• Title/Summary/Keyword: X-ray회절법

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Effects of SiO2 Incorporation on Catalytic Performance and Physico-Chemical Properties of Iron-Based Catalysts for the Fischer-Tropsch Synthesis (Fischer-Tropsch 합성반응용 Fe계 촉매의 성능 및 물리화학적 특성에 미치는 SiO2 첨가효과)

  • Hyun, Sun-Taek;Chun, Dong Hyun;Kim, Hak-Joo;Yang, Jung Hoon;Yang, Jung-Il;Lee, Ho-Tae;Lee, Kwan-Young;Jung, Heon
    • Korean Chemical Engineering Research
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    • v.48 no.3
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    • pp.304-310
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    • 2010
  • The FTS(Fischer-Tropsch synthesis) was carried out over precipitated iron-based catalysts with or without $SiO_2$ in a fixed-bed reactor at $250^{\circ}C$ and 1.5 MPa. The catalysts with $SiO_2$ showed much higher catalytic activity for the FTS than those without $SiO_2$, displaying excellent stability during 144 h of reaction. The X-ray diffraction and $N_2$ physisorption revealed that the catalysts with $SiO_2$ showed enhanced dispersion of $Fe_2O_3$ compared with those without $SiO_2$. Also, the results of temperature-programmed reduction by $H_2$ showed that the addition of $SiO_2$ markedly promoted the reduction of $Fe_2O_3$ into $Fe_3O_4$ and FeO at low temperatures below $260^{\circ}C$. In contrast, surface basicity of the catalysts, which was analyzed by temperature-programmed desorption of $CO_2$, decreased as a result of $SiO_2$ addition. We attribute the high and stable performance of the catalysts with $SiO_2$ to the improved dispersion and reducibility by the $SiO_2$ addition.

Physicochemical Properties of Chestnut Starch According to the Processing Method (전분 제조방법에 따른 밤전분의 이화학적 특성)

  • Kim, Yong-Doo;Choi, Ok-Ja;Shim, Ki-Hoon;Cho, In-Kyung
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.3
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    • pp.366-372
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    • 2006
  • This study is to investigate the physicochemical properties of differently pretreated chestnut starches during starch isolation and to examine their gelatinization properties by both heat and alkali treatments. One kind is starch A made by alkali method from peeled chestnut. The other is starch B made from chestnut with the outer layer. The results are as follows. Starch A has higher water binding capacity of 86.9% than starch B with 80.66%. Swelling powers of both starch A and B increased rapidly from $60^{\circ}C\;to\;80^{\circ}C$ in both, and since then it has changed a bit. Both began to show their solubility at $60^{\circ}C$ and increased continuously as the temperature went up. Starch A has higher swelling power and solubility than starch B. In iodine reaction, starch A has higher ${\lambda}max$ and absorbance at ${\lambda}max$ than starch B. X-ray diffraction patterns showed that starch A is type $C_b$ and that starch B is type B. Starch B has higher relative crystallinity of 37.0% than starch A with 36.2%. The results by differential scanning calorimetry revealed that starch A gelatinized from $66.95^{\circ}C$ to $77.5^{\circ}C$ and its enthalpy is 2.04 cal/g. And starch B gelatinized from $67.09^{\circ}C\;to\;77.5^{\circ}C$, and its enthalpy is 2.29 cal/g. Amylograms of chestnut starch at 6.5% concentration indicated that starch B needs higher onset temperature when beginning to gelatinize than starch A does. But starch A shows much higher peak viscosity, breakdown and setback than starch B does. Starch A shows higher viscosity, gel volume, and optical transmittance in gelatinization properties by alkali than starch B does.

