• Journal of the Korean Magnetics Society
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• v.6 no.2
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• pp.67-72
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• 1996

The crystallographic and magnetic properties of the ferrimagnetic $CoFe_2O_4$ have been studied by X-ray and Mossbauer measurements. The crystal structure is found to be cubic spinel structure with the lattice constant $a_{0}=8.381{\pm}0.005{\AA}\;and\;a_{0}=8.391{\pm}0.005{\AA}$ for slow-cooled and quenched CoFeZ04' respectively. Mossbauer spectra of $CoFe_2O_4$ have been taken at various temperatures ranging from 13 to 780 K. The isorrer shifts indicate that the valence states of the Fe ions for tetrahedral(A) and octahedral(B) sites have ferric character. Debye temperatures for the A and B sites are found to be ${\theta}_A=734{\pm}5K\;and\;{\theta}_B=248{\pm}5K$ for slow-cooled and ${\theta}_A=531{\pm}5K\;and\;{\theta}_B=197{\pm}5K$ for quenched, respectively. Atomic migration from the A to the B sites starts near 400 K and 350 K for slow-cooled and quenched $CoFe_2O_4$, respectively, am increases rapidly with increasing temperature to such a degree that about 69 % for slow-cooled and 91 % for quenched of the ferric ions on the A sites have rmved over to the B sites at 700 K.

• Journal of the Korean Magnetics Society
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• v.26 no.6
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• pp.185-189
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• 2016

By employing photoemission spectroscopy (PES) and soft X-ray absorption spectroscopy (XAS), the electronic structure of the candidate half-metallic antiferromagnet of $Mn_3Ga$ Heusler compound has been investigated. We have studied two ball-milled $Mn_3Ga$ powder samples, one after annealing and the other without annealing, respectively. Based on the Mn 2p XAS study, we have found that Mn ions are nearly divalent in $Mn_3Ga$ and that the Mn ions having the locally octahedral symmetry and those having the locally tetrahedral symmetry are both present in $Mn_3Ga$. We have found relatively good agreement between the measured valence-band PES spectrum of $Mn_3Ga$ and the calculated density of states, which is in agreement with the half-metallic electronic structure of $Mn_3Ga$.

• Journal of the Korean Chemical Society
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• v.50 no.4
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• pp.315-320
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• 2006

manganese oxides have been prepared by Chimie Douce redox reaction between permanganate and chalcogen element fine powder under acidic condition (pH = 1). According to powder X-ray diffraction analyses, the S- and Se-doped manganese oxides are crystallized with layered birnessite and tunnel-type -MnO2 structures, respectively. On the contrary, Te-doped compound was found to be X-ray amorphous. According to EDS analyses, these compounds contain chalcogen dopants with the ratio of chalcogen/manganese = 4-7%. We have investigated the chemical bonding character of these materials with X-ray absorption spectroscopic (XAS) analysis. Mn K-edge XAS results clearly demonstrated that the manganese ions are stabilized in octahedral symmetry with the mixed oxidation states of +3/+4. On the other hand, according to Se K- and Te L1-edge XAS results, selenium and tellurium elements have the high oxidation states of +6, which is surely due to the oxidation of neutral chalcogen element by the strong oxidant permanganate ion. Taking into account their crystal structures and Mn oxidation states, the obtained manganese oxides are expected to be applicable as electrode materials for lithium secondary batteries.

• Journal of the Korean Chemical Society
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• v.36 no.6
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• pp.872-878
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• 1992

Some vanadium(III) complexes have been prepared by the reaction of VCl3${\cdot}$3MeCN with ligands and characterized by elemental analysis, 1H-NMR, infrared and UV-Visible spectroscopy. 3,5-lutidine(lutd), 8-hydroxyquinoline(oxine), 1,2-phenylenediamine(phda), ethylenediamine(en), and sym-diphenylethylenediamine(dpen) were chosen as coordinating ligands. ${\nu}$(V-Cl) of lutidine complex occurs at 418 $cm^{-1}$ and the other complexes (oxine, phda, en, dpen) occur at 337∼347 $cm^{-1}$. The value of ${\nu}$(V-Cl) indicates that the former complex has trigonal bipyramid structure and the latter complexes have octahedral structure. The ${\nu}$(C${\equiv}$N) of acetonitrile in oxine and phda complexes are characteristically shifted to about 70 $cm^{-1}$ higher frequency compared with that of free ligand (2260 $cm^{-1}$). The ${\delta}$(C${\equiv}$N) is also shifted to about 60 $cm^{-1}$ higher frequency compared with that of free ligand (377 $cm^{-1}$). Finally each vanadium(III) complex showed the following formulation; [$VCl_3(lutd)_2$], [$VCl(oxine)_2$MeCN]$Cl_2$, [$VCl(phda)_2$MeCN]$Cl_2$, [$VCl_2(en)_2$]Cl, [$VCl_2(dpen)_2$]Cl.

