• Title/Summary/Keyword: powder X-ray diffraction

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Janggunite, a New Mineral from the Janggun Mine, Bonghwa, Korea (경북(慶北) 봉화군(奉化郡) 장군광산산(將軍鑛山産) 신종광물(新種鑛物) 장군석(將軍石)에 대(對)한 광물학적(鑛物學的) 연구(硏究))

  • Kim, Soo Jin
    • Economic and Environmental Geology
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    • v.8 no.3
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    • pp.117-124
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    • 1975
  • Wet chemical analysis (for $MnO_2$, MnO, and $H_2O$(+)) and electron microprobe analysis (for $Fe_2O_3$ and PbO) give $MnO_2$ 74.91, MnO 11.33, $Fe_2O_3$ (total Fe) 4.19, PbO 0.03, $H_2O$ (+) 9.46, sum 99.92%. 'Available oxygen determined by oxalate titration method is allotted to $MnO_2$ from total Mn, and the remaining Mn is calculated as MnO. Traces of Ba, Ca, Mg, K, Cu, Zn, and Al were found. Li and Na were not found. The existence of (OH) is verified from the infrared absorption spectra. The analysis corresponds to the formula $Mn^{4+}{_{4.85}}(Mn^{2+}{_{0.90}}Fe^{3+}{_{0.30}})_{1.20}O_{8.09}(OH)_{5.91}$, on the basis of O=14, 'or ideally $Mn^{4+}{_{5-x}}(Mn^{2+},Fe^{3+})_{1+x}O_{8}(OH)_{6}$ ($x{\approx}0.2$). X-ray single crystal study could not be made because of the distortion of single crystals. But the x-ray powder pattern is satisfactorily indexed by an orthorhombic cell with a 9.324, b 14.05, c $7.956{\AA}$., Z=4. The indexed powder diffraction lines are 9.34(s) (100), 7.09(s) (020), 4.62(m) (200, 121), 4.17(m) (130), 3.547(s) (112), 3.212(vw) (041), 3.101(s) (300), 2.597(w) (013), 2.469(m) (331), 2.214(vw)(420), 2.098(vw) (260), 2.014 (vw) (402), 1.863(w) (500), 1.664(w) (314), 1.554(vw) (600), 1.525(m) (601), 1.405(m) (0.10.0). DTA curve shows the endothermic peaks at $250-370^{\circ}C$ and $955^{\circ}C$. The former is due to the dehydration: and oxidation forming$(Mn,\;Fe)_2O_3$(cubic, a $9.417{\AA}$), and the latter is interpreted as the formation of a hausmannite-type oxide (tetragonal, a 5.76, c $9.51{\AA}$) from $(Mn,\;Fe)_2O_3$. Infrared absorption spectral curve shows Mn-O stretching vibrations at $515cm^{-1}$ and $545cm^{-1}$, O-H bending vibration at $1025cm^{-1}$ and O-H stretching vibration at $3225cm^{-1}$. Opaque. Reflectance 13-15%. Bireflectance distinct in air and strong in oil. Reflection pleochroism changes from whitish to light grey. Between crossed nicols, color changes from yellowish brown with bluish tint to grey in air and yellowish brown to grey through bluish brown in oil. No internal reflections. Etching reactions: HCl(conc.) and $H_2SO_4+H_2O_2$-grey tarnish; $SnCl_2$(sat.)-dark color; $HNO_3$(conc.)-grey color; $H_2O_2$-tarnish with effervescence. It is black in color. Luster dull. Cleavage one direction perfect. Streak brownish black to dark brown. H. (Mohs) 2-3, very fragile. Specific gravity 3.59(obs.), 3.57(calc.). It occurs as radiating groups of flakes, flower-like aggregates, colloform bands, dendritic or arborescent masses composed of fine grains in the cementation zone of the supergene manganese oxide deposits of the Janggun mine, Bonghwa-gun, southeastern Korea. Associated minerals are calcite, nsutite, todorokite, and some undetermined manganese dioxide minerals. The name is for the mine, the first locality. The mineral and name were approved before publication by the Commission on New Minerals and Mineral Names, I.M.A.

