• Title/Summary/Keyword: Differential scanning calorimetry (DSC)

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Preparation of Poly(vinylidene fluoride)-g-poly(methacrylic acid) Composite Nanofiltration Membrane

  • Kim, Yong-Woo;Choi, Jin-Kyu;Koh, Joo-Hwan;Kim, Jong-Hak
    • Korean Membrane Journal
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    • v.9 no.1
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    • pp.57-63
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    • 2007
  • Amphiphilic graft copolymer from poly(vinylidene fluoride) (PVDF) was synthesized using atom transfer radical polymerization (ATRP) for composite nanofiltration membranes. Direct initiation of the secondary fluorinated site of PVDF facilitates grafting of tert-butyl methacrylate (tBMA). Amphiphilic PVDF-g-PMAA graft copolymer with a 51:49 wt ratio was obtained by hydrolyzing poly(tert-butyl methacrylate) (PtBMA) to poly(methacrylic acid) (PMAA). Wide angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) confirmed the decrease of crystallinity of PVDF upon graft copolymerization. Composite nanofiltration membranes were prepared from PVDF-g-PMAA as a top layer coated onto PVDF ultrafiltration (UF) support membrane. The morphology and hydrophilicity of membranes were characterized using scanning electron microscopy (SEM) and contact angle measurement. The rejections of composite membranes were 80.2% for $Na_2SO_4$ and 28.4% for NaCl, and the solution flux were 9.5 and $14.5\;L/m^2\;h$ at 1.0 MPa pressure.

Structural Changes of Biodegradable Poly(tetramethylene succinate) on Hydrolysis

  • Shin, Jick-Soo;Yoo, Eui-Sang;Im, Seung-Soon;Song, Hyun-Hoon
    • Macromolecular Research
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    • v.9 no.4
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    • pp.210-219
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    • 2001
  • Quenched and slow cooled as well as isothermally crystallized poly(tetramethylene succinate)(PTMS) films at two different temperatures were prepared. In the process of hydrolysis of the four specimens, structural changes such as the crystallinity, crystal size distribution, lattice parameter, lamellar thickness, long period and surface morphology were investigated by using wide and small angle X-ray scattering (WAXS and SAXS), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). The hydrolytic degradation of quenched film was faster than that of slow cooled and isothermally crystallized films. The film crystallized at 100$\^{C}$ exhibited extensive micro voids and thus showed faster degradation than that crystallized at 75$\^{C}$, demonstrating surface morphology is another important factor to govern degradation rate. The crystallinity of the specimen increased by 5-10% and long period decreased after hydrolysis for 20 days. At the initial stage of degradation, the lamellar thickness of quenched film rather increased, while that of slow cooled and isothermally crystallized films decreased. The hydrolytic degradation preferentially occurred in the amorphous region. The hydrolytic degradation in crystal lamellae are mainly at the crystal surfaces.

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Molecular Structure and Gelatinization Properties of Turnip Starch (Brassica rapa L.)

  • Kim, Nam-Hee;Yoo, Sang-Ho
    • Food Science and Biotechnology
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    • v.14 no.4
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    • pp.470-473
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    • 2005
  • Starch was isolated from turnip (Brassica rapa L.), and to elucidate the structure-function relationship its structural and physical properties were characterized. Morphological structure of the starch was analyzed by SEM (Scanning Electron Microscopy). Most of the starch granules were spherical in shape with diameter ranging from 0.5-10mm. Apart from larger granules ($<10\;{\mu}m$) which dominated the population size of turnip starch, significant amount of small ($0.5-2\;{\mu}m$) and mid-size granules (${\sim}\;{\mu}m$) were also detected. It was revealed that presumably, erosion damages occurred due to the attack of amylase-type enzymes on the surface of some granules. Branch chain-length distribution was analyzed by HPAEC (High-Performance Anion-Exchange Chromatography). The chain-length distribution of turnip starch revealed a peak at DP12 with obvious shoulder at DP18-21. The weight-average chain length ($CL_{avg}$) was 16.6, and a large proportion (11.8%) of very short chains (DP6-9) was also observed. The melting properties of starch were determined by DSC (Differential Scanning Calorimetry). The onset temperature ($T_o$) and the enthalpy change (${\Delta}H$) of starch gelatinization were $50.5^{\circ}C$ and 12.5 J/g, respectively. The ${\Delta}H$ of the retrograded turnip starch was 3.5 J/g, which indicates 28.2% of recrystallization. Larger proportion of short chains as well as smaller average chain-length can very well explain relatively lower degree of retrogradation in turnip starch.

