• Title/Summary/Keyword: spinel phase

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Preparation and Characterization of Mesoporous ${\gamma}-Al_2O_3$ Prepared from Kaolinite (카올린나이트로부터 중기공성 ${\gamma}-Al_2O_3$의 제조 및 특성)

  • Lee, Gwang-Hyeon;Go, Hyeong-Sin;Kim, Yun-Seop
    • Korean Journal of Materials Research
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    • v.10 no.12
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    • pp.845-852
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    • 2000
  • Mesoporous ${\gamma}-Al_2O_3$ has been prepared by selective leaching of silica from calcined domestic kaolinite. From XRD and TG-DTA data, it was found that the microstructure of a spinel phase, consisting of ${\gamma}-Al_2O_3$ containing a small mount of amorphous silica, was obtained by calcining kaolinite samples at around $1000^{\circ}C$ for 24h. Porous ${\gamma}-Al_2O_3$ was prepared by selectively dissolving the amorphous silica in KOH solutions of 1~4M at temperatures of $25~90^{\circ}C$ for leaching time of 0.5~4h. In the case of the ${\gamma}-Al_2O_3$ obtained upon KOH treatment of 4M at $90^{\circ}C$ for 1h, it showed a very narrow unimodal pore size distribution, and also formed much mesopore at a diameter of around $40~80{\AA}$. The specific surface area was $250\textrm{m}^2/g$ and the total pore volume was $0.654\textrm{cm}^3/g$.

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Activity Comparison According to Prepared Method of Cu-Mn Oxide Catalyst for Toluene Combustion (톨루엔 분해를 위한 구리-망간 산화물 촉매의 제조방법에 따른 활성 비교)

  • Kim, Hye-Jin;Choi, Sung-Woo;Lee, Chang-Seop
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.3
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    • pp.249-256
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    • 2006
  • Catalytic combustion of toluene was investigated on the Cu-Mn oxide catalysts prepared by the impregnation(Imp) and the deposition-precipitation(DP) methods. The mixing of copper and manganese has been found to enhance the activity of catalysts. It is then found that catalytic efficiency of the Cu-Mn oxide catalyst prepared by the DP method on combustion of toluene is much higher than that of the Cu-Mn oxide catalyst prepared by Imp method with the same chemical composition. The catalyst prepared by the deposition-precipitation method observed no change of toluene conversion at time on stream during 10 days and at the addition of water vapor. On the basis of catalyst characterization data, it has been suggested that the catalysts prepared by the DP method showed uniform distribution and smaller particle size on the surface of catalyst and then enhanced reduction capability of catalysts. Therefore, we think that the DP method leads on progressive capacity of catalyst and promotes stability of catalyst. It was also presumed that catalytic conversion of toluene on the Cu-Mn oxide catalyst depends on redox reaction and $Cu_{1.5}Mn_{1.5}O_4$ spinel phase acts as the major active sites of catalyst.

Mössbauer Studies of Manganese Iron Oxide Nanoparticles (망간-철산화물 나노입자의 뫼스바우어 분광 연구)

  • Hyun, Sung-Wook;Shim, In-Bo;Kim, Chul-Sung;Kang, Kyung-Su;Park, Chu-Sik
    • Journal of the Korean Magnetics Society
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    • v.18 no.1
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    • pp.24-27
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    • 2008
  • We have prepared $MnFe_2O_4$ nanoparticles with polyol method. The crystallographic and magnetic properties were measured by using X-ray diffraction(XRD), vibrating sample magnetometer(VSM) and $M\"{o}ssbauer$ spectroscopy. The high resolution transmission electron microscope(HRTEM) shows uniform nanoparticle-sizes with $6{\sim}8$ nm. The crystal structure is found to be single-phase cubic spinel with space group of Fd3m. The lattice constant of $MnFe_2O_4$ nanparticles is determined to be $8.418{\pm}0.001{\AA}$. $M\"{o}ssbauer$ spectrum of $MnFe_2O_4$ nanparticles at room temperature(RT) shows a superparamagnetic behavior. In VSM analysis, the diagnosis of the superparamagnetic behavior is also shown in hysteresis loop at RT. $M\"{o}ssbauer$ spectrum at 4.2K shows that the well developed two sextets are with different hyperfine field $H_{hfA}=498$(A-site) and $H_{hfB}=521$(B-site) kOe.

Adipic Acid Assisted Sol-Gel Synthesis of Li1+x(Mn0.4Ni0.4Fe0.2)1-xO2 (0 < x < 0.3) as Cathode Materials for Lithium Ion Batteries

  • Karthikeyan, Kaliyappan;Amaresh, Samuthirapandian;Son, Ju-Nam;Kim, Shin-Ho;Kim, Min-Chul;Kim, Kwang-Jin;Lee, Sol-Nip;Lee, Yun-Sung
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.89-94
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    • 2013
  • Layered $Li_{1+x}(Mn_{0.4}Ni_{0.4}Fe_{0.2})_{1-x}O_2$ (0 < x < 0.3) solid solutions were synthesized using solgel method with adipic acid as chelating agent. Structural and electrochemical properties of the prepared powders were examined by means of X-ray diffraction, Scanning electron microscopy and galvanostatic charge/discharge cycling. All powders had a phase-pure layered structure with $R\bar{3}m$ space group. The morphological studies confirmed that the size of the particles increased at higher x content. The charge-discharge profiles of the solid solution against lithium using 1 M $LiPF_6$ in EC/DMC as electrolyte revealed that the discharge capacity increases with increasing lithium content at the 3a sites. Among the cells, $Li_{1.2}(Mn_{0.32}Ni_{0.32}Fe_{0.16})O_2$ (x = 0.2)/$Li^+$ exhibits a good electrochemical property with maximum initial capacity of 160 $mAhg^{-1}$ between 2-4.5 V at 0.1 $mAcm^{-2}$ current density and the capacity retention after 25 cycles was 92%. Whereas, the cell fabricated with x = 0.3 sample showed continuous capacity fading due to the formation of spinel like structure during the subsequent cycling. The preparation of solid solutions based on $LiNiO_2-LiFeO_2-Li_2MnO_3$ has improved the properties of its end members.