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Effects of Mn- and K-addition on Catalytic Activity of Calcium Oxide for Methane Activation (메탄 활성화반응에서 산화칼슘 촉매의 활성에 대한 망간과 칼륨의 첨가효과)

  • Park, Jong Sik;Kong, Jang Il;Jun, Jong Ho;Lee, Sung Han
    • Journal of the Korean Chemical Society
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    • v.42 no.6
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    • pp.618-628
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    • 1998
  • Pure CaO, Mn-doped CaO, Mn/CaO, and K/CaO catalysts were prepared and tested as catalysts for the oxidative coupling of methane in the temperature range of 600 to 800$^{\circ}C$ to investigate the effects of Mn- and K-addition on the catalytic activity of calcium oxide. To characterize the catalysts, X-ray powder diffraction(XRD), XPS, SEM, DSC, and TG analyses were performed. The catalytic reaction was carried out in a single-pass flow reactor using on-line gas chromatography system. Normalized reaction conditions were generally $p(CH_4)/p(O_2)=250$ Torr/50 Torr, total feed flow rate=30 mL/min, and 1 atm of total pressure with He being used as diluent gas. Among the catalysts tested, 6.3 mol% Mn-doped CaO catalyst showed the best $C_2$ yield of 8.0% with a selectivity of 43.2% at 775$^{\circ}C$. The $C_2$ selectivity increased on lightly doped CaO catalysts, while decreased on heavily doped CaO([Mn] > 6.3 mol%) catalysts. 6 wt.% Mn/CaO and 6 wt.% K/CaO catalysts showed the $C_2$ selectivities of 13.2% and 30.9%, respectively, for the reaction. Electrical conductivities of CaO and Mn-doped CaO were measured in the temperature range of 500 to 1000$^{\circ}C$ at Po2's of $10^{-3}\; to\;10^{-1}\;atm.$ The electrical conductivity was decreased with Mn-doping and increased with increasing $P0_2$in the range of $10^{-3}\;to\;10^{-1}\;atm,$ indicating the specimens to be p-type semiconductors. It was suggested that the interstitial oxygen ions formed near the surface can activate methane and the formation of interstitial oxygen ions was discussed on the basis of solid-state chemistry.

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Physicochemical properties of powdered, soft and hard type rice flour by different milling methods (제분방법에 따른 분질, 연질 및 경질미 가루의 이화학적 특성)

  • Choi, Ok Ja;Jung, Hee Nam;Shim, Ki Hoon
    • Food Science and Preservation
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    • v.22 no.2
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    • pp.174-181
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    • 2015
  • This study investigated the physicochemical properties of three different types of rice flour prepared via dry and wet milling. The powder, soft, and hard-types of rice flour were Suwon No. 542, Suwon No. 541, and Unbong No. 30, respectively. The analysis of the proximate compositions of the different types of rice flour showed that their moisture content was 7.03~7.99%, their crude protein was 7.94~8.35%, their crude lipid was 0.71~1.49% and their crude ash was 0.25~0.82%. For the Hunter's color values, the L value was highest in the wet-milled rice flour, the a value was highest in the dry-milled rice flour, and the b value was highest in the dry-milled rice flour. All the samples showed distinctive rice starch particles in the particle analysis using scanning electron microscope. The dry-milled rice flour showed the greatest amount of irregular particles and the coarsest texture. The water absorption and water solubility indices were higher in the wet-milled soft- and hard-type rice flour. The crystallinities of the samples by X-ray diffractography were all A-type, but the crystallinity of the dry-milled hard-type rice flour was higher in diffraction degree. For the amylogram properties, the wet-milled soft-type rice flour showed the highest maximum viscosity, breakdown and setback. In the meanwhile, the dry-milled soft-type rice flour showed the highest initial pasting temperature, onset, peak, and end temperatures despite of the reverse enthalpy.