• Economic and Environmental Geology
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• v.49 no.2
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• pp.77-88
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• 2016

Chrysotile is a 1:1 sheet silicate mineral belonging to serpentine group. It has been highlighted studies because of uses, shapes and structural characteristics of the fibrous chrysotile. However, it was designated as Class 1 carcinogen, so high attentions were being placed on detoxification studies of chrysotile. The objectives of this study were to investigate changes of mineralogical characteristics of chrysotile and to suggest detoxification mechanism of chrysotile by thermal decomposition. Samples for this study were obtained from LAB Chrysotile mine in Canada. The samples were heated in air in the range of 600 to $1,300^{\circ}C$. Changes of mineralogical characteristics such as crystal structure, shape, and chemical composition of the chrysotile fibers were examined by TG-DTA, XRD, FT-IR, TEM-EDS and SEM-EDS analyses. As a result of thermal decomposition, the fibrous chrysotile having hollow tube structure was dehydroxylated at $600-650^{\circ}C$ and transformed to disordered chrysotile by removal of OH at the octahedral sheet (MgOH) (Dehydroxylation 1). Upon increasing temperature, it was transformed to forsterite ($Mg_2SiO_4$) at $820^{\circ}C$ by rearrangement of Mg, Si and O (Dehydroxylation 2). In addition, crystal structure of forsterite had begun to transform at $800^{\circ}C$, and gradually grown 3-dimensionally to enstatite ($MgSiO_3$) by recrystallization after the heating above $1,100^{\circ}C$. And then finally transformed to spherical minerals. This study showed chrysotile structure was collapsed about $600-700^{\circ}C$ by dehydroxylation. And then the fibrous chrysotile was transformed to forsterite and enstatite, as non-hazardous minerals. Therefore, this study indicates heat treatment can be used to detoxification of chrysotile.

• Journal of the Korean Magnetics Society
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• v.12 no.1
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• pp.1-6
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• 2002

Al$\^$3+/ substituted garnet Y$_3$Fe$\_$5-x/Al$\_$x/O$\_$12/ (x=0.0, 0.25, 0.5, 0.75, 1.0) was fabricated by sol-gel method. The crystallographic and magnetic properties of Y$_3$Fe$\_$5-x/Al$\_$x/O$\_$12/ have been studied with Mossbauer spectroscopy, x-ray diffraction (XRD), thermogravimetry analysis (TGA), differential thermal analysis (DTA), and vibrating samples magnetometer (VSM). The crystal structure of Y$_3$Fe$\_$5/O$\_$12/ is found to be a cubic with the lattice constant a$\_$0/= 12.381$\pm$0.005 $\AA$. The lattice constants a$\_$0/ decreases linearly from 12.381 to 12.304 A as the Al concentration (x) increases from x=0.0 to 1.0. Mossbauer spectra of measured at Y$_3$Fe$\_$5-x/A1$\_$x/O$\_$12/ various absorber temperatures of 13 to 600 K. Mossbauer spectrum for x = 0.0 is consist of well resolved two sets of six line patterns. While with increasing Al concentration outer sextet patters, which is originating from octahedral sites, broadens widely. These phenomena are interpreted in terms of random probability distributions of Fe$\^$3+/ and Al$\^$3+/ in tetrahedral site.

• Journal of the Korean Chemical Society
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• v.63 no.6
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• pp.453-458
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• 2019

Synthesis of ZnCo₂O₃ oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P_2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo₂O₃. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O₂ in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at g_iso ~2.230 and g_iso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co²⁺(3d⁷) in the oxide. DC conductivity value of 2.875 ×10^-8 S/cm indicates very weakly semiconducting nature of ZnCo₂O₃ at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions ⁴T_1g(⁴F)→²E_g(²G), ⁴T_1g(⁴F)→⁴T_1g(⁴P), ⁴T_1g(⁴F)→⁴A_2g(⁴F), ⁴T_1g(⁴F)→⁴T_2g(⁴F), respectively in octahedral ligand field around Co²⁺ ions. Direct band gap energy, E_g~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo₂O₃.

