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

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Release Behaviors of Poly(ε-caprolactone)/Poly(ethyleneimine) Microcapsules Containing Fragrant Oil (향오일을 함유한 Poly(ε-caprolactone)/Poly(ethyleneimine) 마이크로캡슐의 방출거동)

  • Park, Soo-Jin;Seok, Su-Ja
    • Korean Chemical Engineering Research
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    • v.43 no.4
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    • pp.482-486
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    • 2005
  • The biodegradable poly(${\varepsilon}$-caprolactone)(PCL)/poly(ethylene imine)(PEI) microcapsules containing $Al_2O_3$ and fragrant oil were prepared with different PEI contents. The effects of stirring rate and concentration of the surfactant on the diameter and morphologies of microcapsules were investigated by using scanning electron microscope (SEM). Thermal behaviors were studied by using a differential scanning calorimetry(DSC), and the release behaviors of fragrant oil from microcapsule were characterized by UV/vis. spectrophotometer. As a result, the average particle size of the microcapsules decreased with increasing the stirring rate or concentration of the surfactant. The surface morphologies of the microcapsules were changed from smooth surfaces to skin-like rough surfaces as increasing the PEI content. These results were mainly due to the increased hydrophilic groups at the microcapsule surfaces, resulting in increasing the release rate of fragrant oil in the microcapsules studied.

Synthesis, chemically and electrochemically polymerization of N-substituted pyrrole containing azo chromophore and its copolymerization with pyrrole

  • Hosseini, Seyed Hossein
    • Advances in materials Research
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    • v.1 no.4
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    • pp.299-310
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    • 2012
  • This article describes the synthesis of a novel N-substituted pyrrole monomer containing an azobenzene group. The 2-[N-ethyl-N-[4-[(4-nitrophenyl) azo]-phenyl] amino] ethyl-3-chloropropionate (RedII) compound was synthesized via reaction of 4-nitro-4'-[N-ethyl-N-(2-hydroxyethyl)-amino] azobenzene (RedI) and 3-chloropropionic acid. RedII was reacted with the potassium salt of pyrrole then 2-[N-ethyl-N-[4-[(nitro phenyl) azo] phenyl] amino] ethyl-N-pyrrolyl propionate (Py-RedII) was prepared. Chemical polymerization of Py-RedII and copolymerization of Py-RedII with pyrrole carried out using $FeCl_3$. Poly (2-[N-ethyl-N-[4-[(nitro phenyl) azo] phenyl] amino] ethyl-N-pyrrolyl propionate) (PPy-RedII) was characterized by UV, IR, $^1HNMR$, $^{13}CNMR$ spectroscopies. Electropolymerization of Py-RedII and electroco-polymerization of Py-RedII and pyrrole were studied using conventional three electrodes system, Ag/AgCl reference electrode, platinum counter electrode and GC disk working electrode. Scanning electron microscopy (SEM), thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC) were used for thermal and rheological studies. The TGA curve of PPy-RedII demonstrated a high thermal stability up to 200°C and its DSC thermogram showed two endothermic peaks at 88 and $122^{\circ}C$. The glass transition temperature of the polymer was found to be above the room temperature. Electrical conductivities of PPy-RedII and it's copolymer with pyrrole (PPy-RedII-co-Py) were studied by the four-probe method and produced conductivities of $7.5{\times}10^{-4}$ and $6.5{\times}10^{-3}Scm^{-1}$, respectively.

Reactive blends of poly(butylene terephthalate)/polyamide-6 with ethylene glycidyl methacrylate

  • Han, M.S.;Lim, B.H.;Jung, H. C.;Hyun, J.C.;Kim, S.R.;Kim, W.N.
    • Korea-Australia Rheology Journal
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    • v.13 no.4
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    • pp.169-177
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    • 2001
  • Morphological, thermal, rheological, and mechanical properties of reactive compatabilized blends of poly(butylene terephthalate) (PBT) and Polyamide-6 (PA) containing EGMA copolymer were investigated using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), advanced rheometric expansion system (ARES), and universal testing machine (UTM). From the results of thermal analysis by DSC, the melting point of the 30/70 PBT-PA blend was broadened after EGMA was added in the blends, since the enthalpy of melting of the PBT-PA somewhat decreased with the increase of EGMA content. From this result, it is suggested that the EGMA affected to the crystallization behavior and crystallinity of the PBT-PA blends. From SEM micrographs of the 70/30, 50/50, and 30/70 PBT-PA blends, the droplet size of the 30/70 PBT-PA blend was about 0.8 ${\mu}{\textrm}{m}$ which was smaller than that of the 50/50 and 70/30 PBT-PA blends. The complex viscosity of the 30/70 PBT-PA blend observed to be higher than that of the 50/50 and 70/30 PBT-PA blends. From the results of the morphology and rheological properties for the PBT-PA blends, it is suggested that the compatibility is increased in the 30/70 PBT-PA blend than the 50/50 and 70/30 PBT-PA blends. From the results of mechanical properties, it was found that the tensile strength of the 30/70 PBT-PA blend increased with the increase of EGMA up to 2 phr, while tensile strength of the blend in which EGMA content was higher than 2 phr decreased with the increase of EGMA content. From the results of morphological, thermal, rheological, and mechanical properties for the PBT-PA-EGMA blends, it is suggested that the EGMA could be used as a compatibilization role in the blends.