Exchange Coupling Field and Thermal Stability of Ni80Fe20/[Ir22/Mn78-Mn]/Co75Fe25 Multilayer Depending on Mn Content (Ni80Fe20/[Ir22/Mn78-Mn]/Co75Fe25 다층박막에서 Mn 함유량에 의존하는 교환결합력과 열적안정성)

  • Kim, B.K.;Lee, J.Y.;Kim, S.S.;Hwang, D.G.;Lee, S.S.;Hwang, J.Y.;Kim, M.Y.;Rhee, J.R.
    • Journal of the Korean Magnetics Society
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    • v.13 no.5
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    • pp.187-192
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    • 2003
  • The magnetic and thermal properties of NiFe/[IrMn-Mn]/CoFe with Mn additions have been studied. As-deposited CoFe pinned layers with [IrMn-Mn]layer had dominantly larger exchange biasing field ( $H_{ex}$) and blocking temperature ( $T_{b}$) than those with pure I $r_{22}$M $n_{78}$ used. The $H_{ex}$ and $T_{b}$ improved with 76.8-78.1 vol% Mn, but those of the NiFe/IrMn/CoFe dropped considerably with more addition of 0.6 vol % Mn. The average x-ray diffraction peak ratios of fcc [(111)CoFe, NiFe]/(111)IrM $n_3$ textures for the Mn inserted total vol of 75.5, 77.5, and 79.3% were about 1.4, 0.8, and 0.6, respectively. For the sample without Mn inserted layer, the $H_{ex}$ between IrMn and CoFe layers was almost zero, but it increased to 100 Oe after annealing of 250 $^{\circ}C$. For as-grown two multilayers samples with ultra-thin Mn layers of 77.5 and 78.7 vol %, the $H_{ex}$s were 259 and 150 Oe, respectively. In case of IrMn with 77.5 vol% Mn, the $H_{ex}$ was increased up to 475 Oe at 350 $^{\circ}C$ but decreased to 200 Oe at 450 $^{\circ}C$, respectively. The magnetic properties and thermal stabilities of NiFe/[IrMn-Mn]/CoFe multilayer were enhanced with Mn additions. In applications where higher $H_{ex}$ and $T_{b}$ are required, proper contents of Mn can be used. be used. used.

Characterization on the Behavior of Heavy Metals and Arsenic in the Weathered Tailings of Songcheon Mine (송천광산의 풍화광미 내 중금속 및 비소 거동 특성)

  • Lee, Woo-Chun;Kim, Young-Ho;Cho, Hyen-Goo;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.2
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    • pp.125-139
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    • 2010
  • Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

Micromorphological and Mineral Characteristics of the Jang-won Series which have Fragipan in the soil Profile (경반층 토양인 장원통의 미세형태학적 및 광물학적 특성)

  • Moon, Yong-Hee;Zhang, Yong-Seon;Chun, Hyen-Chung;Sonn, Yeon-Kyu;Hyun, Byung-Keun;Park, Chan-Won;Song, Kwan-Cheol
    • Korean Journal of Soil Science and Fertilizer
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    • v.44 no.5
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    • pp.916-921
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    • 2011
  • This study was carry out on a Jang-Won series (fine loamy, mixed, mesic family of typic fragipan) that were established and classified as a fragipan soil in Korea. The morphological, physical, chemical and minerals characteristics of Jang-Won series were studied to determine the genesis of fragipan soils in natural environment. Each sample was analyzed for its physical, chemical and mineralogical characteristics. The particle size distribution of samples was measured using pipette method. Clay minerals were investigated on parallel-oriented specimens of the clay fraction ($<2{\mu}m$) from each horizon, separated by sieving and centrifugation, using X-ray diffraction (XRD) analysis. Micromorphological observations were made on thin sections prepared from soil blocks impregnated with Crystic Resin, cut and ground to less than $30{\mu}m$ in thickness, and finally polished with diamond paste. Most horizons have pH values in the range of fewer than 5.0 and have very low base-saturation values. Their textural classification ranges from silt loam to loam, the lower horizons being the finer. The clay fraction revealed the occurrence of illite, kaolinite, chlorite and vermiculite. The micro-morphological analysis carries out thin sections from each soil profile. The silt concentrations occur as extremely dense and homogenous bands or zones of silt-sized materials, brownish in colour in plane-polarized light and anisotropic in cross-polarized light, surrounding or adhering to skeleton grains. The genesis of fragipan in the Jangweon series assumed composition of clay fraction rather than silt concentration. Therefore, this results suggested an authentic interpretation which Jangweon series is classification as Typic Fragiochrepts.

