• Title/Summary/Keyword: Crystal EPR

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Synthesis of Iminoxyl Biradical and the Spectroscopic Study (Iminoxyl Biradical의 합성과 분광학적인 연구)

  • Jung-Sung Yang;Hee Ju Chae;Chul-Hyun Yo
    • Journal of the Korean Chemical Society
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    • v.25 no.1
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    • pp.13-20
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    • 1981
  • Iminoxyl biradical may be useful biradical spin probe for the investigation of the dynamic distribution of the directors in some liquid crystal. The iminoxyl biradical has been synthesized by a new convenient method and the intermediate products of each step were identified by the measurement of melting point and spectroscopic methods such as IR, UV, NMR and Mass spectrometry. The final product, iminoxyl biradical, was identified by the electron paramagnetic resonance spectroscopy and the interaction between two spins of the radical was discussed based on the EPR peaks.

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Thermal Effects on Stoichiometric LiTaO3 Single Crystal (정비조성 LiTaO3 단결정에 대한 열처리 효과)

  • Yeom, T.H.;Lee, S.H.
    • Journal of the Korean Magnetics Society
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    • v.15 no.3
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    • pp.177-180
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    • 2005
  • Ferroelectric $LiTaO_3$ single crystals, grown by the Czochralski method, were thermally treated at temperature $1000^{\circ}C\;and\;1100^{\circ}C$. Electron paramagnetic resonance (EPR) study of stoichiometric $LiTaO_3$ and thermally treated $LiTaO_3$ crystals has been investigated by employing an X-band spectrometer. From the $Fe^{3+}$ EPR spectra, it turned out that there is no change of site location and local site symmetry around $Fe^{3+}$ impurity ion between stoichiometric and thermally treated $LiTaO_3$ single crystals. We confirmed that the ionic state of $Fe^{3+}$ ion changed after thermal treatment. The EPR parameters of $Fe^{3+}$ ion in $LiTaO_3$ single crystals are determined with effective spin Hamiltonian.

Preparation and characterization of nearly stoichiometric $LiNbO_3$ crystals by VTE method (VTE법에 의한 nearly stoichiometric $LiNbO_3$의 성장 및 특성)

  • 김상수;유동선
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.1
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    • pp.6-17
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    • 1997
  • Lithium niobate single crystals with various [Li]/[Nb] ratios were grown by the Czochralski method from melts having compositions varing between 48.6 ~ 58.0 mol % $Li_2O$. A vapor transport equilibration technique has been used to improve the homogeneity and adjust the [Li]/[Nb] ratio in small $LiNbO_3$ single crystals grown by the Czochralski method. When equilibrated with a Li-rich powder (65 mol%$Li_2O$), containing a mixture of $LiNbO_3$ and $Li_3NbO_4$, crystals of nearly stoichiometric composition can be obtained. This was established by studying the composition dependence of the following properties; lineshape, intensity and linewidth for the electron paramagnetic resonance (EPR) of $Fe^{3+}$ energy of the fundamental absorption edge and $OH^-$ absorption spectra.

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ESR Study on Paramagnetic Defects of the $gamma$-irradiated Ammonium Sulfate Single Crystal (${\gamma}$-선에 조사된 황산 암모늄 단결정의 상자성 결함에 관한 전자스핀공명 연구)

  • Yo Chul Hyun;Kim Eun Ok
    • Journal of the Korean Chemical Society
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    • v.29 no.2
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    • pp.80-87
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    • 1985
  • Radiation damage in a single crystal of ammonium sulfate caused by ${\gamma}$-irradiation at room temperature has given rise to several paramagnetic centers. Electron spin resonance (ESR) spectra of crystal are obtained with the X-band EPR spectrometer at room temperature. An intense and isotropic peak of Gaussian shape at g = 2.0036 is assigned to $SO_3^-$, which shows power saturation effects. Angular dependence of spectra is studied for the rotations about three mutually perpendicular axes a, b and c. The g-values are obtained from the relative distances between isotropic peak of $SO_3^-$ and anisotropic peak of the species. Principal $g^-$values and direction cosines were calculated by diagonalizing the 3${\times}$3 matrix whose elements are the $g^-$values for each species. From the analysis of characteristic principal $g^-$values and direction cosines for ammonium sulfate single crystal, anisotropic peaks corresponding to $SO_4^-,\;SO_2^-$ and defect structure corresponding to electron excess type are identified.

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Effect of VO(II) Doping on Structural and Optical Properties of Diaquamalonato(1,10-phenanthroline)zinc(II)

  • Hema, Ramesh;Parthipan, Krishnan;Ramachitra, Somasundaram;Balaji, Subramanian
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3547-3552
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    • 2013
  • Single crystal EPR and optical studies of a mixed ligand zinc(II) complex doped with VO(II) ion is carried out to establish the structural properties. The angular variation of vanadyl hyperfine lines indicates a single site, with spin Hamiltonian parameters as: $g_{xx}=1.985$, $g_{yy}=1.979$, $g_{zz}=1.943$; $A_{xx}=8.71$, $A_{yy}=6.41$ and $A_{zz}=17.80$ mT. By comparing the direction cosines of principal g and A values with the direction cosines of metalligand bonds, it has been confirmed that the vanadyl ion has entered the lattice interstitially. The exact interstitial position of VO(II) in host lattice has been calculated using the fractional coordinates of atoms in the host lattice out of many assumptions. The EPR and optical data have been confirmed to obtain various bonding parameters, from which the nature of the bonding in the complex is discussed. FT-IR confirms the formation of structure of host lattice.

