• Title/Summary/Keyword: polymer synthesis and characterization

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Synthesis and Characterization of Nanocomposite Films Consisting of Vanadium Oxide and Microphase-separated Graft Copolymer

  • Choi, Jin-Kyu;Kim, Yong-Woo;Koh, Joo-Hwan;Kim, Jong-Hak;Mayes, Anne M.
    • Macromolecular Research
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    • v.15 no.6
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    • pp.553-559
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    • 2007
  • Nanocomposite films were prepared by sol-gel synthesis from vanadium triisopropoxide with $poly((oxyethylene)_9$ methacrylate)-graft-poly(dimethyl siloxane), POEM-g-PDMS, producing in situ growth of vanadium oxide within the continuous ion-conducting POEM domains of micro phase-separated graft copolymer. The formation of vanadium oxide was confirmed by wide angle x-ray scattering (WAXS) and Fourier transform infrared (FT-IR) spectroscopy. Small angle x-ray scattering (SAXS) revealed the spatially-selective incorporation of vanadium oxide in the POEM domains. Upon the incorporation of vanadium oxide, the domain periodicity of the graft copolymer monotonously increased from 17.2 to 21.0 nm at a vanadium content 14 v%, above which it remained almost invariant. The selective interaction of vanadium oxide with POEM was further verified by differential scanning calorimetry (DSC) and FT-IR spectroscopy. The nanocomposite films exhibited excellent mechanical properties $(l0^{-5}-10^{-7}dyne/cm^2)$, mostly due to the confinement of vanadium oxide in the POEM chains as well as the interfaces created by the microphase separation of the graft copolymer.

Synthesis and Electrochemical Characterization of Polyaniline/Poly[1,2]bis-thio[1,8]-naphthylidine Composite as Polymer Cathode Material (Polyaniline/Poly[1,2]bis-thio[1,8]-naphthylidine 복합체 고분자 양극재료의 합성과 전기화학적 특성)

  • Oh, Ji-Woo;Ryu, Kwang-Sun
    • Journal of the Korean Electrochemical Society
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    • v.15 no.4
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    • pp.222-229
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    • 2012
  • We studied the electrochemical phenomena and increase of capacity according to the polymer composite electrode of two different polymeric materials with different the voltage range and capacity. Polyaniline (PANI) with relatively high voltage and small capacity and poly [1,2] bis-thio[1,8]-naphthylidine (PTND) with slightly low voltage and large capacity were used as polymer composite electrode materials. After PTND was synthesized, PANI was synthesized on the surface of PTND. The synthesis and the fine structure were analyzed by FT-IR, XPS, FE-SEM, and FE-TEM. Charge/discharge capacity and cyclic voltammetry measurements were carried out for the electrochemical performance as a polymer cathode active material for lithium secondary batteries. The discharge capacities of PANI/PTND after 1,5, and 10 cycles at 1.3~4.0 V voltage range and room temperature 167 mAh/g, 90 mAh/g, and 81 mAh/g. When we compared with PANI (80, 67, and 62 mAh/g), the discharge capacity after 10 cycles was improved about 30%. After 50 cycles, the discharge capacity of PANI/PTND was 67 mAh/g.

Facile Low-temperature Chemical Synthesis and Characterization of a Manganese Oxide/multi-walled Carbon Nanotube Composite for Supercapacitor Applications

  • Jang, Kihun;Lee, Sung-Won;Yu, Seongil;Salunkhe, Rahul R.;Chung, Ildoo;Choi, Sungmin;Ahn, Heejoon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.10
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    • pp.2974-2978
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    • 2014
  • $Mn_3O_4$/multi-walled carbon nanotube (MWCNT) composites are prepared by chemically synthesizing $Mn_3O_4$ nanoparticles on a MWCNT film at room temperature. Structural and morphological characterization has been carried out using X-ray diffraction (XRD) and scanning and transmission electron microscopies (SEM and TEM). These reveal that polycrystalline $Mn_3O_4$ nanoparticles, with sizes of about 10-20 nm, aggregate to form larger nanoparticles (50-200 nm), and the $Mn_3O_4$ nanoparticles are attached inhomogeneously on MWCNTs. The electrochemical behavior of the composites is analyzed by cyclic voltammetry experiment. The $Mn_3O_4$/MWCNT composite exhibits a specific capacitance of $257Fg^{-1}$ at a scan rate of $5mVs^{-1}$, which is about 3.5 times higher than that of the pure $Mn_3O_4$. Cycle-life tests show that the specific capacitance of the $Mn_3O_4$/MWCNT composite is stable up to 1000 cycles with about 85% capacitance retention, which is better than the pure $Mn_3O_4$ electrode. The improved supercapacitive performance of the $Mn_3O_4$/MWCNT composite electrode can be attributed to the synergistic effects of the $Mn_3O_4$ nanoparticles and the MWCNTs, which arises not only from the combination of pseudocapacitance from $Mn_3O_4$ nanoparticles and electric double layer capacitance from the MWCNTs but also from the increased surface area, pore volume and conducting property of the MWCNT network.