Site Competition of Ca2+ and Cs+ Ions in the Framework of Zeolite Y (Si/Al = 1.56) and Their Crystallographic Studies (제올라이트 Y (Si/Al = 1.56) 골격 내의 Ca2+과 Cs+ 이온의 자리 경쟁 및 그들의 결정학적 연구)

  • Kim, Hu Sik;Park, Jong Sam;Lim, Woo Taik
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.4
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    • pp.235-248
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    • 2018
  • The present work was performed in order to study the effect of competing cation of $Ca^{2+}$ ion on ion exchange of $Cs^+$ on zeolite Y (Si/Al = 1.56). Three single-crystals of fully dehydrated and partially $Cs^+$-exchanged zeolites Y (Si/Al = 1.56) were prepared by the flow method using mixed ion-exchange solutions. The $CsNO_3:Ca(NO_3)_2$ molar ratios of the ion exchange solution were 1 : 1 (crystal 1), 1 : 100 (crystal 2), and 1 : 250 (crystal 3) with a total concentration of 0.05 M. The single-crystals were then vacuum dehydrated at 723 K and $1{\times}10^{-4}Pa$ for 2 days. The structures of the crystals were determined by single-crystal synchrotron X-ray diffraction technique in the cubic space group $Fd{\bar{3}}m$, at 100(1) K. The unit-cell formulas of crystals 1, 2, and 3 were ${\mid}Cs_{21}Ca_{27}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$, ${\mid}Cs_2Ca_{36.5}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$, and ${\mid}Cs_1Ca_{37}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$, respectively. In all three crystals, the $Ca^{2+}$ ions preferred to occupy site I in the D6Rs, with the remainder occupying sites I', II', and II. On the other hand, the significant differences in the fractional distribution of $Cs^+$ ions are observed depending on the intial $Cs^+$ concentrations in given ion exchange solution. In Crystal 1, $Cs^+$ ion are located at sites II', II, III, and III', and in crystal 2, at sites II, IIIa, and IIIb. In crystal 3, $Cs^+$ ions are only located at sites IIIa and IIIb. The degree of $Cs^+$ ion exchange decreased sharply from 28.0 to 2.7 to 1.3 % as the initial $Ca^{2+}$ concentration increases and the $Cs^+$ content decreases.

Crystal Structures of $Cd_6-A$ Dehydrated at $750^{\circ}C$ and Dehydrated $Cd_6-A$ Reacted with Cs Vapor ($750^{\circ}C$ 에서 탈수한 $Cd_6-A$의 결정구조와 이 결정을 세슘 증기로 반응시킨 결정구조)