Heavy Metal Contamination of Soils and Stream Sediments at the Sanggok Mine Drainage, Upper Chungju Lake, Korea (충주호 상류, 상곡광산 수계에 분포하는 토양과 하상퇴적물의 중금속 오염)

  • 이현구;이찬희
    • Journal of the Korean Society of Groundwater Environment
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    • v.5 no.1
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    • pp.10-20
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    • 1998
  • Heavy metal contamination in subsurface soils and stream sediments at the Suggok mine area were investigated on the basis of major, trace and rare earth elements geochemistry and mineralogy. The Sanggok mine area is mainly composed of Cambro-Ordovician carbonate rocks. The mine had been mined for Pb-Zn-Fe and Au- Ag, but already closed in past. For major elements, especially Fe (mean value=18.58 wt.%) and Mn (mean value=4. 18 wt.%) are enriched in soils, and the average enrichment indices of soils and sediments are 6.84 and 1.54, respectively. The average enrichment index of rare earth elements are 0.92 of mining drainage sediments and 0.52 of subsurface soils on the tailing dam. Concentrations of minor and/or environmental toxic elements in those samples range from 29 to 3400 for As,1 to 11 for Cd, 35 to 292 for Cu, 50 to 1827 for Pb, 1 to 22 for Sb and 112 to 2644 for Zn. Extremely high concentrations (mean values) are found in subsurface soils on the tailing dam (As=2278, Cd=7, Cu=206, Pb=1372, Sb=14 and Zn=2231 ppm, respectively). Average enrichment index normalized by composition of non-mining drainage sediments is 2.42 in mining drainage sediments and 25.47 in subsurface soils on the tailing dam. Based on EPA value, enrichment index of toxic elements is 0.53 in non-mining drainage sediments, 1.84 in mining drainage sediments and 23.71 in subsurface soils on the tailing dam. As a results from X-ray powder diffraction method, mineral composition of soils and sediments near the mine area varied in part, and are calcite, dolomite, magnesite, quartz, mica, chlorite and clay minerals. With the separation of heavy minerals, soils and sediments of highly concentrated toxic elements included some pyrite, arsenopyrite, sphalerite, galena, goethite and hydroxide minerals on the polished sections.

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Characterization of SiC nanowire Synthesized by Thermal CVD (열 화학기상증착법을 이용한 탄화규소 나노선의 합성 및 특성연구)

  • Jung, M.W.;Kim, M.K.;Song, W.;Jung, D.S.;Choi, W.C.;Park, C.J.
    • Journal of the Korean Vacuum Society
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    • v.19 no.4
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    • pp.307-313
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    • 2010
  • One-dimensional cubic phase silicon carbide nanowires (${\beta}$-SiC NWs) were efficiently synthesized by thermal chemical vapor deposition (TCVD) with mixtures containing Si powders and nickel chloride hexahydrate $(NiCl_2{\cdot}6H_2O)$ in an alumina boat with a carbon source of methane $(CH_4)$ gas. SEM images are shown that the growth temperature (T) of $1,300^{\circ}C$ is not enough to synthesize the SiC NWs owing to insufficient thermal energy for melting down a Si powder and decomposing the methane gas. However, the SiC NWs could be synthesized at T>$1,300^{\circ}C$ and the most efficient temperature for growth of SiC NWs is T=$1,400^{\circ}C$. The synthesized SiC NWs have the diameter with an average range between 50~150 nm. Raman spectra clearly revealed that the synthesized SiC NWs are forming of a cubic phase (${\beta}$-SiC). Two distinct peaks at 795 and $970 cm^{-1}$ in Raman spectra of the synthesized SiC NWs at T=$1,400^{\circ}C$ represent the TO and LO mode of the bulk ${\beta}$-SiC, respectively. XRD spectra are also supported to the Raman spectra resulting in the strongest (111) peaks at $2{\Theta}=35.7^{\circ}$, which is the (111) plane peak position of 3C-SiC. Moreover, the gas flow rate of 300 sccm for methane is the optimal condition for synthesis of a large amount of ${\beta}$-SiC NW without producing the amorphous carbon structure shown at a high methane flow rate of 800 sccm. TEM images are shown two kinds of the synthesized ${\beta}$-SiC NWs structures. One is shown the defect-free ${\beta}$-SiC NWs with a (111) interplane distance of 0.25 nm, and the other is the stacking-faulted ${\beta}$-SiC NWs. Also, TEM images exhibited that two distinct SiC NWs are uniformly covered with $SiO_2$ layer with a thickness of less 2 nm.