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Organic-Inorganic Nanocomposites of Polystyrene with Polyhedral Oligomeric Silsesquioxane (실세스키옥세인을 사용한 폴리스티렌 나노복합재료)

  • Kim Kyung-Min
    • Polymer(Korea)
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    • v.30 no.5
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    • pp.380-384
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    • 2006
  • Polyhedral oligomeric silsesquioxanes (POSS) were used as starting materials for the preparation of hybrid materials with polystyrene (PS). Optically transparent hybrids were obtained in a wide range of weight ratios when phenyl groups were introduced to each corner of the silsesquioxane. In contrast, as cyclohexyl groups were introduced, the obtained hybrid materials with PS resulted in turbid films. The aromatic (${\pi}-{\pi}$) interaction was confirmed to be a quite effective tool for the synthesis of organic-Inorganic polymer hybrids with POSS. The obtained homogeneous and transparent hybrid films could be dissolved in solvents and East again without any separation. The homogeneity of polymer hybrids with POSS was supported by the result of scanning electron microscopy (SEM), X-ray diffraction (XRD), and differential scanning calorimetry (DSC), which demonstrated a nanometer-level integration of PS and POSS.

Characterizations of Flexible Clay-PVA Hybrid Films: Thermo-optical Properties, Morphology, and Gas Permeability (유연한 점토-폴리(비닐 알코올) 하이브리드 필름의 특성 연구: 열적.광학적 성질, 모폴로지, 및 가스 투과성)

  • Shin, Ji-Eun;Ham, Mi-Ran;Kim, Jeong-Cheol;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.35 no.5
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    • pp.402-408
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    • 2011
  • To improve $Na^+$-saponite(SPT) film flexibility, we prepared SPT hybrid clay films with various poly(vinyl alcohol) (PVA) concentrations(0~10 wt%) using the solution intercalation method. In this study, we investigated the thermo-optical properties, morphology, and gas permeability of the SPT hybrid films. We also examined the relationship between the film properties and PVA content using wide angle X-ray diffraction measurements(XRD), field emission scanning electron microscopy(FESEM), differential scanning calorimetry(DSC), thermogravimetric analysis(TGA), thermomechanical analysis(TMA), ultraviolet-visible(UV-vis) spectroscopy, and oxygen transmission rate($O_2$TR) testing. The properties of the clay hybrid films were strongly affected by PVA filler content. The presence of a small amount of PVA was sufficient to improve the flexibility of SPT hybrid films.

Molecular Effect of PVP on The Release Property of Carvedilol Solid Dispersion

  • Oh, Myeong-Jun;Shim, Jung-Bo;Lee, Eun-Yong;Yoo, Han-Na;Cho, Won-Hyung;Lim, Dong-Kyun;Lee, Dong-Won;Khang, Gil-Son
    • Journal of Pharmaceutical Investigation
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    • v.41 no.3
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    • pp.179-184
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    • 2011
  • This study aimed to confirm the effect of molecular weight (MW) in solid dispersion of carvedilol with poly-vinylpyrrolidone (PVP) of various MW. Solid dispersion of carvedilol with PVP was prepared by spray-drying method. Scanning electron microscopy (SEM) was used to analyze the surface of solid dispersion samples. Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) were used to analyze the crystalline of solid dispersion. Fourier transform infrared spectroscopy (FT-IR) was used to analyze the change of chemical structure characteristic of solid dispersion. DSC and XRD show that drug crystalline was changed. FT-IR revealed that chemical structure of solid dispersion comparing the chemical structure of drug was changed. The dissolution studies of solid dispersion presented at simulated gastric juice (pH 1.2). The dissolution rate of solid dispersion was dramatically enhanced than pure drug and the MW of PVP has an effect on the release property of carvedilol in solid dispersion. In conclusion, the present study has confirmed the effect of MW of PVP on release property of solid dispersion formulation of carvedilol with PVP.

