• Bulletin of the Korean Chemical Society
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• v.35 no.7
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• pp.2057-2064
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• 2014

Thermochemical sulfate reduction (TSR) was conducted in autoclave on the system of crude oil and $MgSO_4$ at different temperatures. Gas chromatography pulsed flame photometric detector (GC-PFPD) was used to detected the composition of organic sulfur compounds in oil phase products. The results of the analysis indicate that with increased temperature, the contents of organic sulfur compounds with high molecular weight and thermal stability, such as benzothiophenes and dibenzothiophenes, gradually became dominated. In order to gain greater insight into the formation and distribution of organic sulphur compounds from TSR, positive ion electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was used in detecting the detailed elemental composition and distribution of them. The mass spectra showed that the mass range of sulfur compounds was 200-550 Da. Four sulfur class species, $S_1$, $N_1S_1$, $O_1S_1$ and $O_2S_1$, were assigned in the positive-ion spectrum. Among the identified sulfur compounds, the $S_1$ class species was dominant. The most abundant $S_1$ class species increase associated with the DBE value and carbon number increasing which also indicates the evolution of organic sulfur compounds in TSR is from the labile series to the stable one. In pure blank pyrolysis experiments with crude oil cracking without TSR, different composition and distribution of organic sulfur compounds in oil phase products were seen from mass spectra in order to evaluate their pyrolysis behaviors without $MgSO_4$. FT-IR and XRD were used in analyzing the products of solid phases. Two distinct crystallographic phases MgO and $MgSO_4$ are found to coexist in the products which demonstrated the transformation of inorganic sulfur compounds into organosulfur compounds exist in TSR.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.6
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• pp.243-251
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• 2016

Silanized-hydroxypropyl methylcellulose (Si-HPMC)/phase transformed calcium phosphate (PTCP) composites are prepared to purpose application of injectable bone cements with enhanced biocompatibility. The crystal structure and chemical state of the synthesized PTCP and Si-HPMC as solid and liquid phase of the composite cements were measured by XRD and FT-IR. The handling and mechanical properties of cements were measured by injectability tests and three-point bending tests. The in-vitro mechanical properties, XRD, and SEM results of bone cements were showed that enhanced hardening behavior was an inherent function of bone cements after in-vitro test. The cytotoxicity result of bone cements also was showed enhanced biocompatibility. Therefore, these injectable cements had potential be used as calcium phosphate cements for biomedical applications.

• Journal of the Mineralogical Society of Korea
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• v.25 no.4
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• pp.283-293
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• 2012

In order to have better insights into the chemical differentiation of Earth from its magma ocean phase to the current stratified structure, detailed information of crystallization kinetics of silicate melts consisting of the magma ocean is essential. The structural transitions in oxide glasses and melts upon crystallization provide improved prospects for a systematic and quantitative understanding of the crystallization processes. Here, we report the $^{27}Al$ 3QMAS NMR spectra for sol-gel synthesized $Al_2O_3$ glass with varying temperature and annealing time. The NMR spectra for the amorphous $Al_2O_3$ show well-resolved Al coordination environments, characterized with mostly $^{[4,5]}Al$ and a minor fraction of $^{[6]}Al$. The fraction of $^{[5]}Al$ in the alumina phase decreases with increasing annealing time at constant temperature. The NMR results of $Al_2O_3$ phases also imply that multiple processes (e.g., crystallization and/or changes in structural disorder within glasses) could involve upon its phase transition. The current results and method can be useful to understand crystallization kinetics of diverse natural and multi-component silicate glasses and melts. The potential result may yield atomic-level understanding of Earth's chemical evolution and differentiation from the magma ocean.

• Korean Journal of Materials Research
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• v.21 no.11
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• pp.604-610
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• 2011

The effect of $BaF_2$ flux in $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) formation was investigated. Phase transformation of $Y_3Al_5O_{12}$(YAG) was characterized by using XRD, SEM, and TEM-EDS, and it was revealed that the sequential formation of the $Y_4Al_2O_9$(YAM), $YAlO_3$(YAP) and $Y_3Al_5O_{12}$(YAG) in the temperature range of 1000-1500$^{\circ}C$. Single phase of YAG was revealed from 1300$^{\circ}C$. In order to find out the effect of $BaF_2$ flux, three modeling experiments between starting materials (1.5$Al_2O_3$-2.5$Y_2O_3$, $Y_2O_3$-$BaF_2$, and $Al_2O_3$-$BaF_2$) were done. These modeling experiments showed that the nucleation process occurs via the dissolution-precipitation mechanism, whereas the grain growth process is controlled via the liquid-phase diffusion route. YAG:Ce phosphor particles prepared using a proposed technique exhibit a spherical shape, high crystallinity, and an emission intensity. According to the experimental results conducted in this investigation, 5% of $BaF_2$ was the best concentration for physical, chemical and optical properties of $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) that is approximately 10-15% greater than that of commercial phosphor powder.

