• Title/Summary/Keyword: Homogeneous Solution

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Molecular Structure of PCP Pincer Complexes: Poisoning Catalyst on the Dehydrogenation of Alkanes (알칸의 탈수소화반응에서의 촉매독 화합물의 분자구조)

  • Lee Ji Hyun;Chun Sang Jin;Kwon Ki Hyeok;Lee Do Weon
    • Korean Journal of Crystallography
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    • v.16 no.1
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    • pp.43-53
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    • 2005
  • The dihydrido P-C-P pincer complex, $IrH_2{C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (1), was successfully prepared from the reaction of the hydrochloride complex, $IrClH (C_6H_3-2,6-(CH_2PBu_2^t)_2}$, and super acid $(LiBEt_3H)$ under 1 atm of hydrogen in pentane solution at room temperature and followed by Heating at $130^{\circ}C$ in vacuo. Jensen recently found that the dihydrido P-C-P pincer complex 1 is a highly active homogeneous catalyst for the transfer dehydrogenation of alkanes with unusual longterm stability at temperatures as high as $200^{\circ}C$. The treatment of dihydrido complex 1 with nitrogen, water, carbon dioxide, and carbon monoxide in presence of tert-butylethylene (the) at room temperature in an appropriate solution gave the dinitrogen complex, $[Ir{C-6H_3-2,6-(CH_2PBu_2^t)_2}]_2({\mu}-N_2)$ (2), the hydrido hydroxyl complex, $IrH(OH){C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (3), the carbon dioxide complex, $Ir({\eta}^2-CO_2) {C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (including the bicarbonate complex, $IrH({\kappa}^2-O_2COH){C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(4))$, and the carbonyl complex, $Ir(CO) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(5)$ (including the carboxyl complex, $IrH(C(O)OH) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(6))$, in good yield, respectively. These P-C-P iridium complexes were isolated and characterized by $^1H,\;^{13}C,\;^{31}P\; NMR$, and IR spectroscopy. In addition, the complexes (1-6) were characterized by a single crystal X-ray crystallography. These complexes account for these small molecules' inhibition of dehydrogenation of alkanes catalyzed by the dihydrido complex 1.

A new Method of Stiction Reduction for MEMS Structures Using DDMS (DDMS를 이용한 MEMS 구조물의 새로운 점착방지 방법)

  • Kim, Bong-Hwan;Oh, Chang-Hoon;Chun, Kuk-Jin;Oh, Yong-Soo
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.37 no.6
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    • pp.9-16
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    • 2000
  • In order to achieve stiction-free polysilicon surfaces, we have suggested a new class of chemical coating precursors and confirmed their excellent characteristics. The strategy is to adopt dialkyldichlorosilanes (DDS, $R2SiCl_2$) instead of monoalkyltrichlorosilanes (MTS, $RSiCl_3$) such as octadecyltrichlorosilane (OTS) or 1H,1H2H,2H-perfluorodecyltrichlorosilane (FDTS). Dichlorodimethylsilane (DDMS, $(CH_3)2SiCl_2$) in this study is commercially available DDS with two short chains. DDMS in aprotic media spontaneously deposits on the hydrophilic polysilicon surface, which is completely changed to hydrophobic one. When polysilicon surface is exposed to DDMS solution at room temperature, anti-stiction property and hydrophobicity are clearly comparable to FDTS. DDMS is even superior to MTS in reliability and easy handling, which provides high yield. Since interactions among precursor molecules are reduced, conglomeration both in homogeneous solution and on surface can be effectively avoided. Even the cantilevers of 3 mm in length can be protected successfully from the stiction and the final quality of the modified surfaces is much less dependent on temperature. And no difference was found between the processes in ambient environment and in dry box. In addition, DDMS has advantages of remarkably reduced process time and low cost.