Magnetic and Electric Transport Properties of MnTe Thin Film Grown by Molecular Beam Epitaxy (분자선 증착법에 의해 성장한 MnTe 박막의 자기적 및 전기수송 특성)

  • Kim, Woo-Chul;Bae, Sung-Whan;Kim, Sam-Jin;Kim, Chul-Sung;Kim, Kwang-Joo;Yoon, Jung-Bum;Jung, Myung-Hwa
    • Journal of the Korean Magnetics Society
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    • v.17 no.2
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    • pp.81-85
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    • 2007
  • MnTe layers of high crystalline quality were successfully grown on Si(100) : B and Si(111) substrates by molecular beam epitaxy (MBE). Under tellurium-rich condition and the substrate temperature around $400^{\circ}C$, a layer thickness of $700{\AA}$ could be easily obtained with the growth rate of $1.1 {\AA}/s$. We investigated the structural, magnetic and transport properties of MnTe layers by using x-ray diffraction (XRD), superconducting quantum interference device (SQUID) magnetometry, and physical properties measurement system (PPMS). Characterization of MnTe layers on Si(100) : B and Si(111) substrates by XRD revealed a hexagonal structure of polycrystals with lattice parameters, ${\alpha}=4.143{\pm}0.001{\AA}\;and\;c=6.707{\pm}0.001{\AA}$. Investigation of magnetic and transport properties of MnTe films showed anomalies unlike antiferromagnetic powder MnTe. The temperature dependence of the magnetization data taken in zero-field-tooling (ZFC) and field-cooling (FC) conditions indicates three magnetic transitions at around 21, 49, and 210 K as well as the great irreversibility between ZFC and FC magnetization in the films. These anomalies are attributable to a magnetic-elastic coupling in the films. Magnetization measurements indicate ferromagnetic behaviour with hysteresis loops at 5 and 300 K for MnTe polycrystalline film. The coercivity ($H_c$) values at 5 and 300 K are 55 and 44 Oe, respectively. In electro-transport measurements, the temperature dependence of resistivity revealed a noticeable semiconducting behaviours and showed conduction via Mott variable range hopping at low temperatures.

Phase Transitions of $LiMn_2O_4$ on $CO_2$ Decomposition (($CO_2$ 분해시 $LiMn_2O_4$의 상변화)

  • Kwoen, Tae-Hwan;Yang, Chun-Mo;Park, Young-Goo;Cho, Young-Koo;Rim, Byung-O
    • Journal of the Korean Applied Science and Technology
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    • v.20 no.1
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    • pp.33-43
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    • 2003
  • $LiMn_2O_4$ catalyst for $CO_2$ decomposition was synthesized by oxidation method for 30 min at 600$^{\circ}C$ in an electric furnace under air condition using manganese(II) nitrate $(Mn(NO_3)_2{\cdot}6H_2O)$, Lithium nitrate ($LiNO_3$) and Urea $(CO(NH_2)_2)$. The synthesized catalyst was reduced by $H_2$ at various temperatures for 3 hr. The reduction degree of the reduced catalysts were measured using the TGA. And then $CO_2$ decomposition rate was measured using the reduced catalysts. Phase-transitions of the catalysts were observed after $CO_2$ decomposition reaction at an optimal decomposition temperature. As the result of X-ray powder diffraction analysis, the synthesized catalyst was confirmed that the catalyst has the spinel structure, and also confirmed that when it was reduced by $H_2$, the phase of $LiMn_2O_4$ catalyst was transformed into $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase. After $CO_2$ decomposition reaction, it was confirmed that the peak of $LiMn_2O_4$ of spinel phase. The optimal reduction temperature of the catalyst with $H_2$ was confirmed to be 450$^{\circ}C$(maximum weight-increasing ratio 9.47%) in the case of $LiMn_2O_4$ through the TGA analysis. Decomposition rate(%) using the $LiMn_2O_4$ catalyst showed the 67%. The crystal structure of the synthesized $LiMn_2O_4$ observed with a scanning electron microscope(SEM) shows cubic form. After reduction, $LiMn_2O_4$ catalyst became condensed each other to form interface. It was confirmed that after $CO_2$ decomposition, crystal structure of $LiMn_2O_4$ catalyst showed that its particle grew up more than that of reduction. Phase-transition by reduction and $CO_2$ decomposition ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase at the first time of $CO_2$ decomposition appear like the same as the above contents. Phase-transition at $2{\sim}5$ time ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase by reduction and $LiMn_2O_4$ of spinel phase after $CO_2$ decomposition appear like the same as the first time case. The result of the TGA analysis by catalyst reduction ; The first time, weight of reduced catalyst increased by 9.47%, for 2${\sim}$5 times, weight of reduced catalyst increased by average 2.3% But, in any time, there is little difference in the decomposition ratio of $CO_2$. That is to say, at the first time, it showed 67% in $CO_2$ decomposition rate and after 5 times reaction of $CO_2$ decomposition, it showed 67% nearly the same as the first time.