  • Se Bok Jang;Yang Kim
    • Journal of the Korean Chemical Society
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    • v.37 no.2
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    • pp.191-198
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    • 1993
  • The crystal structures of $Cd_{6-}A$ evacuated at $2{\times}10^{-6}$ torr and $750^{\circ}C$ (a = 12.204(1) $\AA$) and dehydrated $Cd_{6-}A$ reacted with 0.1 torr of Cs vapor at $250^{\circ}C$ for 12 hours (a = 12.279(1) $\AA$) have been determined by single crystal X-ray diffraction techniques in the cubic space group Pm3m at $21(1)^{\circ}C.$ Their structures were refined to final error indices, $R_1=$ 0.081 and $R_2=$ 0.091 with 151 reflections and $R_1=$ 0.095 and $R_2=$ 0.089 with 82 reflections, respectively, for which I > $3\sigma(I).$ In vacuum dehydrated $Cd_{6-}A$, six $Cd^{2+}$ ions occupy threefold-axis positions near 6-ring, recessed 0.460(3) $\AA$ into the sodalite cavity from the (111) plane at O(3) : Cd-O(3) = 2.18(2) $\AA$ and O(3)-Cd-O(3) = $115.7(4)^{\circ}.$ Upon treating it with 0.1 torr of Cs vapor at $250^{\circ}C$, all 6 $Cd^{2+}$ ions in dehydrated $Cd_{6-}A$ are reduced by Cs vapor and Cs species are found at 4 crystallographic sites : 3.0 $Cs^+$ ions lie at the centers of the 8-rings at sites of $D_{4h}$ symmetry; ca. 9.0 Cs+ ions lie on the threefold axes of unit cell, ca. 7 in the large cavity and ca. 2 in the sodalite cavity; ca. 0.5 $Cs^+$ ion is found near a 4-ring. In this structure, ca. 12.5 Cs species are found per unit cell, more than the twelve $Cs^+$ ions needed to balance the anionic charge of zeolite framework, indicating that sorption of Cs0 has occurred. The occupancies observed are simply explained by two unit cell arrangements, $Cs_{12}-A$ and $Cs_{13}-A$. About 50% of unit cells may have two $Cs^+$ ions in sodalite unit near opposite 6-rings, six in the large cavity near 6-ring and one in the large cavity near a 4-ring. The remaining 50% of unit cells may have two Cs species in the sodalite unit which are closely associated with two out of 8 $Cs^+$ ions in the large cavity to form linear $(Cs_4)^{3+}$ clusters. These clusters lie on threefold axes and extend through the centers of sodalite units. In all unit cells, three $Cs^+$ ions fill equipoints of symmetry $D_{4h}$ at the centers of 8-rings.

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Evaluation of Mn Removal Efficiency from the Mine Drainage in the Presence of Fe Using Slag Complex Reactors (제강슬래그 복합매질체를 이용한 철 유입에 따른 광산배수내 망간 제거효율 평가)

  • Kim, Dong-Kwan;Ji, Won Hyun;Kim, Duk-Min;Park, Hyun-Sung;Oh, Youn Soo
    • Economic and Environmental Geology
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    • v.51 no.5
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    • pp.401-407
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    • 2018
  • For the treatment of heavy metals in the mine drainage from the closed mine area, various methods such as passive, active and semi-active treatments are considered. Among contaminated elements in the mine drainage, Mn is one of the difficult elements for the treatment because it needs high pH over 9.0 for its concentration to be reduced. In this study, the efficiency of various slag complex reactors (slag (S), slag+limestone (SL) and slag+Mn coated gravel (SG)) on Mn removal in the presence of Fe, which is a competitive element with Mn, was evaluated to investigate effective methods for the treatment of Mn in mine drainage. As a result of experiments on Mn removal without Fe during 358 days, using influent with $30{\sim}50Mn{\cdot}mg/L$ and pH 6.7 on the average, S reactor showed continuously high Mn removal efficiency with the average of 99.9% with pH 8.9~11.4. Using the same reactors, Mn removal experiments with Fe during 237 days were conducted with the influent with $40{\sim}60Mn{\cdot}mg/L$. The pH range of effluent reached to 6.1~10.0, which is slightly lower than that of effluent without Fe. S reactor showed the highest range of pH with 7.1~9.9, followed by S+L and S+G reactor. However, the efficiency of Mn removal showed S+L>S>S+G with the range of 94~100%, 68~100% and 68~100%, respectively in spite of relatively low pH range. S+L reactor showed the most resistance on Fe input, which means other mechanisms such as $MnCO_3$ formation by the carbonate prouced from the limestone or autocatalysis reaction of Mn contributed to Mn removal rather than pH related mechanisms. The evidence of reactions between carbonates and Mn, rhodochrosite ($MnCO_3$), was found from the X-ray diffraction analysis of precipitates sample from S+L reactor. From this study, the most effective reactors on Mn removal in the presence of Fe was S+L reactor. The results are expected to be applied for the Mn containing mine water treatment in the presence of Fe within the relatively low range of pH.

