measurement of the neutron capture resonances was performed to below neutron energy 1 keV, because of strong X-ray effect from photonuclear reaction in Ta target and short distance from the target to an assembly of detector. The distance of neutron flight path is $12.7{\pm}0.02m$. The large neutron capture resonances were measured from 1 to 400 eV. The energy in the capture resonance was compared with the evaluated values. The large resonances were seen in the present measurement. General agreement can be seen between the present measurement and the previous evaluated data in relevant energy region. In the present study, we measured the continues resonance structure above 1 keV neutron energy region. 91.49 eV new neutron capture resonance was found in present measurement.

A Study of EPMA Analysis for Nitric Acid Insoluble Alloys (질산불용성 합금의 EPMA분석)

  • Park, Soon-Dal;Park, Yong-Joon;Kim, Jong-Goo;Son, Se-Chul;Joe, Kih-Soo
    • Analytical Science and Technology
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    • v.11 no.6
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    • pp.485-494
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    • 1998
  • Ternary and quaternary alloys composed of Mo-Ru-Rh-Pd were prepared and their crystal structure and quantitative chemical compositions were analysed by XRD, WDX, EDX and ICP/AES. The results of X-ray diffraction studies showed that the alloys were crystallized in hexagonal close packing, well known as ${\varepsilon}$-phase with $P6_3/mmc$ of space group. The optimum accelerating voltage for Zr~Cd(40~48) analyzed by EPMA using PET crystal was found to be 15 kV and the linear regression coefficient(R) of atomic number and X-ray intensity was approximately 0.998 without Tc standard specimen. The WDX results of alloys of Mo and Pd by linear regression equations were detected to be 0.1% lower compared to WDX analysis results using standard specimen, while Ru, Rh were detected 3% higher. These alloys were completely dissolved in mixed acid of 12.5 mL HCl and 1 mL $HNO_3$, at $220^{\circ}C$ for 22 hours using autoclave with PTFE vessel. There was no reprecipitating phenomnon when diluted 100 times with 1N-HCl. The results of ICP/AES analysis deviated less than 4% comparing with those of normal WDX analysis.

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Effects of ${\gamma}$-Ray Irradiation on the Color of Pearl Nucleus (감마선 (Co-60) 조사에 의한 진주 핵의 영향)

  • Kim, Hea-Yeon;Min, Bong-Ki;Jeong, Woo-Geon
    • The Korean Journal of Malacology
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    • v.27 no.3
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    • pp.247-252
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    • 2011
  • The effect of ${\gamma}$-ray irradiation on the color of nucleus and cultured pearls was investigated. After ($^{60}Co$) ${\gamma}$-ray irradiation on the pearl nucleus, its color was altered from brownish to blackish brown or gray depending on irradiation dose. It was clearly found that the all samples are composed of aragonite. ESR spectra were based on the measurement of the paramagnetic species $CO_2$-radicals by the interaction with the ${\gamma}$-ray irradiation in $Mn^{2+}$ containing $CaCO_3$. In this study, we investigated optimal detection method of ${\gamma}$-ray irradiation to establish destructive or non-destructive test for pearl nucleus.

The relation of structural transition, thermal and electrical stability deintercalation of Li- CICs(II) : For Li-EaGDICs and Li-EGDICs (Li-CICs의 Deintercalation에 따른 구조변이와 열적, 전기적 안정성과의 관계(II) : Li-EaGDICs와 Li-EGDICs에 관하여)

