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Two Crystal Structures of Dehydrated $Ag^{+}$- and $Ca^{2+}$-Exchanged Zeolite $A,\;Ag_{12-2x}Ca_x-A\;(x=2\;and\;3)$ Treated with Cesium Vapor (탈수한 $Ag^{+}$ 이온과 $Ca^{2+}$ 이온으로 치환한 제올라이트 $A,\;Ag_{12-2x}Ca_x-A\;(x=2\;and\;3)$를 Cs 증기로 처리한 결정구조)

  • Song, Seung Hwan;Kim, Yang
    • Journal of the Korean Chemical Society
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    • v.38 no.9
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    • pp.621-627
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    • 1994
  • Two crystal structures of dehydrated, $Ag^{+}$ and $Ca^{2+}$-exchanged zeolite A treated at $250^{\circ}C$ with 0.15 torr of Cs vapor have been determined by single-crystal X-ray diffraction technique in the cubic space group $Pm{\bar\3m$ at $21(1)^{\circ}C$ (a = 12.344(2) $\AA$ and 12.304(2) $\AA$). Their structures were refined to the final error indices, R (weighted), of 0.091 with 180 reflections, and 0.093 with 179 reflections, respectively, for which I > $3\sigma(I).$ In each structure, Cs species are found at four different crystallographic sites: 3 $Cs^{+}$ ions per unit cell are located at 8-ring centers, ca. 6.81∼7.14 $Cs^{+}$ ions are found on opposite 6-rings on threefold axes in the large cavity, ca. 1.93∼2.03 $Cs^{+}$ ions are found on threefold axes in the sodalite unit, and 0.53∼0.66 $Cs^{+}$ ions lie on opposite 4-rings. Also, ca. 4.12∼4.27 Ag atoms are located near the center of the large cavity. In these structures, excess cesium atoms in a unit cell are associated with other $Cs^{+}$ ions on a single threefold axis to form the linear cationic cluster $(Cs_4)^{3+}$. By blocking 8-rings, the $Cs^{+}$ ions may have prevented silver atoms from migrating out of the structure. The Ag atoms are likely to have formed hexasilver clusters at the centers of the large cavities. Each hexasilver cluster is stabilized by coordination to 14 $Cs^{+}$ ions.

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Synthesis, Structure and Electrical Properties of $Sr_1-_xY_xMnO_3$ System ($Sr_1-_xY_xMnO_3$의 합성 및 조성에 따른 결정구조와 전기적 성질변화)

  • Park, So Jeong;Kim, Seong Jin
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.785-791
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    • 1994
  • The $Sr_1-_xY_xMnO_3$ (x = 0.0∼1.0) system was synthesized using amorphous citrate process. The stability of various structures and the electronic transport properties of this system were investigated. X-ray diffraction study indicated that the $Sr_1-_xY_xMnO_3$ system has three different structures depending on composition, namely, 4L-hexagonal perovskite (when x is less than 0.3), pseudocubic perovskite (when x is 0.3∼0.7), and hexagonal nonperovskite (when x is larger than 0.7) structures. The structural changes and electronic properties were interpreted based on two factors, i.e., the size of cations and the oxidation state of manganese ion. When the concentration of Y substitution exceeds 30%, the Mn-Mn repulsive interaction dominates over intermetallic attraction, and thus structure changes to pseudocubic perovskite. In perovskite phase the unit cell dimensions increases with increasing $Mn^{3+}$ ions due to yttrium substitution. The band gap of $Sr_{0.9}Y_{0.1}MnO_3$ is greater than that of $Sr_{0.5}Y_{0.5}MnO_3$. The greater band gap of $Sr_{0.9}Y_{0.1}MnO_3$ indicates that the 4L-hexagonal structure is more stabilized than cubic perovskite due to the Mn-Mn bond.

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Physico-mechanical, AC-conductivity and microstructural properties of FeCl3 doped HPMC polymer films

  • Prakash, Y.;Somashekarappa, H.;Manjunath, A.;Mahadevaiah, Mahadevaiah;Somashekar, R.
    • Advances in materials Research
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    • v.2 no.1
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    • pp.37-49
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    • 2013
  • The transition metal salt doped solid polymer electrolyte [TSPE] were prepared with HPMC as a host polymer. The virgin and doped films were prepared by solution-casting method and investigated using wide angle X-ray scattering method. Micro structural parameters like lattice strain (g%), stacking/twin faults, the average number of unit cells counted in a direction perpendicular to the Bragg's plane (hkl) spacing of (hkl) planes dhkl, crystallite size Ds, distortion width, standard deviation were determined by whole pattern powder fitting (WPPF) method, which is an extension of single order method. It is found that the crystallite size decreases with the increase in the content of $FeCl_3$. This decrease is due to increase in localized breaking of polymer network which also accounts for the amorphous nature of the material. The filler inorganic salt $FeCl_3$ acts as plasticizer. FTIR study also confirms and justifies the interaction between the polymer and in-organic salt in the matrix. Physical properties like mechanical stability and Ac conductivity in these films are in conformity with the X-ray results.

