• Journal of the Mineralogical Society of Korea
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• v.10 no.2
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• pp.148-161
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• 1997

Based on the X-ray powder diffraction (XRD) and M ssbauer spectroscopy, the thermal behavior and phase transformations of two clays are investigated for raw and fired conditions, which are collected from Kwangryeongli and Ildo district in Cheju Island. M ssbauer spectra at room temperature and 20for two clays show that paramagnetic Fe3- is the structural iron of the layer silicate and ferrihydrite, and superparamagnetic goethite has about 50% of total iron contents. The XRD peaks of hematite for the fired clays appear from 80$0^{\circ}C$ in Kwangryeongli clay and from $600^{\circ}C$ in Ildo district clay, respectively. The structural Fe2+ was completely oxidized into Fe3- at 40$0^{\circ}C$ for Kwangryeongli clay and 50$0^{\circ}C$~$600^{\circ}C$ for Ildo district clay, respectively. The structural Fe2+ was completely oxidized into Fe3- at 40$0^{\circ}C$. For the temperature ranging from 40$0^{\circ}C$ to $700^{\circ}C$~80$0^{\circ}C$, two fired clays exhibit the dehydroxylation of the clay mineral. A disintegration of the clay mineral structure is observed from $700^{\circ}C$~80$0^{\circ}C$ to 110$0^{\circ}C$, followed by the onset and spread of vitrification process. It is also shown that well-crystallized hematite phase is formed at the temperature higher than 110$0^{\circ}C$ and the relative absorption area decreases, which might be related to the recrystallization of alluminosilicate matrix.

• Korean Journal of Materials Research
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• v.15 no.2
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• pp.97-105
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• 2005

[ $11\AA$ ] tobermorite$(5CaO{\cdot}6SiO_2{\cdot}5H_2O)$ is synthesized from the mixtures of calcium hydroride and quartz using alumina in a molar ratio $Ca(OH)_2/SiO_2$ of 0.8 at $180^{\circ}C$ for 8 and 24 hrs under saturated steam pressure. The influence of alumina on the formation of $11\AA$ tobermorite was investigated by X-ray diffraction, differential thermal analysis and infrared spectroscopy. $11\AA$ tobermorite containing increasingly larger amounts of aluminum showed a shift of the basal spacing from 11.3 to $11.6\AA$. In general, there was a direct linear relation between the basal spacing and added content of alumina. The differential thermal analysis curves showed that $11\AA$ tobermorite with increasing alumina contents exhibited the exothermic peak at high temperature, namely $11\AA$ tobermorite containing aluminum gave a sharp exothermic peak at temperature around $850\~860^{\circ}C$ in the case of $S_3\~S_5$. The absorption band at $1607\~1620cm^{-1}$ is attributed to the bending vibration of water, and the position of the main O-H stretching and Si-O lattice vibration of $11\AA$ tobermorite at 3500 and $965cm^{-1}$ respectively is not altered. Consequently the existence of alumina accelerates the crystallization of $11\AA$ tobermorite, and that the aluminum ion appears to substitute for the silicon ion in $11\AA$ tobermorite structure. Al-containing tobermorite is distinguished from Al-free tobermorite.

• Bulletin of the Korean Chemical Society
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• v.26 no.9
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• pp.1395-1402
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• 2005

The reaction of cis-[Cr([14]-decane)$(OH)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = acetylacetonate (acac), oxalate (ox) or malonate (mal)} leads to a new cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O\;(1),\;cis-[Cr([14]-decane)(ox)]ClO_4{\cdot}(1/2)H_2O\;(2)\;or\;cis-[Cr([14]-decane)(mal)]ClO_4{\cdot}(1/4)H_2O\;(3)$. These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two acetylacetonate-oxygen atoms are bonded to the chromium(III) ion in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by $11^{\circ}$ from the ideal value of $180^{\circ}$ for a perfect octahedron. The bond angle O-Cr-O between the chromium(III) ion and the two acetylacetonate-oxygen atoms is close to $90^{\circ}$. The bond lengths of Cr-O between the chromium and the acetylacetonate-oxygen atoms are 1.950(3) and 1.954(2) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 1560 {ν (C=O)}, 1710 {${\nu}_{as}$(OCO)} and 1660 $cm^{-1}$ {${\nu}_{as}$(OCO)} attributed to the acac, ox and mal auxiliary ligands stretching vibrations, respectively.

• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3695-3702
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• 2013

A nickel(II) complex $[Ni(H_2biim)_2(H_2O)_2](ClO_4)_2{\cdot}H_2O$ (1) of biimidazole ligand has been synthesized and characterized (Where $H_2biim$ = 2,2'-biimidazole). The single crystal X-ray diffraction of the complex shows a dimeric structure with six coordinated psudo-octahedral geometry. The cyclic voltammograms of complex exhibited one quasireversible reduction wave ($E_{pc}=-0.61V$) and an irreversible oxidation wave ($E_{pa}=1.28V$) in DMF solution. The interaction of the complex with Calf-Thymus DNA (CT-DNA) has been investigated by absorption and fluorescence spectroscopy. The complex is an avid DNA binder with a binding constant value of $1.03{\times}10^5M^{-1}$. The results suggest that the nickel(II) complex bind to CT-DNA via intercalative mode and can quench the fluorescence intensity of EB bind to CT-DNA with $K_{app}$ value of $3.2{\times}10^5M^{-1}$. The complex also shown efficient oxidative cleavage of supercoiled pBR322 DNA in the presence of hydrogen peroxide as oxidizing agent. The DNA cleavage by complex in presence of quenchers; viz. DMSO, KI, $NaN_3$ and EDTA reveals that hydroxyl radical or singlet oxygen mechanism is involved. The complex showed invitro antimicrobial activity against four bacteria and two fungi. The antimicrobial activity was nearer to that of standard drugs and greater than that of the free ligand.

• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3635-3640
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• 2013

We prepared Ni and Pd-modified $TiO_2@SiO_2$ core-shell nanostructures and then analyzed them by scanning electron microscopy, optical microscopy, X-ray diffraction crystallography, FT-IR and UV-Visible absorption spectroscopy. In addition, their CO oxidation performance was tested by temperature-programmed mass spectrometry. The CO oxidation activity showed an order of Ni-$TiO_2@SiO_2$ ($900^{\circ}C$) < Ni-$TiO_2@SiO_2$ ($90^{\circ}C$) < Ni-$TiO_2@SiO_2$ ($450^{\circ}C$) in the first CO oxidation run, and greatly improved activity in the same order in the second run. The $T_{10%}$ (the temperature at 10% CO conversion) corresponds to the CO oxidation rate of $2.8{\times}10^{-5}$ molCO $g{_{cat}}^{-1}s^{-1}$. For Ni-$TiO_2@SiO_2$ ($450^{\circ}C$), the $T_{10%}$ was observed at $365^{\circ}C$ in the first run and at $335^{\circ}C$ in the second run. For the Pd-$TiO_2@SiO_2$ ($450^{\circ}C$), the $T_{10%}$ was observed at a much lower temperature of $263^{\circ}C$ in the first CO oxidation run, and at $247^{\circ}C$ in the second run. The CO oxidation activities of transition metal modified $TiO_2@SiO_2$ core-shell nanostructures presented herein provide new insights that will be useful in developing catalysts for various environments.

• Journal of Magnetics
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• v.20 no.3
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• pp.229-240
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• 2015

In this study, nanocrystalline ferrite powders with the composition $Ni_{0.5}Zn_{0.5}Fe_2O_4$ were prepared by the autocombustion method. The obtained powders were sintered at $800^{\circ}C$, $900^{\circ}C$ and $1,000^{\circ}C$ for 4 h in air atmosphere. The as-prepared and the sintered powders were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and magnetization studies. An increase in the crystallite size and a slight decrease in the lattice constant with sintering temperature were observed, whereas microstrain was observed to be negative for all the samples. Two significant absorption bands in the wave number range of the $400cm^{-1}$ to $600cm^{-1}$ have been observed in the FT-IR spectra for all samples which is the distinctive feature of the spinel ferrites. The force constants were found to vary with sintering temperature, suggesting a cation redistribution and modification in the unit cell of the spinel. The M-H loops indicate smaller coercivity, which is the typical nature of the soft ferrites. The observed variation in the saturation magnetization and coercivity with sintering temperature has been attributed to the role of surface, inhomogeneous cation distribution, and increase in the crystallite size.

• Journal of the Mineralogical Society of Korea
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• v.2 no.1
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• pp.26-36
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• 1989

Clinopyroxene in the Geodo mine belongs to diopside-hedenbergite series. It is widely distributed throughout the mine area together with garnet and is also closely related with Fe-mineralization. Clinopyroxenes in the Geodo mine including two samples from the sangdong and Ulchin Mines are studied using polarized microscope, EPMA, XRD, and IR spectroscopy for occurrence, chemistry, structure, and crystal chemistry. Especially, variations in unit-cell parameters are examined in relation with the substitution scheme between Fe and Mg cations. Clinopyroxenes in the Geodo mine occur in both endoskarn and exoskarn zone. It is mostly anhedral to subhedral with fine- to medium-grained in texture, but some have bigger crystals of short prismatic or columnar habits. Clinopyroxene occurs as monomineralic or is associated with mostly garnet and sometimes with actinolite, magnetite, epidote, and chlorite. Chemical analysis reveals that the Geodo clinopyroxene is diopsidic in composition (Di: 65-96%). This fact is in good contrast with garnet chemistry showing mostly andraditic (An: 41-82%). Especially, clinopyroxene coexisting with magnetite belongs to nearly end member diopside (Di: 97-99%). Thus, diopside-andradite pair indicates that Geodo skarns were formed under the reduced environment. X-ray diffraction analysis shows unit-cell parameters vary with increase of Fe contents: a = 9.765-9.838$\AA$, b = 8.943-9.020$\AA$, c= 5.240-5.253$\AA$.$\beta$ = 105.70-104.83$^{\circ}$, and V =440.64-448.19$\AA$3. It is noted from the least square regression that a, b and V increase linearly with increase of Fe content, while $\beta$ slightly decreases and c remains nearly unchanged as change in Fe content. These trends are to difference between synthetic and natural clinopyroxenes. This fact is also recognized in IR spectra which show a slight shift of several absorption bands toward lower wavenumber region with increasing Fe content.