• Journal of Korea Foundry Society
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• v.23 no.5
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• pp.276-285
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• 2003

In the undercooled melt of $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy, the solidification behavior including nucleation and growth of crystals at the micrometer level has been observed in-situ by use of a confocal scanning laser microscope combined with an infrared image furnace. The $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy specimens were cooled from the liquid state to glass transition temperature. 575 K, at various cooling late under a helium gas flow. According to the cooling rate, the morphologies of the solidification front are changed among various types, irregular jog like front, columnar dendritic front, cellular grain, star like shape jog and fine grain, etc. The velocities of the solid-liquid interface are measured to be $10^{-5}{\sim}10^{-8}$ m/s which are at least two orders higher than the theoretical crystal growth rates. Combining the morphologies observed in terms of cooling rates and their solidification behaviors, we conclude that phase separation takes place in the undercooled molten $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy. The continuous cooling transformation (CCT) diagram was constructed from solidification onset time at various linear cooling conditions with different rate. The CCT diagram suggests that the critical cooling rate for glassy solidification is about 1.5 K/s, which is in agreement with the previous calorimetric findings.

• Korean Journal of Materials Research
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• v.22 no.4
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• pp.195-201
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• 2012

$Ce^{3+}$-doped yttrium aluminum gallium garnet (YAGG:$Ce^{3+}$), which is a green-emitting phosphor, was synthesized by solid state reaction using ${\alpha}$-phase or ${\gamma}$-phase of nano-sized $Al_2O_3$ as the Al source. The processing conditions and the chemical composition of phosphor for the maximum emission intensity were optimized on the basis of emission intensity under vacuum UV excitation. The optimum heating temperature for phosphor preparation was $1550^{\circ}C$. Photoluminescence properties of the synthesized phosphor were investigated in detail. From the excitation and emission spectra, it was confirmed that the YAGG:$Ce^{3+}$ phosphors effectively absorb the vacuum UV of 120-200 nm and emit green light positioned around 530 nm. The crystalline phase of the alumina nanoparticles affected the particle size and the luminescence property of the synthesized phosphors. Nano-sized ${\gamma}-Al_2O_3$ was more effective for the achievement of higher emission intensity than was nano-sized ${\alpha}-Al_2O_3$. This discrepancy is considered to be because the diffusion of $Al^{3+}$ into $Y_2O_3$ lattice is dependent on the crystalline phase of $Al_2O_3$, which affects the phase transformation of YAGG:$Ce^{3+}$ phosphors. The optimum chemical composition, having the maximum emission intensity, was $(Y_{2.98}Ce_{0.02})(Al_{2.8}Ga_{1.8})O_{11.4}$ prepared with ${\gamma}-Al_2O_3$. On the other hand, the decay time of the YAGG:$Ce^{3+}$ phosphors, irrespective of the crystalline phase of the nano-sized alumina source, was below 1 ms due to the allowed $5d{\rightarrow}4f$ transition of the $Ce^{3+}$ activator.

• Bulletin of the Korean Chemical Society
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• v.30 no.12
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• pp.3011-3015
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• 2009

Structural and thermo-analytical studies were carried out to understand the phase formation kinetics of the single phase $Bi_5Ti_3FeO_{15}$ (BTFO) nanocrystals in $Bi_2O_3-Fe_2O_3-TiO_2$, during the polymerized complex (PC) synthesis method. The crystallization of Aurivillius phase $Bi_5Ti_3FeO_{15}$ layered perovskite was found to be initiated and achieved under the temperature conditions in the range of ${\sim}$800 to 1050$^{\circ}C$. The activation energy for grain growth of $Bi_5Ti_3FeO_{15}$ nanocrystals (NCs) was very low in case of NCs formed by PC (2.61 kJ/mol) than that formed by the solid state reaction (SSR) method (10.9 kJ/mol). The energy involved in the phase transformation of Aurivillius phase $Bi_5Ti_3FeO_{15}$ from $Bi_2O_3-Fe_2O_3-TiO_2$ system was ${\sim}$ 69.8 kJ/mol. The formation kinetics study of $Bi_5Ti_3FeO_{15}$ synthesized by SSR and PC methods would not only render a large impact in the nanocrystalline material development but also in achieving highly efficient visible photocatalysts.

