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

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Microphase Separation and Crystallization in Binary Blends Consisting of Poly (methyl methacrylate)-block-Polystyrene Copolymer and Poly (vinylidene fluoride) (폴리(메틸 메타크릴레이트)-폴리스티렌 이종 블록 공중합체/폴리(비닐리덴 플루오라이드) 블렌드의 미세 상분리와 결정화)

  • 김지선;이광희;조성무;류두열;김진곤
    • Polymer(Korea)
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    • v.28 no.6
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    • pp.509-518
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    • 2004
  • Microdomain structures and crystallization behavior of the binary blends consisting of an asymmetric block copolymer and a homopolymer were investigated using small-angle X-ray scattering (SAXS), optical micro scope (OM) and differential scanning calorimetry (DSC). Poly(methyl methacrylate)-block-polystyrene block copolymer (PMMA-b-PS) (weight fraction of PMMA =0.53) was mixed with low molecular weight poly(vinylidene fluoride) (PVDF). As the PVDF concentration was increased, the morphological change from a lamellar to a cylindrical structure occurred. The crystallization of PVDF significantly disturbed the orientation of the pre-existing microdomain structure, resulting in a poorly ordered morphology. In the blends, PVDF exhibited unique crystallization behavior due to the PMMA block which is preferentially miscible to PVDF and the space constraint imposed by the microdomains.

Extensional and Complex Viscosities of Linear and Branched Polycarbonate Blends

  • Park, Jung-Hoon;Hyun, Jae-Chun;Kim, Woo-Nyon;Kim, Sung-Ryong;Ryu, Seung-Chan
    • Macromolecular Research
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    • v.10 no.3
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    • pp.135-139
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    • 2002
  • Blends of the linear bisphenol-A polycarbonate (L-PC) and randomly branched bisphenol-A polycarbonate (Br-PC), prepared by co-rotating twin screw extrusion, were investigated using differential scanning calorimetry (DSC), sag resistance time tester, extensional rheometry, and advanced rheometric expansion system (ARES). From the DSC results, the glass transition temperature (T$_{g}$) of the L-PC/Br-PC blend was increased with the increase of Br-PC in the blend, and the blend showed a single T$_{g}$, which suggests a miscible blend. The sag resistance time of the L-PC/Br-PC blend was increased with the increase of Br-PC in the blends. From the results of rheological measurements of the L-PC/Br-PC blends, the extensional viscosity and the complex viscosity of the blends were found to increase with the increase of Br-PC in the blends. The increase of extensional viscosity and complex viscosity was related with the increase of sag resistance time with the Br-PC in the L-PC/Br-PC blends.nds.

Crystal Form of Celecoxib: Preparation, Characterization and Dissolution

  • Jin, Mi-Ryung;Sohn, Young-Taek
    • Journal of the Korean Chemical Society
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    • v.62 no.5
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    • pp.352-357
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    • 2018
  • Celecoxib (4-[5-(4-methylphenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide) is a cyclooxygenase-2 inhibitor used in the treatment of arthritis, acute pain, and dysmenorrhoea. Celecoxib is a Biopharmaceutics Classification System (BCS) class II compound whose oral bioavailability is highly limited owing to its poor aqueous solubility. Several polymorphs of celecoxib have been identified as Form I, Form II, and Form III with melting points of about $162.8^{\circ}C$, $161.5^{\circ}C$, and $160.8^{\circ}C$, respectively. Form IV was generated from the precipitated suspension in the presence of HPMC (Hydroxypropyl methylcellulose) and Polysorbate 80. A rapid rate of dissolution is useful because the rate of dissolution of a drug typically increases its bioavailability. The aim of this study was to investigate the possibility of production of new crystal form of celecoxib that has higher solubility than Form III. New crystal form of celecoxib (Form A) has been isolated by recrystallization and characterized by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis and powder X-ray diffractometry (PXRD). Form A was dissolved faster than Form III. At 30 minutes, the dissolution of Form A was 97.3%, whereas the dissolution of Form III was 82.2% (p < 0.1). After storage of three months at $20^{\circ}C$, in 24% RH (Relative Humidity), the crystal form was not transformed.