Synthesis, Characterization and Haemocompatibility of Poly(styrene-b-isobutylene-b-styrene) Triblock Copolymers (폴리(스티렌-이소부틸렌-스티렌) 삼중블록 공중합체의 합성, 분석 및 혈액적합성)

  • Ren, Ping;Wu, Yi-Bo;Guo, Wen-Ii;Li, Shu-Xin;Mao, Jing;Xiao, Fei;Li, Kang
    • Polymer(Korea)
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    • v.35 no.1
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    • pp.40-46
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    • 2011
  • The synthesis of well-defined poly(styrene-b-isobutylene-b-styrene) (SIBS) triblock copolymers was accomplished by cationic sequential block copolymerization of isobutylene (IB) with styrene (St) using 1,4-di(2-chloro-2-propyl) benzene (DCC) /$TiCl_4$/2,6-di-tert-butylpyridine(DtBP) as an initiating system in methyl chloride ($CH_3Cl$)/methylcyclohexane(MeChx) (50/50 v/v) solvent mixture at $-80^{\circ}C$. The triblock copolymers exhibited excellent thermoplastic and elastomeric characteristics. Tensile strengths and Shore hardness increased with increasing polystyrene (PS) content, while elongation at break decreased. The blood-compatibility of SIBS was assessed by SEM observation of the platelet adhesion, blood clotting time and haemolysis ratio. The haemolysis ratios were below 5% which met the medical materials standard. The platelet adhesion test further indicated that SIBS block copolymers had a good blood compatibility.

Synthesis and Characterization of Phosphoric Acid-doped Poly (2,5-benzimidazole) Membrane for High Temperature Polymer Electrolyte Membrane Fuel Cells (고온 고분자 연료전지용 인산 도핑 폴리(2,5-벤지이미다졸) 막의 제조 및 특성)

  • Nguyen, Thi Xuan Hien;Mishra, Ananta Kumar;Choi, Ji-Sun;Kim, Nam-Hoon;Lee, Joong-Hee
    • Transactions of the Korean hydrogen and new energy society
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    • v.23 no.1
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    • pp.26-33
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    • 2012
  • Phosphoric acid-doped poly (2,5-benzimidazole) (DABPBI) was prepared by condensation polymerization of 3,4-diaminobenzoic acid for high temperature proton electrolyte membrane fuel cells. The membranes were casted directly using a hot-press unit and characterized by fourier transform infrared spectroscopy, thermogravimetric analysis, conductivity measurement, scanning electron microscopy and tensile test. The proton conductivities of DABPBI are observed to be 0.062 and 0.018 $S{\cdot}cm^{-1}$ under 30 and 1% relative humidity, respectively at a temperature of $120^{\circ}C$ which is appreciably higher than that of Nafion 115 under similar conditions. The DABPBI membrane has demonstrated excellent thermo- mechanical properties and proton conductivity suggesting its suitability as a high temperature membrane.

One-Pot Reaction Involving Two Different Amines and Formaldehyde Leading to the Formation of Poly(Macrocyclic) Cu(II) Complexes

  • Lee, Yun-Taek;Kang, Shin-Geol
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2517-2522
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    • 2012
  • New polynuclear poly(hexaaza macrocyclic) copper(II) complexes $[1](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$, $[2](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$, and $[3](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$ have been prepared by the one-pot reaction of formaldehyde with ethylenediamine and 1,2-bis(2-aminoethoxy)ethane, 1,3-diaminopropane, or 1,6-diaminohexane in the presence of the metal ion. The polymer complexes contain fully saturated 14-membered hexaaza macrocyclic units (1,3,6,8,10,13-hexaazacyclotetradecane) that are linked by $N-(CH_2)_2-O-(CH_2)_2-O-(CH_2)_2-N$, $N-(CH_2)_3-N$, or $N-(CH_2)_6-N$ chains. The mononuclear complex $[Cu(H_2L^5)](ClO_4)_4$ ($H_2L^5$ = a protonated form of $L^5$) bearing two $N-(CH_2)_2-O-(CH_2)_2-O-(CH_2)_2-NH_2$ pendant arms has also been prepared by the metal-directed reaction of ethylenediamine, 1,2-bis(2-aminoethoxy)ethane, and formaldehyde. The polymer complexes were characterized employing elemental analyses, FT-IR and electronic absorption spectra, molar conductance, X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and scanning electron micrograph (SEM). Electronic absorption spectra of the complexes show that each macrocyclic unit of them has square-planar coordination geometry with a 5-6-5-6 chelate ring sequence. The polymer complexes as well as $[Cu(H_2L^5)]^{4+}$ are quite stable even in concentrated $HClO_4$ solutions. Synthesis and characterization of the polynuclear and mononuclear copper(II) complexes are reported.