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High Tc Superconductor Fiber $YBa_2Cu_3O_{7-{\sigma}}$ Synthesized by the Sol-gel Process (Sol-gel 법에 의한 고온 초전도체 $YBa_2Cu_3O_{7-{\sigma}}$ 선재 합성에 관한 연구)

  • Jin Ho Choy;Jong Seok Yoo;Bae Whan Kim;Seung Tae Hong
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.326-331
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    • 1989
  • Superconducting fiber of high Tc $YBa_2Cu_3O_{7-{\sigma}}$ was successfully prepared by the sol-gel method. The stoichiometric mixture of Y, Ba and Cu nitrates was dissolved in water, to which citric acid solution was added. Then ammonium hydroxide was added to the mixture in order to increase the pH to a value between 5.8 and 6.2. The mixture was heated carefully to form a homogeneous colloid sol at 358 K. The solution was viscous enough to draw a long gel fiber, which was then heated at 1223K for 8 hrs. under oxygen partial pressure of $Po_2$ = 1 atm., cooled slowly and annealed at 723K for 13 hrs.. The reacted superconducting sample maintained a fiber form with some shrinkage of its volume. The superconducting transition temperatures (Tc, onset and Tc, offset) of $YBa_2Cu_3O_{7-{\sigma}}$ have been determined to be approximately 95K and 82K, respectively. The superconducting phase was also confirmed by Meissner effect at liquid nitrogen boiling temperature.

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Synthesis of $TiO_2$Anchored on a Porous Clay Ceramic Support Using Dropping Precipitant Method (침전제 적하법을 이용한 $TiO_2$고정화 다공체 제조)

  • 신대용;한상목;김경남
    • Journal of the Korean Ceramic Society
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    • v.38 no.12
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    • pp.1097-1103
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    • 2001
  • TiO$_2$anchored on a porous clay ceramic support (PCS) for use in lightweight photocatalyst were synthesized by the dropping precipitant method. A PCS of macro and micro pore size of around several mm~${\mu}{\textrm}{m}$ in diameter were prepared by the rapid heat treatment at, 1,15$0^{\circ}C$ for 10 min from low grade of clay. The change in pH of reaction solution due to the different addition rate of NH$_4$HCO$_3$as a precipitant, the reaction temperature and the concentration of TiCl$_4$had a pronounced effect on the nature of precipitated TiO$_2$particles on the surface of a PCS and the crystal structure of precipitated TiO$_2$particles. At an addition rate of 0.8 ml/min of NH$_4$HCO$_3$and pH=6 of reaction solution, homogeneous precipitation of TiO$_2$particles on a PCS was achieved. TiO$_2$particles with anatase phase was precipitated on the surface of a PCS at the low concentration of TiCl$_4$, the high addition rate of NH$_4$HCO$_3$and the high reaction temperature.

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Formation Behavior of Precipitated Calcium Carbonate Polymorphs by Supersaturation (과포화도에 의한 침강성 탄산칼슘 다형체의 생성거동)

  • Ahn, Young jun;Jeon, ong Hyuk;Lee, Shin Haeng;Yu, Young Hwan;Jeon, Hong Myeong;Ahn, Ji Whan;Han, Choon
    • Resources Recycling
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    • v.24 no.4
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    • pp.22-31
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    • 2015
  • From results obtained by adjusting experimental variables based on the kinetic, the nucleation rate for formation of precipitated calcium carbonate (PCC) was investigated. Formation behavior of PCC was investigated for various concentrations of NaOH solution and $Na_2CO_3$ addition methods in the $Ca(OH)_2$ slurry. The range of nucleation rate was investigated for dissolution rates of major ion concentrations, $Ca^{2+}$ and $CO{_3}^{2-}$. In case of high concentration of major ions, vaterite and calcite were synthesized. The high nucleation rate was achieved for lower either $Ca^{2+}$ or $CO{_3}^{2-}$ ion concentration, calcite was mainly synthesized and when concentration of major ions was low, aragonite was synthesized. Furthermore, the formation of calcite was decreased with increasing concentration of NaOH. homogeneous aragonite could be obtained by addition 5 M NaOH. Therefore, in this study, specific shape of polymorphs could be prepared through controlling supersaturation.