Pressure-load Calibration of Multi-anvil Press and the Thermal Gradient within the Sample Chamber (멀티 앤빌 프레스의 압력-부하 보정 작업과 시료 내의 온도구배 연구)

  • Kim, Eun Jeong;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.3
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    • pp.161-172
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    • 2018
  • Multi-anvil press (MAP) is one of the high pressure apparatuses and often generates the pressure-conditions ranging from 5 to 25 GPa and temperature-conditions up to $2,300^{\circ}C$. The MAP is, therefore, suitable to explore the pressure-induced structural changes in diverse earth materials from Earth's mantle and the bottom of the mantle transition zone (~660 km). In this study, we present the experimental results for pressure-load calibration of the 1,100-ton multi-anvil press equipped in the authors' laboratory. The pressure-load calibration experiments were performed for the 14/8 step, 14/8 G2, 14/8 HT, and 18/12 assembly sets. The high pressure experiments using ${\alpha}$-quartz, wollastonitestructure of $CaGeO_3$, and forsterite as starting materials were analyzed by powder X-ray diffraction spectroscopy. The phase transition of each mineral indicates the specific pressure that is loaded to a sample at $1,200^{\circ}C$: a transition of ${\alpha}$-quartz to coesite at 3.1 GPa, that of garnet-structure of $CaGeO_3$ to perovskite-structure at 5.9 GPa, that of coesite to stishovite at 9.2 GPa, and that of forsterite to wadsleyite at 13.6 GPa. While the estimated pressure-load calibration curve is generally consistent with those obtained in other laboratories, the deviation up to 50 tons is observed at high pressure above 10 GPa. This is partly because of the loss of oil pressure at high pressure resulting from the differences in a sample chamber, and the frictional force between pressure medium and second anvil. We also report the ${\sim}200^{\circ}C/mm$ of thermal gradient in the vertical direction of the sample chamber of 14/8 HT assembly. The pressure-load calibration curve and the observed thermal gradient within the sample chamber can be applied to explain the structural changes and the relevant macroscopic properties of diverse crystalline and amorphous earth materials in the mantle.

Glycerol Steam Reforming for Hydrogen Production on Metal-ceramic Core-shell CoAl2O4@Al Composite Structures (금속-세라믹 Core-Shell CoAl2O4@Al 구조체를 적용한 불균일계 촉매의 글리세롤 수소전환 반응특성)

  • Kim, Jieun;Lee, Doohwan
    • Clean Technology
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    • v.21 no.1
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    • pp.68-75
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    • 2015
  • In this study, we investigated the structure and properties of a highly heat conductive metal-ceramic core-shell CoAl2O4@Al micro-composite for heterogeneous catalysts support. The CoAl2O4@Al was prepared by hydrothermal surface oxidation of Al metal powder, which resulted in the structure with a high heat conductive Al metal core encapsulated by a high surface area CoAl2O4 shell. For comparison, CoAl2O4 was also prepared by co-precipitation method and also utilized for a catalyst support. Rh catalysts supported on CoAl2O4@Al and CoAl2O4 were prepared by incipient wetness impregnation and characterized by N2 adsorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), CO chemisorption, and temperature-programmed reduction (TPR). The properties of catalysts were investigated for glycerol steam reforming reaction for hydrogen production at 550 ℃. Rh/CoAl2O4@Al exhibited about 2.8 times higher glycerol conversion turnover frequency (TOF) than Rh/CoAl2O4 due to facilitated heat transport through the core-shell structure. The CoAl2O4@Al and CoAl2O4 also showed some catalytic activities due to a partial reduction of Co on the support, and a higher catalytic activity was also found on the CoAl2O4@Al core-shell than CoAl2O4. These catalysts, however, displayed deactivation on the reaction stream due to carbon deposition on the catalysts surface.