Chemical Bonding Nature and Mesoporous Structure of Nickel Intercalated Montmorillonite Clay

  • Park, Hye-Mi;Kim, Tae-Woo;Hwang, Seong-Ju;Choy, Jin-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1323-1328
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    • 2006
  • Mesoporous nickel intercalated aluminosilicate nanohybrid has been synthesized through a recombination reaction between the colloidal suspension of exfoliated montmorillonite nanosheets and aqueous nickel acetate solution. According to powder X-ray diffraction and field emission-scanning electron microscopic analyses, the intercalation of nickel species expands significantly the basal spacing of the host montmorillonite clay and the crystallites of the intercalation compound are assembled to form a house-of-card structure. $N_2$ adsorption-desorption isotherm measurements with BJH pore analyses clearly demonstrated that the porosity of the intercalate originates mainly from mesopores (diameter $\sim50\;\AA$) formed by the house-of-card type stacking of clay crystallites. From FT-IR and X-ray absorption spectroscopic analyses, it becomes certain that intercalated nickel ion is stabilized in an isolated $NiO_6$ octahedral unit. The present mesoporous intercalation compound is expected to be applicable as efficient catalysts or absorbents.

Synthesis, Thermal Decomposition Pattern and Single Crystal X-Ray Studiesof Dimeric [Cu(dmae)(OCOCH3)(H2O)]2: A Precursor for the Aerosol Assisted Chemical Vapour Deposition of Copper Metal Thin Films

  • Mazhar, Muhammad;Hussain, S.M.;Rabbani, Faiz;Kociok-Kohn, Gabriele;Molloy, Kieran C.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.10
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    • pp.1572-1576
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    • 2006
  • A dimeric precursor, $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ for the CVD of copper metal films, (dmaeH = N,N-dimethylaminoethanol) was synthesized by the reaction of copper(II) acetate monohydrate ($Cu(OCOCH_3)_2{\cdot}H_2O$) and dmaeH in toluene. The product was characterized by m.p. determination, elemental analysis and X-ray crystallography. Molecular structure of $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ shows that a dimeric unit $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ is linked to another through hydrogen bond and it undergoes facile decomposition at 300 C to deposit granular copper metal film under nitrogen atmosphere. The decomposition temperature, thermal behaviour, kinetic parameters, evolved gas pattern of the complex, morphology, and the composition of the film were also investigated.

Synthesis and Characterization of PtPd and PtRuPd Anode Catalysts for Direct Methanol Fuel Cells

  • Horvath G.;Park K. W.;Sung Y. E.
    • 한국전기화학회:학술대회논문집
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    • 2002.07a
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    • pp.211-218
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    • 2002
  • In this study, Pt/Pd (1.1), PtPd (2:1) and PtPd (3:1) binary catalysts and Pt/Ru/Pd (5:4:1) ternary catalyst were designed. The catalysts were synthesized by impregnation method using $NaBH_4$ as a reducing agent. A good catalyst for methanol oxidation requires low on-set potential, stable durability and low activation energy. In order to investigate the catalytic activity for the methanol oxidation, electrochemical measurements such as cyclic voltammetry and chronoamperometry were peformed in sulfuric acid with/without methanol solution. In order to calculate the activation energy of the reaction, electrochemical measurements were also tested at different temperatures. For investigation of the structural analysis such as particle size and alloying, X-ray diffraction and transmission electron microscopy analysis were used. In order to identify the role of the Pd and to determine the composition of the surface of the Pt/Pd nanoparticles, X-ray photoelectron spectroscopy (XPS) analysis was investigated. The XPS spectra of Pd showed that Pd appears only as a metallic state in the binary catalysts. The chemical states of Pt in PtPd catalysts are both metallic and oxidative. Polarization curves and power density data were obtained by testing the DMFC unit cell performance of PtPd and PtRuPd catalysts. These data showed that Pt/Pd (2:1) and Pt/Ru/Pd (5:4:1) have better performance than Pt and Pt/Ru, respectively.

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Recycling of Waste Cellulose Biomass - I. Synthesis of Cellulose Acetate and Mehtylcellulose from Waste Cellulose - (폐 cellulose계 biomass 자원의 재활용 - I. 목면 폐기물로부터 cellulose acetate 및 methyl cellulose 합성 -)