• Analytical Science and Technology
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• v.12 no.5
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• pp.421-427
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• 1999

Two shapes of crystals have been isolated by the interdiffusion of $Co(NCS)_2$ dissolved in methanol with 1,2-bis(2,2'-bipyridyl-6-yl)ethane (bbpe) dissolved in chloroform. The two crystals have been elucidated as $trans-Co^{II}(NCS)_2(bbpe)$ and $trans-Co^{II}(NCS)_2(bbpe){\cdot}2CHCl_3$, by X-ray crystallography, elemental analysis, IR, and thermal analysis. The two molecular structures are very similar except for the absence or presence of chloroform solvate molecules. The bbpe ligand coordinates to the cobalt(II) ion in an open-ended tetradentate mode, resulting in discrete mononuclear cobalt(II) complex. The cobalt atom adopts a typical octahedral arrangement with six nitrogen donating atoms with two NCS groups in trans positions. A significant solid-to-solid phase transition occurs presumably due to the change of conformationally flexible bbpe ligand. The formation of both crystals oeeurs in a successive two-step process, the formation of $trans-Co^{II}(NCS)_2(bbpe)$ and its transformation into $trans-Co^{II}(NCS)_2(bbpe){\cdot}2CHCl_3$. The thermal stability and favorable formation of the solvate crystals may be ascribed to the interaction between S atom of NCS group and Cl of chloroform.

• Journal of the Korean Society for Heat Treatment
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• v.19 no.1
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• pp.10-19
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• 2006

Microstructure and morphology of precipitates in $Ni_3Al$- and TiAl-based intermetallics containing carbon have been investigated in terms of transmission electron microscopy(TEM). In an $L1_2$-ordered $Ni_3Al$ alloy with 4 mol.% of chromium and 0.2~3.0 mol.% of carbon, fine octahedral precipitates of $M_{23}C_6$ type carbide were formed in the matrix by aging at temperatures around 973 K after solution annealing at 1423 K. TEM examination revealed that the $M_{23}C_6$ phase and the matrix lattices have a cube-cube orientation relationship and keep partial atomic matching at the {111} interface. After prolonged aging or by aging at higher temperatures, the $M_{23}C_6$ precipitates then adopt a rod-like morphology elongated parallel to the <100> directions. In the $L1_0$-ordered TiAl containing 0.1~2.0 mol.% carbon, TEM observations revealed that needle-like precipitates, which lie only in one direction parallel to the [001] axis of the $L1_0$ matrix, appear in the matrix and preferentially at dislocations. Selected area electron diffraction(SAED) patterns analyses have shown that the needle-shaped precipitate is $Ti_3AlC$ of perovskite type. The orientation relationship between the $Ti_3AlC$ and the $L1_0$ matrix is found to be $(001)_{Ti3AlC}//(001)_{L10\;matrix}$ and $[010]_{Ti3AlC}//[010]_{L10\;matrix}$. By aging at higher temperatures or for longer period at 1073 K, plate-like precipitates of $Ti_2AlC$ with a hexagonal structure are formed on the {111} planes of the $L1_0$ matrix. The orientation relationship between the $Ti_2AlC$ and the $L1_0$ matrix is $(0001)_{Ti2AlC}//(111)_{L10\;matrix}$ and $_{Ti2AlC}//_{L10\;matrix}$.

• Journal of the Korean Chemical Society
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• v.35 no.6
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• pp.645-652
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• 1991

The stability constants$(K_f)$ of the complexes of some transition and post-transition metal ions (Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ), Zn(Ⅱ), Cd(Ⅱ), Pb(Ⅱ), Hg(Ⅱ)) with $N_2O_3$-donor macrocyclic ligand, 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane ($NtnOdienH_4$), have been determined by potentiometry in aqueous solution at $25^{\circ}C$. Log $K_f$ values of the complexes were : Co(Ⅱ): 3.83, Ni(Ⅱ) : 4.56, Cu(Ⅱ) : 7.74, Zn(Ⅱ) : 4.98, Cd(Ⅱ) : 3.91, Pb(Ⅱ) : 6.65, and Hg(Ⅱ) : 14.87. The order of stabilities of transition metal complexes was the same as the natural order of stability proposed by Williams-Irving. In post-transition metal complexes, the order of stabilities was Cd(Ⅱ) < Pb(Ⅱ) < Hg(Ⅱ), and the covalent character in metal ion-donor atoms bonds appeared a dominant factor in the stability. In methanol solution, each metal ion forms 1 : 1 complex, while Ni(Ⅱ) ion forms both 1 : 1 and 1 : 2 complexes. It was confirmed by $^1H-$ and $^{13}C-$NMR spectral study that the nitrogen atoms in the ligand were major contributors for the complexation of post-transition metal ions with the ligand. It was shown, by elementry analysis, electrical conductivity and magnetic susceptibility measurements, and spectral analysis, that solid Cu(Ⅱ)-and Zn(Ⅱ)-complexes have a distorted octahedral and a tetrahedral structure, respectively.