• The Journal of Advanced Prosthodontics
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• v.6 no.3
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• pp.207-214
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• 2014

PURPOSE. This study characterized the synthesis of a modified PMMA (Polymethyl methacrylate) denture acrylic loading platinum nanoparticles (PtN) and assessed its bacterial inhibitory efficacy to produce novel antimicrobial denture base material. MATERIALS AND METHODS. Polymerized PMMA denture acrylic disc ($20mm{\times}2mm$) specimens containing 0 (control), 10, 50, 100 and 200 mg/L of PtN were fabricated respectively. The obtained platinum-PMMA nanocomposite (PtNC) was characterized by TEM (transmission electron microscopy), SEM/EDX (scanning electron microscope/energy dispersive X-ray spectroscopy), thermogravimetric and atomic absorption spectrophotometer analysis. In antimicrobial assay, specimens were placed on the cell culture plate, and $100{\mu}L$ of microbial suspensions of S. mutans (Streptococcus mutans) and S. sobrinus (Streptococcus sobrinus) were inoculated then incubated at $37^{\circ}C$ for 24 hours. The bacterial attachment was tested by FACS (fluorescence-activated cell sorting) analysis after staining with fluorescent probe. RESULTS. PtN were successfully loaded and uniformly immobilized into PMMA denture acrylic with a proper thermal stability and similar surface morphology as compared to control. PtNC expressed significant bacterial anti-adherent effect rather than bactericidal effect above 50 mg/L PtN loaded when compared to pristine PMMA (P=.01) with no or extremely small amounts of Pt ion eluted. CONCLUSION. This is the first report on the synthesis and its antibacterial activity of Pt-PMMA nanocomposite. PMMA denture acrylic loading PtN could be a possible intrinsic antimicrobial denture material with proper mechanical characteristics, meeting those specified for denture bases. For clinical application, future studies including biocompatibility, color stability and warranting the long-term effect were still required.

• Korean Journal of Materials Research
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• v.27 no.4
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• pp.206-210
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• 2017

In this study, an ${\alpha}-Fe_2O_3$ (hematite) coated porcelain plate was sintered in a temperature range from $1100^{\circ}C$ to $1250^{\circ}C$ using ferrous sulfate. The specimens were investigated by X-ray diffractometer (XRD), scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), and UV-visible spectrophotometer. It was confirmed that ${\alpha}-Fe_2O_3$ (hematite) was densely fused to the surface at several tens of ${\mu}m$, the ${\alpha}-Fe_2O_3$ (hematite) was in the form of thin platelet and polyhedra, and no other compounds appeared in the sintering process. In the specimen coated with ${\alpha}-Fe_2O_3$ (hematite), the reflectance spectra show a red absorption band of 560-650 nm. The $L^*$ value decreased from 53.18 to 46.94 with the firing temperature. The values of $a^*$ and $b^*$ were at 19.03 and 15.25 at $1100^{\circ}C$ and gradually decreased with increasing temperature; these values decreased rapidly at $1250^{\circ}C$ to 11.54 and 7.98, respectively. It is considered that the new phases are formed by the phase transition of the porcelain plate (clay), and thus the $a^*$ and $b^*$ values are greatly influenced.

• Journal of the Korean Magnetics Society
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• v.16 no.1
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• pp.14-17
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• 2006

[ $AIFeO_3$ ]has been studied by x-ray diffraction (XRD), vibrating sample magnetometer, Mossbauer spectroscopy. The crystal structure is found to orthorhombic with the lattice parameters being $a_0=4.983\;{\AA},\;b_0=8.554\;{\AA},\;c_0=9.239\;{\AA}$, Magnetic hysteresis curve for $AIFeO_3$ showed weakly ferromagnetic phase at room temperature and a asymmetric shape dependent on the direction of applied field at low temperature. The Curie temperature determined by the temperature dependence of magnetization is 250 K. Mossbauer spectra of $AIFeO_3$ have been taken from 4.2 K to 295 K. Isomer shift at room temperature are found to be $0.11\~0.32\;mm/s$, which is consistent with ferric state. The absorption lines widths become broader with increasing temperature, which is attributed to the Fe ions distribution of each cation site and anisotropy energy difference of each sublattice.