Study on The Thermal Properties of Poly(methyl methacrylate) and Poly($\alpha$-methylstyrene-co-acrylonitrile) Mix tures (Poly(methyl methacrylate)와 Poly($\alpha$-methylstyrene-co-acrylonitrile) 혼합물의 열적특성에 관한 연구)

  • Moon, Deog-Ju;Kim, Byung-Chul;Kim, Dong-Keun;Seul, Soo-Duk;Sohn, Jin-Eon
    • Elastomers and Composites
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    • v.23 no.4
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    • pp.289-298
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    • 1988
  • The thermal degradation of poly(methyl methacrylate)(PMMA) and poly($\alpha$-methylstyrene-co-acrylonitrile)(SAN) mixtures were carried out using the thermogravimetry(TG) and differential scanning calorimetry(DSC) in the stream of nitrogen and air with 50 ml/min at the various heating rate from 4 to $20^{\circ}C/min$ and temperature from 20 to $500^{\circ}C$. The value of activation energies of thermal degradation determined by TG and DSC in the various PMMA/SAN mixtures were 34-54 kcal/mol in the stream of nitrogen. The value of activation energy of SAN 60% mixture were appeared high in comparison with addition rule. PMMA/SAN mixtures by the analysis of infrared spectrophotometer were decomposed by main chain scission in the stream of nitrogen.

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Kinetic Study on the Thermal Degradation of Poly(Methyl Methacrylate) and Poly(Acrylonitrile Butadiene Styrene) Mixtures (Poly(methyl methacrylate)와 Poly(acrylonitrile butadiene styrene)와의 혼합에 의한 열분해속도에 관한 연구)

  • Moon, Deok-Ju;Kim, Dong-Keun;Seul, Soo-Duk
    • Elastomers and Composites
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    • v.24 no.1
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    • pp.11-18
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    • 1989
  • The thermal degradation of Poly(methyl methacrylate) (PMMA) and poly(acrylonitrile butadiene styrene)(ABS) terpolymer as well as their mixtures were carried out using the thermogravimetry and differential scanning calorimetry(DSC) in the stream of nitrogen and air with 50 ml/min at the various heating rate from 4 to $20^{\circ}C/min$ and temperature from 200 to $300^{\circ}C$ The values of activation energies of thermal degradation determined by TG and DSC in the various PMMA/ABS mixtures were $34{\sim}58Kcal/mol,\;35{\sim}54Kcal/mol$ in the stream of nitrogen. The values of activation energy of ABS20% mixture was appeared high in camparison with addition rule. According to increasing the composition of ABS, the temperatures of glass transition and initial decomposition temperature were increased. PMMA/ABS mixtures by the analysis of infrared spectrophotometer were decomposed by main chain scission in the stream of nitrogen.

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Lithium Ion Concentration Dependant Ionic Conductivity and Thermal Properties in Solid Poly(PEGMA-co-acrylonitrile) Electrolytes

  • Kim, Kyung-Chan;Roh, Sae-Weon;Ryu, Sang-Woog
    • Journal of Electrochemical Science and Technology
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    • v.1 no.1
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    • pp.57-62
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    • 2010
  • The lithium ion concentration dependant ionic conductivity and thermal properties of poly(ethylene glycol) methyl ether methacrylate (PEGMA)/acrylonitrile-based copolymer electrolytes with $LiClO_4$ have been studied by differential scanning calorimetry (DSC), linear sweep voltammetry (LSV) and AC complex impedance measurements. In systems with 11 wt% of acrylonitrile all liquid electrolytes were obtained regardless of lithium ion concentration. Complex impedance measurements with stainless steel electrodes give ambient ionic conductivities $8.1\times10^{-6}\sim1.4\times10^{-4}S cm^{-1}$. On the other hand, a hard and soft films at ambient temperature were obtained in copolymer electrolyte system consists of 15 wt% acrylonitrile with 6 : 1 and 3 : 1 of [EO] : [Li] ratio, respectively. DSC measurements indicate the crystalline melting temperature of poly(PEGMA) disappeared completely after addition of $LiClO_4$ in this system due to the complex formation between ethylene oxide (EO) unit and lithium salt. As a result, free standing film with room temperature ionic conductivity of $1.7\times10^{-4}S cm^{-1}$ and high electrochemical stability up to 5.5V was obtained by controlling of acrylonitrile and lithium salt concentration.