A Study on Emulsion Copolymerization of $\alpha,\omega$-Diacrylate Poly(dimethylsiloxane) Containing Vinyl Ester of Versatic Acid/Vinyl Acetate (Versatic Acid/vinyl Acetate의 비닐 에스테르를 가지는 $\alpha$,$\omega$-Diacrylate Poly(dimethylsiloxane)의 에멀션 공중합 연구)

  • Naghash, Hamid Javaherian;Mallakpour, Shadpour;Forushani, Parivash Yavari;Uyanik, Nurseli
    • Polymer(Korea)
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    • v.32 no.2
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    • pp.95-102
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    • 2008
  • The $\alpha$,$omega$-diacrylate poly(dimethylsiloxane) (DA-PDMS) containing vinyl ester of versatic acid/vinyl acetate (Veova-10/VAc) was prepared by emulsion copolymerization of (DA-PDMS), Veova-10 (with VAc), and auxiliary agents at $85^{\circ}C$ in the presence of ammonium peroxodisulfate (APS) as an initiator. Sodium dodecyl sulfate (SDS) and nonylphenol ethylene oxide-40 units (NP-40) were used as anionic and nonionic emulsifiers, respectively. The resulting copolymers were characterized by using Fourier transform infrared spectroscopy (FT-IR). Thermal properties of the copolymers were studied by using thermogravimetric analysis(TGA) and differential scanning calorimetry (DSC). The morphology of copolymers was also investigated by scanning electron microscopy (SEM) and then the effects of variables such as temperature, agitation speed, surfactant kinds, molecular weights, initiator, and DA-PDMS concentrations on the properties of the silicone-containing Veova-10/VAc emulsions were examined. The calculation of monomer conversion versus time histories indicates that by increasing the DA-PDMS concentration the polymerization rate and the number of polymer particles decrease, respectively.

Effect of Surface-Modified Carbon Fiber on the Mechanical Properties of Carbon/Epoxy Composite for Bipolar Plate of PEMFC (표면처리 탄소섬유가 PEMFC용 탄소/에폭시 복합재료 분리판의 기계적 강도에 미치는 영향)

  • LEE, HONGKI;HAN, KYEONGSIK
    • Journal of Hydrogen and New Energy
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    • v.31 no.1
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    • pp.49-56
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    • 2020
  • Epoxy/carbon composite was used to prepare a bipolar plate for polymer electrolyte membrane fuel cell (PEMFC). Phenol novolac-type epoxy and diglycidyl ether of bisphenol A (DGEBA)-type epoxy mixture was used as a matrix and graphite powder, carbon fiber (CF) and graphite fiber (GF) were used as carbon materials. In order to improve the mechanical properties of the bipolar plate, surface-modified CF was incorporated into the epoxy/carbon composite. To determine the cure temperature of the epoxy mixture, differential scanning calorimetry (DSC) analysis was performed and the data were introduced to Kissinger equation in order to get reaction activation energy and pre-exponential factor. Tensile and flexural strength was obtained by using universal testing machine (UTM). The surface morphology of the fractured specimen and the interfacial morphology between epoxy matrix and CF or GF were observed by a scanning electron microscopy (SEM).

Preparation of Nanoparticles in Drug Delivery System Using Guar Derivatives and Dialysis Method

  • Na, Kun;Kim, Yu-Eun;Lee, Ki-Young
    • Journal of Microbiology and Biotechnology
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    • v.9 no.1
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    • pp.50-55
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    • 1999
  • To develop a new form of controlled release dosage for administering for indomethacin (IND), two formulations of IND-loaded nanoparticles were designed based on polysaccharide (guar) derivatives. Nanoparticles prepared by the dialysis method were characterized with respect to morphology, size distribution, drug content, and in vitro drug release. Morphological studies by scanning electron microscopy (SEM) indicated that guar acetate (GA) nanoparticles were spherical in shape and had a smooth surface. The particle size distributions of formulation I (40mg of GA) and formulation II (80mg of GA) were shown to be $250.78\pm185.13nm$ and $718\pm145.90nm$ in distilled water ($20$^{\circ}C$), respectively. The drug loading efficiencies of nanoparticles were approximately 26% and 31% for formulations I and II, respectively. The differential scanning calorimetry (DSC) results indicated that the IND was perfectly distributed within GA nanoparticles. We also found, from the X-ray diffractometry analysis, that a decrease in the degree of crystallinity of the drug occurred in the nanoparticles. No changes between the original IND and the released IND from GA nanoparticles were detected by FT-IR. Using guar acetate, it is possible to design nanoparticles which allow the controlled release of IND over an extended period of time.