• Bulletin of the Korean Chemical Society
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• v.25 no.4
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• pp.511-516
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• 2004

A Li$[Co_{0.17}Li_{0.28}Mn_{0.55}]O_2$ cathode compound was prepared by a simple combustion method. The X-ray diffraction pattern showed that this compound could be classified as ${\alpha} -NaFeO_2$ structure type with the lattice constants of a = 2.8405(9) ${\AA}$ and c = 14.228(4) ${\AA}$. According to XANES analysis, the oxidation state of Mn and Co ions in the compound were 4+ and 3+, respectively. During the first charge process, the irreversible voltage plateau at around 4.65 V was observed. The similar voltage-plateau was observed in the initial charge profile of other solid solution series between $Li_2MnO_3\;and\;LiMnO_2$ (M=Ni, Cr...). The first discharge capacity was 187 mAh/g and the second discharge capacity increased to 204 mAh/g. As the increase of cycling number, one smooth discharge profile was converted to two distinct sub-plateaus and the discharge capacity was slowly decreased. From the Co and Mn K-edge XANES spectra measured at different cyclic process, it can be concluded that irreversible transformation of phase is occurred during continuous cycling process.

• Journal of the Korean Magnetics Society
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• v.7 no.4
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• pp.173-179
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• 1997

Change in phases, microstructures, and magnetic properties by the variation of quench rate and heat treatment were investigated for melt-spun $Fe_{77}Pr_{15}C_8$ ribbons. The amorphization of as-spun ribbons increased as the quench rate increased. As a result, the ribbon quenched at 40 m/s was almost entirely amorphous. Similarly to cast alloys, the primary phase in crystalline ribbons quenched at 10 m/s was $\alpha$-Fe followed by the secondary $Fe_{17}Pr_2C_x$. Crystalline phases were still dominant in the ribbon spun at 20 m/s, but in this case crystallization of $Fe_{17}Pr_2C_x$ was remarkable with a little suppression of $\alpha$-Fe. At 30 m/s an amorphous phase obviously dominated in the as-spun ribbons with small fraction of crystals. Therefore, substantial amount of hard magnetic $Fe_{14}Pr_2C$ was not obtained from the as-spun state but, as in cast alloys, produced only by a solid-state transformation. Within a few minutes fine grains of $Fe_{14}Pr_2C$ were easily obtained at relatively low temperature when the degree of amorphization of as-spun ribbons was higher. The grain size of $Fe_{14}Pr_2C$ was well less than 1${\mu}{\textrm}{m}$. The ribbons quenched at 20 or 30 m/s yielded higher coercivities after heat treatment.

• Journal of the Mineralogical Society of Korea
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• v.29 no.3
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• pp.131-139
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• 2016

Detailed knowledge on maskelynite, a glassy phase of plagioclase found in shocked meteorites and impact craters, is essential to understand a shock metamorphism. Here, we explore an inhomogeneous shock metamorphism in the lunar meteorite Mount DeWitt (DEW) 12007 with an aim to understand the formation mechanism of maskelynite. Most plagioclase grains in the DEW 12007 partially amorphized into maskelynite with a unidirectional orientation. Back-scattered electron (BSE) images of maskelynite show a remnant of planar deformation fracture possibly indicating that the maskelynite would be formed by solid-state transformation(i.e., diaplectic glass). Plagioclase with flow texture is also observed along the rim of maskelynite, which would be a result of recrystallization of melted plagioclase. Results of Raman experiments suggest that shock pressure for plagioclase and maskelynite in the DEW 12007 is approximately 5-32 GPa and 26-45 GPa, respectively. The difference in shock pressures between plagioclase and maskelynite can be originated from 1) external factors such as inhomogeneous shock pressure and/or 2) internal factors such as chemical composition and porosity of rock. Unfortunately, Raman spectroscopy has a limitation in revealing the detailed atomic structure of maskelynite such as development of six- or five-coordinated aluminum atom upon various shock pressure. Further studies using nuclear magnetic resonance spectroscopy are necessary to understand the formation mechanism of maskelynite under high pressure.