• Journal of the Korean Electrochemical Society
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• v.16 no.3
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• pp.157-161
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• 2013

Porous $LiMn_{0.6}Fe_{0.4}PO_4$ (LMFP) was synthesized by a sol-gel process. Uniform dispersion of the conductive carbon source throughout LMFP with uniform carbon coating was achieved by heating a stoichiometric mixture of raw materials at $600^{\circ}C$ for 10 h. The crystal structure of LMFP was investigated by Rietveld refinement. The surface structure and pore properties were investigated by SEM, TEM and BET. The LMFP so obtained has a high specific surface area with a uniform, porous, and web-like nano-sized carbon layer at the surface. The initial discharge capacity and energy density were 152 mAh/g and 570 Wh/kg, respectively, at 0.1 C current density, and showed stable cycle performance. The combined effect of high porosity and uniform carbon coating leads to fast lithium ion diffusion and enhanced electrochemical performance.

• Economic and Environmental Geology
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• v.45 no.2
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• pp.79-88
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• 2012

The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

• Journal of the Korean Magnetics Society
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• v.17 no.1
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• pp.38-42
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• 2007

The crystallographic and magnetic properties of $KFeO_2$ powder prepared by ball-mill method, have been studied by x-ray diffraction(XRD), $M\"{o}ssbauer$ spectroscopy, and vibrating sample magnetometer(VSM) measurements. The crystal structure of $KFeO_2$ powder at room temperature is determined to be an orthorhombic structure of Pbca with its lattice constants $a_0=5.557{\AA},\;b_0=11.227{\AA},\;c_0=15.890{\AA}$ by Rietveld refinement. $M\"{o}ssbauer$ spectra of $KFeO_2$ were taken at various temperatures ranging from 4.2 to 818 K. The magnetic hyperfine field and isomer shift value at 4.2 K and RT were 519 kOe, 489 kOe and 0.19 mm/s, 0.05 mm/s respectively. The average hyperfine field $H_{hf}(T)$ of the $KFeO_2$ shows a temperature dependence of $[H_{hf}(T)-H_{hf}(0)]/H_{hf}(0)=-0.36(T/T_N)^{5/2}$ for $T/T_N$<0.7, indicative of spin-wave excitation.

• Journal of the Korean Magnetics Society
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• v.17 no.1
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• pp.47-50
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• 2007

[ $ZnCr_2O_4$ ] shows geometrically frustrated magnet. Recently, $CoCr_2O_4$ has been investigated for multiferroic property and dielectric anomalies by spin-current model. Polycrystalline $CoCr_2O_4$ and $CoCrFeO_4$ compounds was prepared by wet-chemical process. Crystallographic and magnetic properties of $CoCr_2O_4$ and $CoCrFeO_4$ were investigate by using the x-ray diffractometer(XRD), vibrating sample magnetometer(VSM), superconducting quantum interference device magnetometer(SQUID), and $M\"{o}ssbauer$ spectroscopy. The crystal structure was found to be single-phase cubic spinel with space group of Fd3m. The lattice constants of $CoCr_2O_4$ and $CoCrFeO_4$ $a_0$ were determined to be 8.340 and 8.377 ${\AA}$, respectively. The ferrimagnetic transition temperature for the both samples were observed at 97 K and 320 K. The $M\"{o}ssbauer$ absorption spectra at 4.2 K show that the well developed two sextets are superposed with small difference of hyperfine field($H_{hf1}=507\;and\;H_{hf2}=492\;kOe$). Isomer shift values($\delta$) of the two sextets are found to be 0.33 and 0.34 mm/s relative to the Fe metal, respectively, which are consistent with the high spin $Fe^{3+}$ charge state.

• Journal of the Korean Chemical Society
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• v.47 no.6
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• pp.614-618
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• 2003

$Sr_2Ru_{1-x}Cu_xO_{4-y}(0.0{\le}x{\le}0.5)$ compounds were prepared using a conventional solid state reaction. Based on the Rietveld refinements of X-ray diffraction results, it is revealed that $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds are the single phases with K2NiF4 type tetragonal system in the range of 0=x=0.3, while the mixed phases of$Sr_2RuO_4$ and $Sr_2CuO_3$ in the range of $0.4{\le}x{\le}0.5$. By means of X-ray photoelectron spectroscopy, the valence states of Ru and Cu in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, have been confirmed to 4+ and 2+, respectively. The bond length difference between $Ru-O_1 ({\times}4)\;and\;Ru-O_2 ({\times}2)\;in\;RuO_6$ octahedron is gradually decreased with increasing Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, which results in the lower c/a ratio. So, it might be assured that the variation of local symmetry of $RuO_6$ octahedron is very closely related to the transporting property of $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds. The behavior of resistivity discloses that the metallic property in $Sr_2RuO_4$ changes into the semiconducting one in proportion to the Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$.