The pH Effect on the Preparation of MFI Type Ferrisilicate Zeolites

  • 염영훈;남상성;김성보;이규완
    • Bulletin of the Korean Chemical Society
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    • v.20 no.7
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    • pp.781-785
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    • 1999
  • Ferrisilicates with MFI type structure were hydrothermally synthesized. The structural environments of iron in the ferrisilicates were characterized by XRD, SEM, IR, EPR, and ammonia-TPD. It has been shown that pH of the final gel mixture during the synthesis affects the crystal size, morphology, chemical composition and catalyticactivity. The results of the lattice parameters, IR, and EPR indicate the existence of a framework iron and the content of framework iron depends on pH of the synthesis gel. Finally, the catalytic activity of these zeolites was examined for the cyclohexane oxidation to cyclohexanol and cyclohexanone in the liquid phase. The conversion of this reaction was increased with increasing iron content of the framework lattice positions.

Electron Paramagnetic Resonance Study of impurity Fe3+ ion in LiTaO3 single crystal (Fe3+ 불순물이 첨가된 LiTaO3 단결정에서의 전자 상자성 공명 연구)

  • Min, S.G.;Yeon, T.H.;Lee, S.H.;Lee, M.K.;Shin, H.K.;Yu, Y.M.;Kim, T.H.;Yu, S.C.
    • Journal of the Korean Magnetics Society
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    • v.13 no.4
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    • pp.171-175
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    • 2003
  • Electron paramagnetic resonance (EPR) of Fe$^{3+}$ in LiTaO$_3$ single crystal, grown by Czochralski method, has been studied by employing an X-band spectrometer. Resonance spectra of Fe$^{3+}$ ion on the crystallographic principal axes were obtained with 9.447 ㎓ at room temperature. The spectroscopic splitting parameter g and zero-field splitting (ZFS) parameter D (= 3 B$_{2}$sup 0/) are calculated with effective spin Hamiltonian. Fe$^{3+}$ center in stoichometric single crystal turns out to be different with that in congruent single crystal reported previously. From the analysis of temperature dependence of resonance fields for Fe$^{3+}$ ion, there is no any phase transition at the temperature range (from -160 $^{\circ}C$ to 20 $^{\circ}C$).

Synthesis, Structure, and Peroxidase Activity of an Octahedral Ru(III) Complex with a Tripodal Tetraamine Ligand

  • Cho, Jang-Hoon;Kim, Kwan-Mook;Noh, Dong-Youn;Lee, Hong-In
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.3904-3908
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    • 2011
  • A new octahedral Ru(III) complex with a tripodal tetraamine ligand, tpea = tris[2-(1-pyrazoyl)ethyl]amine, has been prepared and characterized. The single crystal X-ray crystallographic study of the complex revealed that the complex has a near octahedral geometry with the tetradentate ligand and two chloride ions. Peroxidase activity was examined by observing the oxidation of 2,2'-azinobis(3-ethylbenzothiazoline)-6-sulfonic acid (ABTS) with hydrogen peroxide in the presence of the complex. Amount of $ABTS^{+{\bullet}}$ generated during the reaction was monitored by UV/VIS and EPR spectroscopies. After the initiation of the peroxidase reaction, $ABTS^{+{\bullet}}$ concentration increases and then decreases after certain time, indicating that both ABTS and $ABTS^{+{\bullet}}$ are the substrates of the peroxidase activity of the Ru(III) complex.

Magneto-optical Properties of 55Mn-doped SrTiO3 Single Crystal (55Mn이 첨가된 SrTiO3 단 결정의 광 전이 특성연구)

  • Bae, Kyu-Chan;Park, Jung-Il;Lee, Hyeong-Rag
    • Journal of the Korean Magnetics Society
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    • v.21 no.6
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    • pp.208-213
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    • 2011
  • We calculated the EPR (electron paramagnetic resonance) line-shape function. The line-widths of a -doped single crystal was studied as a function of the temperature with 0.5 and 2 at. at a frequency of (X-band). The line-width decreases with increasing temperature, such temperature behavior of the line-width can indicate a motional narrowing of the spectrum, when impurity ions substitute for host ions in an off-center position, and thus there can be fast jumping of dipoles between several symmetrically equivalent configurations. Therefore, the present technique is considered to be more convenient to explain the resonant system as in the case of other optical transition problems.

Synthesis and Characterization of Paramagnetic Copper(Ⅱ) Complexes (상자성 구리(Ⅱ) 화합물의 합성과 그 특성 연구)

  • Oh, Yeong-Hee
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.507-512
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    • 2000
  • A new copper(II) complex, Cu(dpb)(NO$_3$)$_2$(H$_2$O) (dpb=2,2'-dipyridylbenzylamine) (1) was synthesized from the reaction of Cu(NO$_3$)$_2$·3H$_2$O and dpb in ethanol solution followed by recrystallization in acetonitrile. The structure of 1 was determined by X-ray diffraction methods. The single crystal structure was characterized as follows: space group P2$_1$/c, Z=4, a=12.501(9)$\AA$, b=9.231(10)$\AA$, c=17.119(6)$\AA$, $\alpha$=90$^{\circ}$, $\beta$=107.33(4)$^{\circ}$, $\gamma$=90$^{\circ}$, V=1885.8(2)$\AA^3$, R$_1$=0.0647, $_{w}R$_2$$=0.1866 for 3258 reflections. Compound was a typical paramagnetic copper(II) complex coordinated by 2,2'-dipyridylamine derivative ligand, which was confirmed by EPR, NMR, UV/VIS, and IR spectroscopy.

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