• Title/Summary/Keyword: Synthesis of $LiCoO_2$

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In Situ-DRIFTS Study of Rh Promoted CuCo/Al2O3 for Ethanol Synthesis via CO Hydrogenation

  • Li, Fang;Ma, Hongfang;Zhang, Haitao;Ying, Weiyong;Fang, Dingye
    • Bulletin of the Korean Chemical Society
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    • v.35 no.9
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    • pp.2726-2732
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    • 2014
  • The promoting effect of rhodium on the structure and activity of the supported Cu-Co based catalysts for CO hydrogenation was investigated in detail. The samples were characterized by DRIFTS, $N_2$-adsorption, XRD, $H_2$-TPR, $H_2$-TPD and XPS. The results indicated that the introduction of rhodium to Cu-Co catalysts resulted in modification of metal dispersion, reducibility and crystal structure. DRIFTS results of CO hydrogenation at reaction condition (P=2 MPa, $T=260^{\circ}C$) indicated the addition of 1 wt % rhodium improved hydrogenation ability of Cu-Co catalysts. The ethanol selectivity and CO conversion were both improved by 1 wt % Rh promoted Cu-Co based catalysts. The alcohol distribution over un-promoted and rhodium promoted Cu-Co based catalysts obeys A-S-F rule and higher chain growth probability was got on rhodium promoted catalyst.

A Study on Co-precipitation of Positive Electrode Active Material for Recycled Lithium-ion Batteries Using Black Powder Leaching Solution (블랙 파우더 침출용액을 이용한 재활용 리튬이온전지의 양극 활물질 공침법에 대한 연구)

  • JAEGEUN LEE;JAEKYUNG LEE;SUNGGI KWON;GYECHOON PARK
    • Journal of Hydrogen and New Energy
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    • v.35 no.3
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    • pp.336-344
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    • 2024
  • In this study, a Ni0.9Co0.05Mn0.05(OH)2 precursor used as an anode active material using a black powder leaching solution of a recycled lithium ion battery was prepared through coprecipitation synthesis with co-precipitation time, NH4OH concentration, pH, and stirring time as variables. The characteristics of the prepared powder were analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM), particle size analysis (PSA), and inductively coupled plasma optical emission spectroscopy (ICP-OES). It was confirmed that the single crystal thickness of the LiNi1-x-yCoxMnyO2 (NCM) precursor changes depending on the NH4OH concentration and reaction pH value, and thicker single crystals are formed at 2 M NH4OH compared to 1 M and at pH 10.8-11.8 compared to pH 11.8-12.0. NCM precursor particles increased with coprecipitation time, and it was confirmed that the 72 hours NCM precursor had the largest particle size. Through ICP-OES analysis, it was confirmed that the NCM precursor was synthesized with the target composition of Ni2+:Co2+:Mn2+=90:5:5.

Synthesis of Multi-component Olivine by a Novel Mixed Transition Metal Oxalate Coprecipitation Method and Electrochemical Characterization

  • Park, Yeong-Uk;Kim, Jong-Sun;Gwon, Hyeok-Jo;Seo, Dong-Hwa;Kim, Seong-Uk;Hong, Ji-Hyeon;Gang, Gi-Seok
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2010.05a
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    • pp.37.1-37.1
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    • 2010
  • The multi-component olivine cathode material, $LiMn_{1/3}Fe_{1/3}Co_{1/3}PO_4$, was prepared via a novel coprecipitation method of the mixed transition metal oxalate, $Mn_{1/3}Fe_{1/3}Co_{1/3}(C_2O_4){\cdot}2H_2O$. The stoichiometric ratio and distribution of transition metals in the oxalate, therefore, in the olivine product, was affected sensitively by the environments in the coprecipitation process, while they are the important factors in determining the electrochemical property of electrode materials with multiple transition metals. The effect of the pH, atmosphere, temperature, and aging time was investigated thoroughly with respect to the atomic ratio of transition metals, phase purity, and morphology of the mixed transition metal oxalate. The electrochemical activity of each transition metal in the olivine synthesized through this method clearly was enhanced as indicated in the cyclic voltammetry (CV) and galvanostatic charge/discharge measurement. Three distinctive contributions from Mn, Fe, and Co redox couples were detected reversibly in multiple charge and discharge processes. The first discharge capacity at the C/5 rate was $140.5\;mAh\;g^{-1}$ with good cycle retention. The rate capability test showed that the high capacity still is retained even at the 4C and 6C rates with 102 and $81\;mAh\;g^{-1}$, respectively.