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Morphology Evolution of Poly(L-lactic acid) (PLLA), Poly(ε-caprolactone) (PCL) and Polyethylene Oxide (PEO) Ternary Blend and Their Effects on Mechanical Properties for Bio Scaffold Applications (폴리락틱산, 폴리카프로락톤, 폴리에틸렌 옥사이드 삼성분계 블렌드의 형태학적 변화와 이들이 의료용 스캐폴더의 기계적 특성에 미치는 영향)

  • Ezzati, Peyman;Ghasemi, Ismaeil;Karrabi, Mohammad;Azizi, Hamed;Fortelny, Ivan
    • Polymer(Korea)
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    • v.38 no.4
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    • pp.449-456
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    • 2014
  • Ternary blends of poly(L-lactic acid) (PLLA), poly(${\varepsilon}$-caprolactone) (PCL) and polyethylene oxide (PEO) were produced with different concentrations of components via melt blending. By leaching the PEO from the samples by water, porous materials were obtained with potential application for bio scaffolds. Sample porosity was evaluated by calculating the ratio of porous scaffold density (${\rho}^*$) to the non-porous material density (${\rho}_s$). Highest porosity (51.42%) was related to the samples containing 50 wt%. of PEO. Scanning electron microscopy (SEM) studies showed the best porosity resulted by decreasing PLLA/PCL ratio at constant concentration of PEO. Crystallization behavior of the ternary blend samples was studied using differential scanning calorimetry (DSC). Results revealed that the crystallinity of PLLA was improved by addition of PEO and PCL to the samples. The porosity plays a key role in governing the compression properties. Mechanical properties are presented by Gibson-Ashby model.

Microstructural Change and Magnetic Properties of Nanocrystalline Fe-Si-B-Nb-Cu Based Alloys Containing Minor Elements

  • Nam, Seul-Ki;Moon, Sun-Gyu;Sohn, Keun Yong;Park, Won-Wook
    • Journal of Magnetics
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    • v.19 no.4
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    • pp.327-332
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    • 2014
  • The effect of minor element additions (Ca, Al) on microstructural change and magnetic properties of Fe-Nb-Cu-Si-B alloy has been investigated, in this paper. The Fe-Si-B-Nb-Cu(-Ca-Al) alloys were prepared by arc melting in argon gas atmosphere. The alloy ribbons were fabricated by melt-spinning, and heat-treated under a nitrogen atmosphere at $520-570^{\circ}C$ for 1 h. The soft magnetic properties of the ribbon core were analyzed using the AC B-H meter. A differential scanning calorimetry (DSC) was used to examine the crystallization behavior of the amorphous alloy ribbon. The microstructure was observed by X-ray diffraction (XRD), transmission electron microscope (TEM) and scanning electron microscope (SEM). The addition of Ca increased the electrical resistivity to reduce the eddy current loss. And the addition of Al decreased the intrinsic magnetocrystalline anisotropy $K_1$ resulting in the increased permeability. The reduction in the size of the ${\alpha}$-Fe precipitates was observed in the alloys containing of Ca and Al. Based on the results, it can be concluded that the additions of Ca and Al notably improved the soft magnetic properties such as permeability, coercivity and core loss in the Fe-Nb-Cu-Si-B base nanocrystalline alloys.

Re-synthesis and Electrochemical Characteristics of LiFePO4 Cathode Materials Recycled from Scrap Electrodes

  • Kim, Hyung Sun;Shin, Eun Jung
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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    • pp.851-855
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    • 2013
  • This paper describes an environmentally friendly process for the recovery of $LiFePO_4$ cathode materials from scrap electrodes by a simple thermal treatment method. The active materials were easily separated from the aluminum substrate foil and polymeric binders were also decomposed at different temperatures ($400^{\circ}C$, $500^{\circ}C$, $600^{\circ}C$) for 30 min under nitrogen gas flow. The samples were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM), Raman spectroscopy, Thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The electrochemical properties of the recycled $LiFePO_4$ cathode were evaluated by galvanostatic charge and discharge modes. The specific charge/discharge capacities of the recycled $LiFePO_4$ cathode were similar to those of the original $LiFePO_4$ cathode. The $LiFePO_4$ cathode material recovered at $500^{\circ}C$ exhibits a somewhat higher capacity than those of other recovered materials at high current rates. The recycled $LiFePO_4$ cathode also showed a good cycling performance.

Hydrogen Permeation Properties of Ni-based Amorphous Alloys Membrane (Ni-based 비정질 합금막의 수소투과 특성)

  • Seok, Song;Lee, Dock-Young;Kim, Yoon-Bae
    • Journal of Hydrogen and New Energy
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    • v.19 no.1
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    • pp.35-40
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    • 2008
  • Ni-based amorphous alloy ribbon was prepared by a single-roller melt-spinning technique. Palladium coating was found to enhance significantly the absorption/desorption behavior of hydrogen in amorphous alloy. The hydrogen permeability of a Pd-coated $(Ni_{60}Nb_{40}){_{100-X}}$TaX(x=5, 10) amorphous alloy was examined in the temperature range of $623{\sim}773K$, comparable with those of $Pd_{60}-Cu_{40}$ alloys. The permeated hydrogen flux was increased with increasing the temperature and the difference of hydrogen pressure between the feed side and permeates side of the membrane. The Ni-based amorphous alloys were characterized by X-ray diffractometry(XRD) and differential scanning calorimetry(DSC). The morphology of surface and roughness was observed by using scanning electron microscopy(SEM) and atomic force microscopy(AFM).