K Addition Effect of Co3O4-based Catalyst for N2O Decomposition (N2O 분해반응용 Co3O4 기반 촉매의 K첨가 효과)

  • Hwang, Ra Hyun;Park, Ji Hye;Baek, Jeong Hun;Im, Hyo Been;Yi, Kwang Bok
    • Clean Technology
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    • v.24 no.1
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    • pp.35-40
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    • 2018
  • $Co_3O_4$ catalysts for $N_2O$ decomposition were prepared by co-precipitation method. Ce and Zr were added during the preparation of the catalyst as promoter with the molar ratio (Ce or Zr) / Co = 0.05. Also, 1 wt% $K_2CO_3$ was doped to the prepared catalyst with impregnation method to investigate the effect of K on the catalyst performance. The prepared catalysts were characterized with SEM, BET, XRD, XPS and $H_2-TPR$. The $Co_3O_4$ catalyst exhibited a spinel crystal phase, and the addition of the promoter increased the specific surface area and reduced the particle and crystal size. It was confirmed that the doping of K improves the catalytic activity by increasing the concentration of $Co^{2+}$ in the catalyst which is an active site for catalytic reaction. The catalytic activity tests were carried out at a GHSV of $45,000h^{-1}$ and a temperature range of $250{\sim}375^{\circ}C$. The K-impregnated $Co_3O_4$ catalyst showed much higher activity than $Co_3O_4$ catalysts with promoter only. It is found that the K-impregnation increased the concentration of $Co^{2+}$ more than the added of promoter did, and lowered the reduction temperature to a great extent.

The Processing control of NiCuZn Ferrite (I) - Mixing and Size Reduction of Raw Materials by Wet Ball Milling. (NiCuZn Ferrite의 제조공정 제어 (제1보) - 습식 볼밀링에 의한 다성분 원료의 혼합 및 분쇄 공정의 고찰)

  • 류병환;김선희;최경숙;고재천
    • Journal of the Korean Magnetics Society
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    • v.5 no.6
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    • pp.928-936
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    • 1995
  • In this research, the processing control of NiCuZn Ferrite has been developed. The mixing and the size reduction of raw materials have been proceeded. In order to produce NiCuZn Ferrite, highly concentrated slurry with fixed ratio and wet ball milling were used. First, the dispersion behavior of raw mixture at the region of pH4~pH11 has been studied. Using wet ball milling operation, the best conditions of mixing and size reduction have been determined. Further more, the most suitable conditions, such as, dispersant kind, dispersant amount, milling time, and slurry concentration have been studied. The poly acrylic ammonium salt (PAN) was chosen as a suitable dispersant to have effective dispersion in basic region. The slurry of raw mixture without dispersant, showed high viscosity and poor grindability. As 0.7 wt% of PAN was added, the concentrated slurry (up to 55 vol%) was possible, and showed well grindability. After 18 h ball milling of 30 vol% of mixture slurry with 0.7 wt% of PAN, the average particle size and specific surface area of raw mixture were $0.54\mu\textrm{m}$ and $12.92m^{2}/cc$, respectively. The ball milled raw mixture, calcined at $700^{\circ}C$ for 3h, was totally changed into NiCuZn Ferrite with spinel phase.

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Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

Mantle-derived CO2-fluid Inclusions in Peridotite Xenoliths from the Alkali Basalt, Jeju Island, South Korea (제주도 현무암에 포획된 페리도타이트에 산출되는 맨틀 기원의 CO2-유체포유물)

  • Seo, Minyoung;Woo, Yonghoon;Park, Geunyeong;Kim, Eunju;Lim, Hyoun Soo;Yang, Kyounghee
    • The Journal of the Petrological Society of Korea
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    • v.25 no.1
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    • pp.39-50
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    • 2016
  • Negative crystal shaped $CO_2$-rich fluid inclusions, trapped as primary inclusions in neoblasts and as secondary inclusions in porphyroblasts, were studied in spinel peridotite xenoliths from Jeju Island. Based on microthermometric experiments, the solid phase melts at $-57.1^{\circ}C$(${\pm}0.9^{\circ}C$) with no other observable melting events, indicating that the trapped fluid is mostly $CO_2$. The homogenization temperatures show a much wider range from $-39^{\circ}C$(${\rho}=1.12g/cm^{3)}$) to $23^{\circ}C$(${\rho}=0.82g/cm^{3)}$), suggesting that most of the inclusions (originally trapped at mantle conditions) re-equilibrated to lower density values. Nevertheless, the highest density $CO_2$ in our fluid inclusions is consistent with entrapment of fluids at upper mantle pressures (and depths). The calculated trapping pressure from $CO_2$-rich fluid inclusions that appear to be free from re-equilibrium, e.g., showing the lowest homogenization temperatures, is ${\approx}0.9GPa$. Based on the petrographic evidences, the fluid entrapment can be regarded as a late stage event in the evolution of the shallow lithospheric mantle.