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Synthesis and Solution Properties of Zwitterionic Copolymer of Acrylamide with 3-[(2-Acrylamido)dimethylammonio]propanesulfonate

  • Xiao, Hui;Hu, Jing;Jin, Shuailin;Li, Rui Hai
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2616-2622
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    • 2013
  • A novel zwitterionic monomer 3-[(2-acrylamido)dimethylammonio]propanesulfonate (DMADAS) was designed and synthesized in this study. Then it was polymerized with acrylamide (AM) by free radical polymerization in 0.5 mol/L NaCl solution with ammonium persulfate ($(NH_4)_2S_2O_8$) and sodium sulfate ($NaHSO_3$) as initiator. The structure and composition of DMADAS and acrylamide-3-[(2-acrylamido)-dimethylammonio]propanesulfonate copolymer (P-AM-DMADAS) were characterized by FT-IR spectroscopy, $^1H$ NMR and elemental analyses. Isoelectric point (IEP) of P-AM-DMADAS was tested by nanoparticle size and potential analyzer. Solution properties of copolymer were studied by reduced viscosity. Antipolyelectrolyte behavior was observed and was found to be enhanced with increasing DMADAS content in copolymer. The results showed that the viscosity of P-AM-DMADAS is 5.472 dl/g in pure water. Electrolyte was added, which weakened the mutual attraction between sulfonic acid group and quaternary ammonium group. The conformation became loose, which led to the increase of reduced viscosity. The ability of monovalent and divalent cation influencing the viscosity of zwitterionic copolymer obeyed the following sequence: $Li^+$ < $Na^+$ < $K^+$, $Mg^{2+}$ < $Ca^{2+}$ < $Ba^{2+}$, and that of anion is in the order: $Cl^-$ < $Br^-$ < $I^-$, $CO{_3}^{2-}$ > $SO{_3}^{2-}{\approx}SO{_4}^{2-}$.

Cobalt Oxide-Tin Oxide Composite: Polymer-Assisted Deposition and Gas Sensing Properties (PAD법으로 제작된 산화코발트-산화주석 복합체의 가스 감응 특성)

  • An, Sea-Yong;Li, Wei;Jang, Dong-Mi;Jung, Hyuck;Kim, Do-Jin
    • Korean Journal of Materials Research
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    • v.20 no.11
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    • pp.611-616
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    • 2010
  • A cobalt oxide - tin oxide nanocomposite based gas sensor on an $SiO_2$ substrate was fabricated. Granular thin film of tin oxide was formed by a rheotaxial growth and thermal oxidation method using dc magnetron sputtering of Sn. Nano particles of cobalt oxide were spin-coated on the tin oxide. The cobalt oxide nanoparticles were synthesized by polymer-assisted deposition method, which is a simple cost-effective versatile synthesis method for various metal oxides. The thickness of the film can be controlled over a wide range of thicknesses. The composite structures thus formed were characterized in terms of morphology and gas sensing properties for reduction gas of $H_2$. The composites showed a highest response of 240% at $250^{\circ}C$ upon exposure to 4% $H_2$. This response is higher than those observed in pure $SnO_2$ (90%) and $Co_3O_4$ (70%) thin films. The improved response with the composite structure may be related to the additional formation of electrically active defects at the interfaces. The composite sensor shows a very fast response and good reproducibility.