  • 이성구;최길영;김수진;정우영;조순채;이종문
    • Textile Coloration and Finishing
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    • v.5 no.3
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    • pp.221-228
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    • 1993
  • Cellulose acetate and methyl cellulose were synthesized from waste cellulose in order to make waste knit on value added highly. Crystal waste cellulose by oxidation using $HIO_4$ and then acetylation was decrystallized. A degee of crystallinity was measured by X-ray diffraction and the structure was identified by FT-IR spetroscopy, respectively. Cellulose acetate was prepared from the reaction of decrystallized cellulose with acetic acid, cone-$H_{2}SO_{4}$ and acetic anhydride. Also, structure identification by FT-IR and a degree of crystallinity by X-ray diffraction were performed. DS of the synthesized cellulose acetate was 2.8 and viscosity average molecular weight was 238,000. Also, methyl cellulose was synthesized by treating cellulose acetate with NaOH and iodomethane. DS of the synthesized methyl cellulose was 3.0. Glucose unit with three hydroxy groups was all substituted by methoxyl groups. It was identified by FT-IR spectroscopy. Also, the thermal properties of the synthesized methyl cellulose were examined by DSC. It shewed two shewed melting peaks at 22$0^{\circ}C$ and 24$0^{\circ}C$ in the 2nd scan. It proved that DS=3.0 of methyl cellulose was a thermotropic liquid crystal.

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Idiopathic acute eosinophilic pneumonia in a 14-month-old girl

  • Park, Ha Neul;Chung, Bo Hyun;Pyun, Jung Eun;Lee, Kwang Chul;Choung, Ji Tae;Lim, Choon Hak;Yoo, Young
    • Clinical and Experimental Pediatrics
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    • v.56 no.1
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    • pp.37-41
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    • 2013
  • Idiopathic acute eosinophilic pneumonia (IAEP), characterized by acute febrile respiratory failure associated with diffuse radiographic infiltrates and pulmonary eosinophilia, is rarely reported in children. Diagnosis is based on an association of characteristic features including acute respiratory failure with fever, bilateral infiltrates on the chest X-ray, severe hypoxemia and bronchoalveolar lavage fluid >25% eosinophils or a predominant eosinophilic infiltrate in lung biopsies in the absence of any identifiable etiology. We present a 14-month-old girl who was admitted to our pediatric intensive care unit because of acute respiratory distress. She had a fever, dry cough, and progressive dyspnea for 1 day. Chest X-ray showed multifocal consolidations, increased interstitial markings, parenchymal emphysema and pneumothorax. IAEP was confirmed by marked pulmonary infiltrates of eosinophils in the lung biopsy specimen. Most known causes of acute eosinophilic pneumonia, such as exposure to causative drugs, toxins, second-hand smoking and infections were excluded. Her symptoms were resolved quickly after corticosteroid therapy.

Overexpression, Purification, and Preliminary X-ray Crystallographic Analysis of Human Brain-Type Creatine Kinase

  • Bong, Seung-Min;Moon, Jin-Ho;Jang, Eun-Hyuk;Lee, Ki-Seog;Chi, Young-Min
    • Journal of Microbiology and Biotechnology
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    • v.18 no.2
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    • pp.295-298
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    • 2008
  • Creatine kinase (CK; E.C. 2.7.3.2) is an important enzyme that catalyzes the reversible transfer of a phosphoryl group from ATP to creatine in energy homeostasis. The brain-type cytosolic isoform of creatine kinase (BB-CK), which is found mainly in the brain and retina, is a key enzyme in brain energy metabolism, because high-energy phosphates are transfered through the creatine kinase/phosphocreatine shuttle system. The recombinant human BB-CK protein was overexpressed as a soluble form in Escherichia coli and crystallized at $22^{\circ}C$ using PEG 4000 as a precipitant. Native X-ray diffraction data were collected to $2.2{\AA}$ resolution using synchrotron radiation. The crystals belonged to the tetragonal space group $P4_32_12$, with cell parameters of a=b=97.963, $c=164.312{\AA},\;and\;{\alpha}={\beta}={\gamma}=90^{\circ}$. The asymmetric unit contained two molecules of CK, giving a crystal volume per protein mass $(V_m)$ of $1.80{\AA}^3\;Da^{-1}$ and a solvent content of 31.6%.

Interfacial Stability Between Anode and Electrolyte of LSGM-Based SOFCs (LSGM계 고체산화물 연료전지의 전해질-음극 사이의 계면안정성)

  • Kim, Kwang-Nyeon;Moon, Jooho;Son, Ji-Won;Kim, Joosun;Lee, Hae-Weon;Lee, Jong-Ho;Kim, Byung-Kook
    • Journal of the Korean Ceramic Society
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    • v.42 no.7 s.278
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    • pp.509-515
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    • 2005
  • Interfacial reactions at LSGM electrolyte and NiO-GDC anode interfaces were thoroughly investigated with Environmental Scanning Electron Microscopy (ESEM-PHlLIPS XL-30) and Energy Dispersive X-ray (EDX-Link XL30). According to the analysis, serious reaction zone was observed at LSGM/NiO-GDC interface. It was found that the reaction layer was originated from the chemical reaction between NiO and LSGM. The reaction products were identified as La deficient form of LSGM based perovskite and Ni-La-O compounds such as LaSrGa$_{3}$O$_{7}$ and LaNiO$_{3}$ from the X-Ray Diffraction (XRD, Philips) analysis. According to the electrical characterization, interfacial layer was very electrically resistive which would be the cause of high internal resistance and low power generating characteristic of the unit cell.