  • Oh, Won-Chun;Park, Chung-Oh;Back, Dae-Jin;Ko, Young-Shin
    • Analytical Science and Technology
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    • v.9 no.1
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    • pp.43-51
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    • 1996
  • We have discussed on the deintercalation process of Li-EaGICs and Li-EGICs synthesized under pressure and temperature by spontaneous oxidation reaction of those compounds based on the results of X-ray diffraction, thermal analysis and electrical specific resistivity analysis. According to the results of the X-ray analysis for the intercalation process, we have found that the stage 1 for Li-EaGICs and Li-EGICs were not completly formed, but their lower stages were formed mainly. And from this results of the deintercalation process, we have found that the deintercalation process did not occur any more after 4 weeks, and the Li-EGDICs have more residual lithium metals than LiEaGDICs between the graphite interlayers. According to the thermal decomposition analysis, Li-two compounds had included very hard exothermic reaction. And we have found that these compounds did not occrurred deintercalation reaction above $400^{\circ}C$. According to the results of the electrical specific resistivity measurements, Li-EGDICs have relatively lower electrical specific resistivity than Li-EaGDICs, and Li-EaGDICs showed a formation of the ideal curve. From these results, we can suggest that Li-EaGDICs have a better properties as an anode material secondary than Li-EGICs.

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The studies of Structure and Ferromagnetism on Co doped ZnO powders (자성반도체 Co-doped ZnO 다결정계의 구조 및 강자성 특성)

  • 박정환;장현명;김민규
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.176-176
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    • 2003
  • 강자성 반도체(DMS)는 반도체에 전이금속을 doping함으로써 반도체의 전자 수송 특성과 전이 금속 이온에 의한 자기적 특성을 동시에 발현할 수 있도록 설계된 물질로서 '스핀 전자공학'의 구현을 위해 현재 활발히 연구되고 있는 분야이다. 특히 높은 전기 전도도와 투명 광 특성을 가지는 ZnO계는 전이금속을 첨가 할 경우 상온에서도 강자성 특성을 보일 것이라는 연구가 발표 된 이후 큰 주목을 받고 있으며, 실제로 Tc가 상온 이상인 결과들이 최근 발표되고 있다. 그러나 PLD에 의해 증착 된 Co-doped ZnO 경우 강자성 물성의 재현성이 아주 낮은 것으로 알려져 있는 둥 강자성 발현의 기원이 아직도 명확히 규명되지 못한 상태이다. 이에 본 연구에서는 Co-doped ZnO 계의 강자성 발현의 기원을 밝히고자 고상 반응법을 이용하여 다결정계를 제조한 후 X-선 회절 분석과 Raman 분광법을 이용하여 제2차상의 존재 유무 및 Co 이온의 치환 정도를 분석하였다. 다음으로 방사광 EXAFS 분석을 행하여 ZnO내에서의 Co 이온의 원자가 상태를 분석하고, PPMS를 사용 M-T curve를 측정/분석함으로써 강자성 발현의 기원을 규명하고자 하였다.

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The Study of Formation of Ti-silicide deposited with Composite Target [II] (Composite Target으로 증착된 Ti-silicide의 현성에 관한 연구[II])

  • Choi, Jin-Seog;Paek, Su-Hyon;Song, Young-Sik;Sim, Tae-Un;Lee, Jong-Gil
    • Korean Journal of Materials Research
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    • v.1 no.4
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    • pp.191-197
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    • 1991
  • The surface roughnesses of titanium silicide films and the diffusion behaviours of dopants in single crystal and polycrystalline silicon substrates durng titanium silicide formation by rapid thermal annealing(RTA) of sputter deposited Ti-filicide film from the composite $TiSi_{2.6}$ target were investigated by the secondary ion mass spectrometry(SIMS), a four-point probe, X-ray diffraction, and surface roughness measurements. The as-deposited films were amorphous but film prepared on single silicon substrate crystallized to the orthorhombic $TiSi_2$(C54 structure) upon rapid thermal annealing(RTA) at $800^{\circ}C$ for 20sec. There was no significant out-diffusion of dopants from both single crystal and polycrystalline silicon substrate into titanum silicide layers during annealing. Most of the implanted dopants piled up near the titanium silicide/silicon interface. The surface roughnesses of titanium silicide films were in the range between 16 and 22nm.

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