Preparation and Electrochemical Properties of Freestanding Flexible S/CNT/NiO Electrodes for Li-S Batteries (리튬-황 전지용 프리스탠딩 플렉서블 S/CNT/NiO 전극의 제조 및 전기화학적 특성)

  • Shin, Yun Jung;Lee, Won Yeol;Kim, Tae Yun;Moon, Seung-Guen;Jin, En Mei;Jeong, Sang Mun
    • Korean Chemical Engineering Research
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    • v.60 no.2
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    • pp.184-192
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    • 2022
  • Porous NiO synthesized via hydrothermal synthesis was used in the electrodes of lithium-sulfur batteries to inhibit the elution of lithium polysulfide. The electrode of the lithium-sulfur battery was manufactured as a freestanding flexible electrode using an economical and simple vacuum filtration method without a current collector and a binder. The porous NiO-added S/CNT/NiO electrode exhibited a high initial discharge capacity of 877 mA h g-1 (0.2 C), which was 125 mA h g-1 higher than that of S/CNT, and also showed excellent retention of 84% (S/CNT: 66%). This is the result of suppressing the dissolution of lithium polysulfide into the electrolyte by the strong chemical bond between NiO and lithium polysulfide during the charging and discharging process. In addition, for the flexibility test of the S/CNT/NiO electrode, the 1.6 × 4 cm2 pouch cell was prepared and exhibited stable cycle characteristics of 620 mA h g-1 in both the unfolded and folded state.

Efficient Synthesis of hypho-2,5-$S_2B_7H_{11}$ and Preparation of New nido-, arachno-, and hypho-Metalladithiaborane Clusters Derived from Its Anion hypho-$S_2B_7H_{10}{^-}$

  • 강창환;김성준;고재정;강상욱
    • Bulletin of the Korean Chemical Society
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    • v.16 no.11
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    • pp.1067-1074
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    • 1995
  • Reaction of arachno-S2B7H8- with either THF or 1,2-dimethoxyethane upon refluxing condition results in the formation of the previously known compound hypho-S2B7H10-. Protonation of hypho-S2B7H10- with HCl/Et2O generates hypho-2,5-S2B7H11 in good yield. This hypho-S2B7H10- anion has been employed to generate a series of new nido-, arachno-, and hypho-metalladithiaborane clusters. Reaction of the anion with Cp(CO)2FeCl results in direct metal insertion and the formation of a complex containing the general formula (η5-C5H5)FeS2B7H8. Spectroscopic studies of nido-6-CpFe-7,9-S2B7H8 Ⅰ demonstrated that compound Ⅰ was shown to have an nido-type cage geometry derived from an octadecahedron missing one vertex, with the iron atom occupying the three-coordinate 6-position in the cage and the two sulfurs occupying positions on the open face of the cage. Reaction of hypho-S2B7H10- with CoCl2/Li+[C5H5]- gave the previously known complex arachno-7-CpCo-6,8-S2B6H8 Ⅱ. Also, the reaction of the anion with [Cp*RhCl2]2 gave the complex arachno-7-Cp*Rh-6,8-S2B6H8 Ⅲ, the structure of which was shown to be that of complex Ⅱ. The similarity of the NMR spectra of Ⅱ and Ⅲ suggest that Ⅲ adopts cage structure similar to that previously confirmed for Ⅱ. A series of 9-vertex hypho clusters in which the sulfur atoms are bridged by different species isoelectronic with a BH3 unit, such as HMn(CO)4 or SiR2 have been prepared. Compounds Ⅳ,Ⅴ and Ⅵ are each 2n+4 skeletal electron systems and would be expected according to skeletal electron counting theory to adopt hypho-type polyhedral structures derived from an icosahedron missing three vertices. The complex hypho-1-(CO)4Mn-2,5-S2B6H9 Ⅳ was obtained by the reaction of the anion with (CO)5MnBr and has been shown from spectroscopic data to consist of a (CO)4Mn fragment bound to the two sulfur atoms S2 and S5 of hypho-S2B7H10-. Also, similar hypho-type complexes hypho-1-R2Si-2,5-S2B6H8 (R=CH3 Ⅴ, R=C6H5 Ⅵ) have been prepared from the reaction of hypho-S2B7H10- with R2SiHCl.