A study on synthesis of $Li_{x}Mn_{2}O_{4}$ for asecondary battery with various $MnO_{2}$ structure (다양한 $MnO_{2}$ 구조에 따른 2차전지용 $Li_{x}Mn_{2}O_{4}$ 합성에 관한 연구)

  • 김익진;이영훈;이종호;이재한;장동환;이경희;고영신
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.6 no.4
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    • pp.600-608
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    • 1996
  • Specific structural properties of Li intercalation reaction into the spinel relatedmanganese dioxide, $Li_{x}Mn_{2}O_{4}(0.2{\leq}x{\leq}2.0)$, are investigated by X-ray diffractional and electrochemical studies of Li/1M $LiClO_{4}$-propylene carbonate solution/$Li_{x}Mn_{2}O_{4}$ cell. The effect of the chemical composition and the reaction temperature on electrochemical parameter of $Li_{x}Mn_{2}O_{4}$ are studied by the phenomena of phase-transition, analysis of crystal lattice, fine structure, and thermal analysis. Treatment of the spinel $Li_{x}Mn_{2}O_{4}$ with aqueous acid was found to result in conversiton of $Li_{x}Mn_{2}O_{4}$ to nearly pure $MnO_{2}$, as evidenced by a reduction in the lattice constant $a_{c}$ from 8.255 to $8.031\;{\AA}$. At a composition range of $0.2{\leq}x{\leq}0.6$ in $Li_{x}Mn_{2}O_{4}$ the reduction proceeded in a homogeneous phase, which was characterized by a constant voltage of 3.9~3.7 V together with a lattice constant of $8.255\;{\AA}$.

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Immuno-stimulating Polysaccharides from the Fruiting Bodies of Fomitella fraxinea (I) - Characterization of polysaccharides extracted with neutral sodium chloride solution - (Fomitella fraxinea로부터 분리한 면역활성 다당류 (I) -중성염 용액 추출 다당류의 특성-)

  • Cho, Soo-Muk;Lee, Jae-Hoon;Han, Sang-Bae;Kim, Hwan-Mook;Yu, Seung-Hun;Yoo, Ick-Dong
    • The Korean Journal of Mycology
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    • v.23 no.4 s.75
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    • pp.332-339
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    • 1995
  • Water-soluble polysaccharide (FCW) was extracted from the fruiting body of Fomitella fraxinea with neutral sodium chloride solution. The polysaccharide was further fractionated into FCW-I and FCW-II by ion exchange chromatography. The FCW-I and FCW-II were then purified by gel permeation chromatography and named as FCW-Ia and FCW-IIa, respectively. FCW-IIa showed relatively strong immuno-stimulating activity but FCW-Ia did not. By analyses of HPLC and GPC, FCW-Ia and FCW-IIa were identified to be homogeneous and their molecular weights were estimated to be about 15,000 and 8,700, respectively. FCW-Ia consisted of fucose, galactose, and mannose as main sugars and their molar ratio was 19.5 : 63.2 : 25.0. Protein was not detected in FCW-Ia. However, FCW-IIa was composed of glucose, galactose, and mannose at a molar ratio of 1.0 : 0.3 : 0.4 and contained 0.4% protein with a higher amount of glutamic acid. A small amount of uronic acid was detected in both FCW-Ia and FCW-IIa.

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A Study on the Development of Soil-based PTMs for Analysis of Benzo[a]pyrene - Focusing on the Evaluation of Homogeneity and Stability for the Certification of Benzo[a]pyrenecandidate Reference Materials - (Benzo[a]pyrene 분석용 토양 숙련도 표준시료 개발에 관한 연구 - 후보 표준물질의 인증을 위한 균질성, 안정성 평가를 중심으로 -)