CO2 Sequestration and Utilization of Calcium-extracted Slag Using Air-cooled Blast Furnace Slag and Convert Slag (괴재 및 전로슬래그를 이용한 CO2 저감 및 칼슘 추출 후 슬래그 활용)

  • Yoo, Yeongsuk;Choi, Hongbeom;Bang, Jun-Hwan;Chae, Soochun;Kim, Ji-Whan;Kim, Jin-Man;Lee, Seung-Woo
    • Applied Chemistry for Engineering
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    • v.28 no.1
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    • pp.101-111
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    • 2017
  • Mineral carbonation is a technology in which carbonates are synthesized from minerals including serpentine and olivine, and industrial wastes such as slag and cement, of which all contain calcium or magnesium when reacted with carbon dioxide. This study aims to develop the mineral carbonation technology for commercialization, which can reduce environmental burden and process cost through the reduction of carbon dioxide using steel slag and the slag reuse after calcium extraction. Calcium extraction was conducted using NH4Cl solution for air-cooled slag and convert slag, and ${\geq}98%$ purity calcium carbonate was synthesized by reaction with calcium-extracted solution and carbon dioxide. And we conducted experimentally to minimize the quantity of by-product, the slag residue after calcium extraction, which has occupied large amount of weight ratio (about 80-90%) at the point of mineral carbonation process using slag. The slag residue was used to replace silica sand in the manufacture of cement panel, and physical properties including compressive strength and flexible strength of panel using the slag residue and normal cement panel, respectively, were analyzed. The calcium concentration in extraction solution was analyzed by inductively coupled plasma optical emission spectrometer (ICP-OES). Field-emission scanning electron microscope (FE-SEM) was also used to identify the surface morphology of calcium carbonate, and XRD was used to analyze the crystallinity and the quantitative analysis of calcium carbonate. In addition, the cement panel evaluation was carried out according to KS L ISO 679, and the compressive strength and flexural strength of the panels were measured.

Ti-Getter Effects on Magnetic Properties of Ti0.96Co0.02Fe0.02O2 (Ti-Getter가 Ti0.96Co0.02Fe0.02O2의 자기적 특성에 미치는 영향)

  • Nam, H.D.;Kim, S.J.;Baek, J.K.;Lee, S.R.;Park, Cheol-Su;Kim, E.C.
    • Journal of the Korean Magnetics Society
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    • v.18 no.3
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    • pp.109-114
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    • 2008
  • The samples were synthesized by using a solid state reaction. The X-ray diffraction pattern for $Ti_{0.96}Co_{0.02}Fe_{0.02}O_2$ showed a pure rutile phase with tetragonal structure, Mixtures of the proper proportions of the elements sealed in evacuated quartz ampoule were heated at $870{\sim}930^{\circ}C$ for one day and then slowly cooled down to room temperature at a rate of $10^{\circ}C$/h. In order to obtain single phase material, it was necessary to grind the sample after the first firing and to press the powders into pellets before annealing them for a second time in evacuated and sealed quartz ampoule. Magnetic properties have been investigated using the vibrating sample magnetometer (VSM). Room temperature magnetic hysteresis (M-H) curve showed an obvious ferromagnetic behavior and the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $1.5\;{\mu}_B$/CoFe. But the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $0.02\;{\mu}_B$/CoFe without Ti-getter. Size of particles is about $1\;{\mu}m$ using the transmission electron microscope (TEM). The ingredients of sample are distributed irregular in particles. Only Fe get shown on the surface of particles.