Investigation of direct growth behavior of carbon nanotubes on cathode powder materials in lithium-ion batteries (리튬이차전지 양극 분말 소재 위 탄소나노튜브의 직접 성장 거동 고찰)

  • Hyun-Ho Han;Jong-Hwan Lee;Goo-Hwan Jeong
    • Journal of Surface Science and Engineering
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    • v.57 no.1
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    • pp.22-30
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    • 2024
  • This study reports a direct growth of carbon nanotubes (CNTs) on the surface of LiCoO2 (LCO) powders to apply as highly efficient cathode materials in lithium-ion batteries (LIB). The CNT synthesis was performed using a thermal chemical vapor deposition apparatus with temperatures from 575 to 625 ℃. Ferritin molecules as growth catalyst of CNTs were mixed in deionized (DI) water with various concentrations from 0.05 to 1.0 mg/mL. Then, the LCO powders was dissolved in the ferritin solution at a ratio of 1g/mL. To obtain catalytic iron nanoparticles on the LCO surface, the LCO-ferritin suspension was dropped in silicon dioxide substrates and calcined under air at 550℃. Subsequently, the direct growth of CNTs on LCO powders was performed using a mixture of acetylene (10 sccm) and hydrogen (100 sccm) for 10 min. The growth behavior was characterized by scanning and transmission electron microscopy, Raman scattering spectroscopy, X-ray diffraction, and thermogravimetric analysis. The optimized condition yielding high structural quality and amount of CNTs was 600 ℃ and 0.5 mg/mL. The obtained materials will be developed as cathode materials in LIB.

Radiosynthesis of $[^{11}C]6-OH-BTA-1$ in Different Media and Confirmation of Reaction By-products. ($[^{11}C]6-OH-BTA-1$ 조제 시 생성되는 부산물 규명과 반응용매에 따른 표지 효율 비교)

  • Lee, Hak-Jeong;Jeong, Jae-Min;Lee, Yun-Sang;Kim, Hyung-Woo;Lee, Eun-Kyoung;Lee, Dong-Soo;Chung, June-Key;Lee, Myung-Chul
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.3
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    • pp.241-246
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    • 2007
  • Purpose: $[^{11}C]6-OH-BTA-1$ ([N-methyl-$^{11}C$]2-(4'-methylaminophenyl)-6-hydroxybenzothiazole, 1), a -amyloid imaging agent for the diagnosis of Alzheimer's disease in PET, can be labeled with higher yield by a simple loop method. During the synthesis of $[^{11}C]1$, we found the formation of by-products in various solvents, e.g., methylethylketone (MEK), cyclohexanone (CHO), diethylketone (DEK), and dimethylformamide (DMF). Materials and Methods: In Automated radiosynthesis module, 1 mg of 4-aminophenyl-6-hydroxybenzothiazole (4) in 100 l of each solvent was reacted with $[^{11}C]methyl$ triflate in HPLC loop at room temperature (RT). The reaction mixture was separated by semi-preparative HPLC. Aliquots eluted at 14.4, 16.3 and 17.6 min were collected and analyzed by analytical HPLC and LC/MS spectrometer. Results: The labeling efficiencies of $[^{11}C]1$ were $86.0{\pm}5.5%$, $59.7{\pm}2.4%$, $29.9{\pm}1.8%$, and $7.6{\pm}0.5%$ in MEK, CHO, DEK and DMF, respectively. The LC/MS spectra of three products eluted at 14.4, 16.3 and 17.6 mins showed m/z peaks at 257.3 (M+1), 257.3 (M+1) and 271.3 (M+1), respectively, indicating their structures as 1, 2-(4'-aminophenyl)-6-methoxybenzothiazole (2) and by-product (3), respectively. Ratios of labeling efficiencies for the three products $([^{11}C]1:[^{11}C]2:[^{11}C]3)$ were $86.0{\pm}5.5%:5.0{\pm}3.4%:1.5{\pm}1.3%$ in MEK, $59.7{\pm}2.4%:4.7{\pm}3.2%:1.3{\pm}0.5%$ in CHO, $9.9{\pm}1.8%:2.0{\pm}0.7%:0.3{\pm}0.1%$ in DEK and $7.6{\pm}0.5%:0.0%:0.0%$ in DMF, respectively. Conclusion: The labeling efficiency of $[^{11}C]1$ was the highest when MEK was used as a reaction solvent. As results of mass spectrometry, 1 and 2 were conformed. 3 was presumed.