Synthesis and Characterization of Thermoplastic Elastomer Poly(ether-b-amide) Containing Aromatic Moiety (방향족 구조가 포함된 열가소성 탄성체 Poly(ether-b-amide)의 합성 및 특성)

  • Lee, Ji Hun;Kim, Hyung Joong
    • Polymer(Korea)
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    • v.38 no.5
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    • pp.596-601
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    • 2014
  • Polyamide (PA) oligomers, which are the hard segment of poly(ether-block-amide) (PEBA), presenting thermoplastic and high performance elastomeric properties were prepared by polycondensation between 4-aminobenzoic acid and 12-aminododecanoic acid. Subsequently PEBAs were obtained by addition polymerization of the PA oligomers and various molecular weights of poly(tetramethylene glycol) (PTMG). The structure of the final PEBA was identified by using FTIR and $^1H$ NMR and the thermal properties depending on changes in the structure of hard segment were collected by using DSC and UTM analysis. As the results, the melt temperature ($T_m$), the initial modulus, and the maximum strength of PEBAs increased with an increase in aromatic moiety up to 30% without reducing crystallinity.

Synthesis and Characterization of Transparent Copolyimide Films (II) (투명한 공중합체 폴리이미드 필름의 합성 및 특성 연구(II))

  • Park, Jong-Su;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.33 no.4
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    • pp.313-318
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    • 2009
  • Copolyimides were synthesized from bis (3-aminophenyl) sulfone (APS) and 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) containing a fluorine substituent ($-CF_3$) with different mole ratios of 3,3',4,4'-diphenylsulfonetetracarboxylic dianhydride (DSDA) containing a sulfone group (-$SO_2$-). The PI films were obtained from poly (amic acid) (PAA) by solution casting through thermal imidization on a glass plate. Wide-angle X-ray diffraction (XRD), scanning electron microscopy (FE-SEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), universal tensile machine (UTM) measurements, and UV-Vis spectrometry were used to assess thermo-mechanical properties, morphology, and optical transparency. Thermal properties and optical transparency decreased with increasing DSDA mole fraction. In contrast, mechanical properties increased with increasing DSDA mole fraction. As compared to conventional PI films, however, the PI copolymer films in this work were found to exhibit better optical transparency.

Synthesis and Characterization of Transparent Copolyimide Films (I) (투명한 폴리이미드 공중합체 필름의 합성과 특성 연구 (I))

  • Park, Jong-Su;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.32 no.6
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    • pp.580-586
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    • 2008
  • Copolyimides were synthesized from 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and 1,3-bis(3-aminophenoxy)benzene (BAPB) with different mole ratios of 2,2-bis[4-(4-aminophenoxy)pheny1]hexafluoropropane (BAPP). The solution cast film of poly(amic acid) (PAA) was heat treated at different temperatures to create copolyimide films. The PI copolymer films were found to exhibit good optical transparencies. The thermomechanical properties, morphology, and optical transparency of PI films were examined using fourier transform infrared spectroscopy (FT-IR), wide-angle X-ray diffraction (XRD), scanning electron microscopes (SEM), differential scanning calorimeter(DSC), thermo-gravimetric analyzer (TGA), universal tensile machine (UTM), and IN - Vis. spectrometer. The glass transition temperature ($T_g$), ultimate strength, and initial modulus linearly increased with increasing BAPP mole fraction. However, thermal stability($T_D{^i}$) of the copolyimide remains constant regardless of BAPP loadings. It was found, however, that the optical transparency decreases slightly upon increasing the BAPP content because of the formation of the charge transfer complexes.

Synthesis and Characterization of Novel Aromatic Polyimides from Bis (3-aminophenyl) 3,5-bis (trifluorormethyl) phenyl Phosphine Oxide

  • Jeong, Kwang-Un;Kim, Jang-Joo;Yoon, Tae-Ho
    • Macromolecular Research
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    • v.8 no.5
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    • pp.215-223
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    • 2000
  • A novel diamine monomer, containing fluorine and phosphine oxide, bis(3-aminophenyl) 3,5-bis(trifluoromethyl)phenyl phosphine oxide (mDA6FPPO), was prepared via Grignard reaction, and utilized to prepare polyimides with dianhydrides such as PMDA, 6FDA, BTDA or ODPA, by the conventional two-step route; preparation of poly(amic acid), followed by solution imidization. The polyimides were characterized by FT-IR, NMR, and DSC with intrinsic viscosity and refractive index also being evaluated. A phosphine oxide containing monomer, bis(3-aminophenyl)phenyl phosphine oxide (mDAPPO) and a commercial 3,3-diaminodiphenyl sulfone (mDDS) were also used for comparison. The polyimides derived from mDA6FPPO exhibited high T$\sub$g/, excellent solubility and low birefringence.

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