Evaluations of Sb20Se80-xGex (x = 10, 15, 20, and 25) Glass Stability from Thermal, Structural and Optical Properties for IR Lens Application

  • Jung, Gun-Hong;Kong, Heon;Yeo, Jong-Bin;Lee, Hyun-Yong
    • Journal of the Korean Ceramic Society
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    • v.54 no.6
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    • pp.484-491
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    • 2017
  • Chalcogenide glasses have been investigated in their thermodynamic, structural, and optical properties for application in various opto-electronic devices. In this study, the $Sb_{20}Se_{80-x}Ge_x$ with x = 10, 15, 20, and 25 were selected to investigate the glass stability according to germanium ratios. The thermal, structural, and optical properties of these glasses were measured by differential scanning calorimetry (DSC), X-ray diffraction (XRD), and UV-Vis-IR Spectrophotometry, respectively. The DSC results revealed that $Ge_{20}Sb_{20}Se_{60}$ composition showing the best glass stability theoretically results due to a lower glass transition activation energy of 230 kJ/mol and higher crystallization activation energy of 260 kJ/mol. The structural and optical analyses of annealed thin films were carried out. The XRD analysis reveals obvious results associated with glass stabilities. The values of slope U, derived from optical analysis, offered information on the atomic and electronic configuration in Urbach tails, associated with the glass stability.

Characterization of Microcapsules for Self-Healing in Polymeric Composites

  • Lee Jong Keun;Hong Soon Ji;Liu Xing;Park Hee Won;Yoon Sung Ho
    • Proceedings of the Korean Society For Composite Materials Conference
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    • 2004.04a
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    • pp.190-193
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    • 2004
  • Two different diene monomers [dicyclopentadiene (DCPD) and 5-ethylidene-2-norbomene (ENB)] as self­healing agent for polymeric composites were microencapsuled by in-situ polymerization of urea and formaldehyde. The healing agents were investigated by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). Exothermic reaction and glass transition temperature from DSC and storage modulus (G') and tan $\delta$ from DMA curves were analyzed for the samples cured for 5 min and 24 h in the presence of different amounts of catalyst. Micorcapsules were successfully formed for both diene monomers. Microcapsules containing the healing agent were manufactured and its thermal properties were characterized by thermo gravimetric analysis (TGA). Optical microscope (OM) and particle size analyzer (PSA) were employed to observe morphology and size distribution of microcapsules, respectively. Comparison of the two self-healing agents and their microcapsules with the two was made in this study.

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Synthesis and Characterization of Tetrazine Derivatives as High Energy Propellants (테트라진 계열의 추진 물질 합성 연구)

  • Lee, Woonghee;Park, Youngchul;Joo, Young-Hyuk
    • Journal of the Korean Society of Propulsion Engineers
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    • v.17 no.6
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    • pp.38-47
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    • 2013
  • Traditional propellants release toxic gases during combustion that are harmful to the environment. This study describes a novel synthetic process of two high nitrogen containing tetrazines, TATTz and BTATz, which can be adapted as solid fuels for a solution to environmental concerns. The compounds were characterized by NMR, IR spectroscopy, and differential scanning calorimetry(DSC). Detonation properties were calculated with the EXPLO5 program based on calculated heats of formation and measured densities.

Effect of Polyhedral Oligomeric Silsesquioxane on Cure Characterization of an Epoxy/Amine System (에폭시/아민계의 경화 특성에 미치는 Polyhedral Oligomeric Silsesquioxane의 영향)

  • Gu, Puzhong;Lee, Jong Keun
    • Polymer(Korea)
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    • v.37 no.1
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    • pp.41-46
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    • 2013
  • The glass transition temperature ($T_g$) and conversion (${\alpha}$) were measured for a diglycidyl ether of bisphenol A (DGEBA) epoxy/aromatic amine system incorporated with an organic-inorganic hybrid molecule, polyhedral oligomeric silsesquioxane (POSS). Samples isothermally cured at varying cure temperatures and times were analyzed by differential scanning calorimetry (DSC). $T_g$ vs. ln (time) data at an arbitrary reference were superposed by time-temperature shifts for the kinetically controlled reaction, and the shift factors were used to calculate an Arrhenius activation energy. Influence of POSS was investigated from $T_g$ vs. ${\alpha}$ data, which in turn were fitted with DiBenedetto equation.