• Journal of the Korean Recycled Construction Resources Institute
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• v.8 no.3
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• pp.294-301
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• 2020

This study evaluated the burnability and hydration reaction of clinker burned with high Al₂O₃ content OPC to apply large amounts of industrial by-products in the cement manufacturing process. Specifically, after preparing a clinker with a high C₃A content by burning the OPC raw material with a high content of Al₂O₃ in a laboratory electric furnace, the burnability of the clinker was evaluated through XRD Rietveld analysis and polarization microscopy, and clinker hydration reactivity was reviewed through the Isothermal conduction calorimetry analysis and the cement compressive strength. As a result, the kiln burning temperature for the production of high Al₂O₃ content clinker lower, and the compressive strength was equal to or higher than OPC. Therefore it was confirmed the possibility to manufacturing energy-saving high Al₂O₃ content clinker using a large amount of industrial by-products.

• Journal of the Korean Recycled Construction Resources Institute
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• v.9 no.1
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• pp.20-25
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• 2021

The cement clinker, the main raw material of cement, is manufactured using limestone as the main material. Depending on the quality of limestone, the use of subsidiary materials changes, and has a great influence on the production of cement clinkers. In this study, the effect of CaO content of limestone, a cement clinker material, on Raw Mill grinding and sintering of cement clinker was investigated. The grinding time of the union materials changed in the content of limestone CaO was measured to identify the grinding properties. The raw material combination was cleaned within a range of 1,350-1,500℃. The sintering performance of cement clinker by Burnability index calculation was identified. The lower the grade of limestone, the lower the grinding quality of the raw material combination. The lower the CaO content of limestone, the greater the variation in F-CaO for sintering temperature. The lower the class of limestone, the higher B. I. value was calculated, indicating the lower cement clinker sintering. In addition, the mineral analysis results of cement clinker showed that if the F-CaO value was low due to the increase in sintering temperature, the Belite content decreased and the Alite content increased. In the case of Alite, the ratio of R-type decreased and that of M-type increased as the content of limestone CaO increased.

• Journal of the Mineralogical Society of Korea
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• v.15 no.4
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• pp.329-344
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• 2002

Mineralogical and chemical characterization of some domestic bentonites, such as quantitative XRD analysis, chemical leaching experiments, pH and CEC determinations, were done without any separation procedures to understand their relationships among mineral composition, characteristics, and cation exchange properties. XRD quantification results based on Rietveld method reveal that the bentonites contain totally more than 25 wt% of impurities, such as zeolites, opal-CT, and feldspars, in addition to montmorillonite ranging 30～75 wt%. Cation exchange properties of the zeolitic bentonites are deeply affected by the content of zeolites identified as clinoptilolite-heulandite series. Clinoptilolite is common in the silicic bentonites with lighter color. and occurs closely in association with opal-CT. Ca is mostly the dominant exchangeable cation, but some zeolitic bentonites have K as a major exchangeable cation, The values of cation exchange capacity (CEC) determined by Methylene Blue method are comparatively low and have roughly a linear relationship with the montmorillonite content of the bentonite, though the correlated data tend to be rather dispersed. Compared to this, the CEC determined by Ammonium Acetate method, i.e.‘Total CEC’, has much higher values (50～115 meq/100 g). The differences between those CEC values are much greater in zeolitic bentonites, which obviously indicates the CEC increase affected by zeolite. Other impurities such as opal-CT and feldspars seem to affect insignificantly on the CEC of bentonites. When dispersed in distilled water, the pH of bentonites roughly tends to increase up to 9.3 with increasing the alkali abundance, especially Na, in exchangeable cation composition. However, some bentonites exhibit lower pH (5～6) so as to regard as ‘acid clay’. This may be due to the presence of $H^{＋}$ in part as an exchangeable cation in the layer site of montmorillonite. All the works of this study ultimately suggest that an assesment of domestic bentonites in grade and quality should be accomplished through the quantitative XRD analysis and the ‘Total CEC’measurement.

• Korean Journal of Mineralogy and Petrology
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• v.35 no.2
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• pp.111-123
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• 2022

Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO₃^2-) and sulfate (SO₄^2-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH^-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.

• Journal of the Korean Electrochemical Society
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• v.15 no.3
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• pp.172-180
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• 2012

The $LiMn_2O_4$ cathodes for lithium ion battery were synthesized from various precursors of manganese oxides and manganese hydroxides. As the first step, nanosized precursors such as ${\alpha}-MnO_2$ (nano-sticks), ${\beta}-MnO_2$ (nano-rods), $Mn_3O_4$ (nano-octahedra), amorphous $MnO_2$(nano-spheres), and $Mn(OH)_2$ (nano-plates) were prepared by a hydrothermal or a precipitation method. Spinel $LiMn_2O_4$ with various sizes and shapes were finally synthesized by a solid-state reaction method from the manganese precursors and LiOH. Nano-sized (500 nm) octahedron $LiMn_2O_4$ showed high capacities of 107 mAh $g^{-1}$ and 99 mAh $g^{-1}$ at 1 C- and 50 C-rate, respectively. Three dimensional octahedral crystallites exhibit superior electrochemical characteristics to the other one-dimensional and two-dimensional shaped $LiMn_2O_4$ nanoparticles. After 500 consecutive charge discharge battery cycles at 10 C-rate with the nano-octahedron $LiMn_2O_4$ cathode, the capacity retention of 95% was observed, which is far better than any other morphologies studied in this work.