  • Lee, Minhyo;Lee, Guntaek;Joo, Changkyu;Kim, Yonghun;Lee, Bupyoel;Choe, Sunghun;Kim, Myeongock;Hong, Sukyoung;Kim, Gumhee;Lee, Wonseok
    • Journal of Soil and Groundwater Environment
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    • v.19 no.6
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    • pp.49-58
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    • 2014
  • This study was implemented as a part of the experiment to develop two kinds of soil-based Benzo[a]pyrene (BaP) proficiency testing materials (PTMs) for soil analysis. A test was carried out for the check of solubility of the reference material (high purity reagent) using several solvents. Another test was also conducted for the evaluation of homogeneity and stability of two kinds of candidate soil reference materials. The test analysis of BaP in terms of the candidate materials was conducted according to the Standard Soil Analytical Methods by Ministry of Environment. Dissolution of the reference material was shown to vary depending on solvent type and was higher in the order of Dichloromethane > Acetone > Acetone/MeOH (9 : 1) > N-hexane. In addition, the slope on calibration curve for BaP standard solutions was largest on BaP standard solutions prepared with dichloromethane of the tested solvents. Such tendency appeared egually in the commercial BaP standard solution. Therefore, it is thought to be reasonable to use dichloromethane as the solvent in case of the standard stock solution that is used for the measurement of BaP concentration in soil. ISO 13528 and IUPAC protocol were used for verification of homogeneity on the two kinds of soil candidate materials, Both candidate materials were sufficiently homogeneous. Stability assessment of the two candidate materials was made according to ISO Guide 35 and the result showed that both batches did not have any long-term and short term stability issues that might occur during shipping. However, monitoring results of BaP concentration in soil showed that BaP concentration of the two batches measured at 15 days after the sample preparation was reduced by about 24~37% compared with that of the samples measured on 0 day of the sample preparation. Identification was done with several treatments such as irradiation and sterilization etc. The major cause was shown to be irradiation to the samples.

Synthesis of akermanite bioceramics by solid-state reaction and evaluation of its bioactivity (고상반응법에 의한 아커마나이트 분말의 합성 및 생체활성도 평가)

  • Go, Jaeeun;Lee, Jong Kook
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.5
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    • pp.191-198
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    • 2022
  • Zirconia and titanium alloys, which are mainly used for dental implant materials, have poor osseointegration and osteogenesis abilities due to their bioinertness with low bioactivity on surface. In order to improve their surface bioinertness, surface modification with a bioactive material is an easy and simple method. In this study, akermanite (Ca2MgSi2O7), a silicate-based bioceramic material with excellent bone bonding ability, was synthesized by a solid-state reaction and investigated its bioactivity from the analysis of surface dissolution and precipitation of hydroxyapatite particles in SBF solution. Calcium carbonate (CaCO3), magnesium carbonate (MgCO3), and silicon dioxide (SiO2) were used as starting materials. After homogeneous mixing of starting materials by ball milling and the drying of at oven, uniaxial pressing was performed to form a compacted disk, and then heat-treated at high temperature to induce the solid-state reaction to akermanite. Bioactivity of synthesized akermanite disk was evaluated with the reaction temperature from the immersion test in SBF solution. The higher the reaction temperature, the more pronounced the akermanite phase and the less the surface dissolution at particle surface. It resulted that synthesized akermanite particles had high bioactivity on particle surface, but it depended on reacted temperature and phase composition. Moderate dissolution occurred at particle surfaces and observed the new precipitated hydroxyapatite particles in synthetic akermanite with solid-state reaction at 1100℃.

A Nuclide Transport Model in the Fractured Rock Medium Using a Continuous Time Markov Process (연속시간 마코프 프로세스를 이용한 균열암반매질에서의 핵종이동 모델)

  • Lee, Y.M.;Kang, C.H.;Hahn, P.S.;Park, H.H.;Lee, K.J.
    • Nuclear Engineering and Technology
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    • v.25 no.4
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    • pp.529-538
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    • 1993
  • A stochastic way using continuous time Markov process is presented to model the one-dimensional nuclide transport in fractured rock matrix as an extended study for previous work [1]. A nuclide migration model by the continuous time Markov process for single planar fractured rock matrix, which is considered as a transient system where a process by which the nuclide is diffused into the rock matrix from the fracture may be no more time homogeneous, is compared with a conventional deterministic analytical solution. The primary desired quantities from a stochastic model are the expected values and variance of the state variables as a function of time. The time-dependent probability distributions of nuclides are presented for each discretized compartment of the medium given intensities of transition. Since this model is discrete in medium space, parameters which affect nuclide transport could be easily incorporated for such heterogeneous media as the fractured rock matrix and the layered porous media. Even though the model developed in this study was shown to be sensitive to the number of discretized compartment showing numerical dispersion as the number of compartments are decreased, with small compensating of dispersion coefficient, the model agrees well to analytical solution.

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