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.

Study on the Oil Seal Application Using Polytetrafluoroethylene Composites (Polytetrafluoroethylene 복합재료를 이용한 오일씰 응용에 관한 연구)

  • Ha, Ki-Ryong;Lee, Jong-Cheol;Lee, Young-Seok
    • Elastomers and Composites
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    • v.45 no.1
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    • pp.32-39
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    • 2010
  • The mechanical properties of PTFE 100%, PTFT 90% + carbon black 10%, PTFE 85% + glass fiber 15%, PTFE 80% + glass fiber 15% + molybdenum disulfide ($MoS_2$) 5%, PTFE 75% + glass fiber 25%, and PTFE 75% + carbon black 18% + graphite 7% composites were investigated in this study. The differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were used to examine the heat of fusion(${\Delta}H_f$) and thermal stability of the composites. Also, the wear surface and wear volume of PTFE lip seal were examined using the durability test. Wear surface was observed using scanning electron microscope (SEM). It was found that the hardness, wear resistance and durability were enhanced by adding glass fiber and molybdenum disulfide into pure PTFE, but tensile strength and elongation were decreased. According to the experimental results, the composite (PTFE + 15% glass fiber + 5% molybdenum disulfide) showed the best properties for applying to oil-seal among six types of PTFE composites.

Improvement of Toughness of Tetrafunctional Epoxy (TGDDM) Resin Using Polyamideimide (PAI) Resin (폴리아미드이미드 수지를 이용한 4관능성 에폭시 수지의 강인화 향상)

  • 박수진;허건영;이재락;홍영택;최길영
    • Polymer(Korea)
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    • v.26 no.5
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    • pp.599-606
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    • 2002
  • In this study, 4,4'-tetraglycidyl diaminodiphenyl methane (TGDDM)/polyamideimide (PAI) blends were cured using diaminodiphenyl sulfone (DDS). And the effect of addition of different PAI contents to neat TGDDM was investigated in the thermal, mechanical, and morphological properties of the blends. The cure behavior and thermal stability of the cured specimens were monitored by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), respectively. Also, the critical stress intensity factor (K$\_$IC/) was measured in UTM, and the phase separation behavior and final morphology of TGDDM/PAI blends were examined in scanning electron microscopy(SEM). As a result, the cure temperature and cure activation energy (E$\_$a/) were decreased with increasing the PAI content. The decreasing of cure temperature and cure activation energy were probably due to the presence of secondary amine group of PAI backbone used as co-initiator. But, the decomposition activation energy (E$\_$t/) and K$\_$IC/ value were increased up to 5. 10 phr of PAI content, respectively and they were decreased above the PAI contents. These results were explained on the basis of chain scission reaction by etherification. And morphology of blends observed from SEM was confirmed in co-continuous structures.

Synthesis and Physical Properties of Sm Doped Pb Free 3 Phase-Glasses (Sm 농도에 따른 무연 3상 유리계의 합성과 물리적 성질)

  • Park, Jong-Ho
    • Korean Journal of Materials Research
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    • v.22 no.7
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    • pp.368-373
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    • 2012
  • Glasses were prepared with compositions of $(13-x)BaO-80B2_O_3-7Li_2O{\cdot}xSm_2O_3$, BBLSx(x=0.5, 0.4, 0.3) by melting the starting materials of boron oxide(99.9%), lithium oxide(99.9%), barium carbon oxide(99.9%), and samarium oxide(99.9%) and then quenching the melt at $1350^{\circ}C$. This led to good-quality BBLSx(x=0.4, 0.3) and poor-quality BBLSx(x=0.5) glasses. The physical and structural properties of the BBLSx glasses were studied by means x-ray diffraction, scanning electron microscopy(SEM), differential scanning calorimetry(DSC), and dielectric spectroscopy. From the x-ray diffraction and SEM results, the quality of the BBLSx glasses significantly depends on the $Sm_2O_3$ concentration. The x-ray diffraction pattern showed that the crystallites in the BBLSx glasses after heat treatment at $700^{\circ}C$ may be $LiBaB_9O_{15}$. From the DSC results, the glass transition temperatures($T_g$), crystallization temperatures($T_c$), and the maximum temperatures of the crystallized($T_p$) BBLSx glasses all changed with the $Sm_2O_3$ concentration. According to the dielectric spectroscopy results, the values of the real dielectric constant and Tan ${\delta}$ of the BBLSx glasses depended on the $Sm_2O_3$ concentration. The values of the real dielectric constant and Tan ${\delta}$ were also shown to depend on the measuring temperature, possibly due to the ion migration in the bulk of the BBLSx glasses.