• Title/Summary/Keyword: dynamic differential scanning calorimetry

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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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Study on the rheological properties of PP-SEBS/silicate composites (PP-SEBS/실리케이트 복합체의 유변학적 특성 연구)

  • Kim, Youn-Cheol
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.12 no.4
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    • pp.1988-1992
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    • 2011
  • Polypropylene (PP)-SEBS/silicate composites with PP content of 35, 40, and 45wt% were fabricated by melt compounding at $200^{\circ}C$, using lab scale Brabender mixer. The content of silicate was fixed at 5wt%. The thermal properties of the PP-SEBS/silicate composites were investigated by differential scanning calorimetry (DSC) and thermogravimetric analyzer (TGA). The melting temperature of PP-SEBS compound decreased up to $141^{\circ}C$ with SEBS content. TGA result indicates an increase in degradation temperature when the silicate was added in the PP-SEBS compound. The rheological properties of the compounds were measured by dynamic Rheometer. PP-SEBS/silicate composite indicates higher shear thinning and elastic property than PP-SEBS compound. Van Gurp-Palmen analysis was applied in order to certify an increase in elasticity.

Synthesis and Characterization of Ruthenium Doped TiO2 Nanofibers

  • Park, Jung-Yeon;Lee, Deuk-Yong;Cho, Nam-Ihn;Oh, Young-Jei
    • Journal of Sensor Science and Technology
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    • v.20 no.2
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    • pp.82-89
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    • 2011
  • Ruthenium(Ru)-doped $TiO_2$ nanofibers were prepared using electrospun Ru-$TiO_2$/poly(vinyl acetate) (PVAc) fibers and subsequent annealing for 1 h at temperatures in the range of $500^{\circ}C$ to $1000^{\circ}C$ in air. The properties of the Ru-$TiO_2$ fibers were characterized as a function of the Ru content and calcination temperature using X-ray diffraction, thermal gravimetry with differential scanning calorimetry, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and viscometer, pycnometer and dynamic tensiometer measurements. Although the diameter of the fiber decreased slightly with increasing calcination temperature, no dramatic changes were observed with respect to the ruthenium content. The XRD and FT-IR results revealed that anatase phase and ruthenium metal began to be formed after calcination at temperatures above $500^{\circ}C$. Anatase and rutile phases and ruthenium metal coexisted in the fibers calcined above $600^{\circ}C$. No anatase phase was detected in the fibers containing ruthenium when they were calcined at $1000^{\circ}C$. The morphology of the fibers changed from smooth and uniform to porous with increasing temperature. The experimental results suggest that the calcination temperature and Ru content were influential in determining the morphology and structure of the fibers.

Preparation and Comparison the Physical Properties of Polyurethane-Urea Using Biomass Derived Isosorbide (바이오매스 유래 이소소르비드를 이용한 폴리우레탄-우레아의 제조 및 특성 비교)

  • Park, Ji-Hyeon;Park, Jong-Seung;Choi, Pil-Jun;Ko, Jae-Wang;Lee, Jae-Yeon;Sur, Suk-Hun
    • Textile Coloration and Finishing
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    • v.31 no.3
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    • pp.165-176
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    • 2019
  • Polyurethane-ureas(PUUs) were prepared from 4,4'-methylenebis(cyclohexyl isocyanate) and various diols including isosorbide. Isosorbide is starch-derived monomer that exhibit a wide range of glass transition temperature and are therefore able to be used in many applications. PUU was synthesized by a pre-polymer polymerization using a catalyst. Successful synthesis of the PUU was characterized by fourier transform-infrared spectroscopy. Thermal properties were determined by differential scanning calorimetry, thermogravimetric analysis, and dynamic mechanical analysis. It was found that by tuning isosorbide content in the resin, their glass transition temperature(Tg) slightly decreased. Physical properties were also determined by tensile strength and X-ray diffraction. There is no significant differences between petroleum-derived diol and isosorbide in XRD analysis. Moreover, their physical and optical properties were determined. The result showed that the poly(tetramethylene ether glycol)/isosorbide-based PUU exhibited enhanced tensile strength, transmittance, transparency and biodegradability compared to the existing diols. After 11 weeks composting, the biodegradability of blends increased in ISB-PUU. The morphology of the fractured surface of blend films were investigated by scanning electron microscopy.

Effect of Salt Concentration on the Glass Transition Temperature and Ionic Conductivity of Poly(ethylene glycol)-Polyurethane/$LiClO_4$ Complexes

  • Huh, Pil-Ho;Park, Myung-Geun;Jo, Nam-Ju;Lee, Jin-Kook;Lee, Jang-Oo;Wongkang Yang
    • Macromolecular Research
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    • v.12 no.4
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    • pp.422-426
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    • 2004
  • Solid polymer electrolytes based on poly(ethylene glycol)-polyurethane (PEG-PU) complexed with LiClO$_4$ salt have been prepared by the solvent casting method. A PEG-PU material (PEG:4,4'-diphenylmethane diisocyanate: l,4-butanediol = 1:2:1) was synthesized through a typical two-step condensation reaction. We investigated the effects of the salt concentration on the ionic conductivity ($\sigma$) and the glass transition temperature (T$_{g}$ ) of the complex electrolytes by using alternating current impedance spectroscopy, differential scanning calorimetry, and dynamic mechanical thermal analysis. The measured values of both $\sigma$ and T$_{g}$ exhibited similar tendencies in that they had maxima within the range studied, probably because of two opposite effects, i.e., the increased number of carrier ions and the decreased chain mobility (or increased T$_{g}$ ) caused by the increase in the salt concentration. The highest conductivity, on the order of 2.43 ${\times}$ 10$^{6}$ S$cm^{-1}$ /, was obtained at an [O]/[Li$^{+}$] ratio of ca. 16 (0.92 ㏖ salt per kg of matrix polymer).

Study on Cure Behavior of Low Temperature and Fast Cure Epoxy with Mercaptan Hardener (Mercaptan 경화제에 의한 저온속경화 에폭시의 경화거동에 관한 연구)

  • Eom, Se Yeon;Seo, Sang Bum;Lee, Kee Yoon
    • Polymer(Korea)
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    • v.37 no.2
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    • pp.240-248
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    • 2013
  • The curing behaviors of diglycidyl ether of bisphenol A (DGEBA) with mercaptan hardener were studied by the comparison with amine-adduct type hardener. Curing behaviors were evaluated by DSC at dynamic and isothermal conditions. In the DSC, the dynamic experiments were based on the method of Kissinger's equation, and the isothermal experiments were fitted to the Kamal's kinetic model. Activation energy of epoxy/amine-adduct type hardener was ca. 40 kcal/mol. As the functional group of mercaptan hardener, -SH increased, on epoxy/mercaptan hardeners, the activation energies decreased from 28 to 19 kcal/mol. Epoxy/amine-adduct type hardener was initiated at $90^{\circ}C$ or higher. However, epoxy/mercaptan hardeners reduced the initiation temperatures below $80^{\circ}C$ and shortened the durations of curing reaction within 10 min. We found out that the reaction kinetics of epoxy with mercaptan hardener followed the autocatalytic reaction models, and the maximum reaction rates were shown at the conversions of 20~40%.

Fabrication and Characterization of Zirconia-Alumina Composites by Organic-Inorganic Solution Technique (유기물-무기물 용액법을 이용한 지르코니아-알루미나 복합체의 제조 및 특성)

  • Kim, Youn Cheol;Bang, Moon-Soo;Lee, Sang Jin
    • Applied Chemistry for Engineering
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    • v.16 no.5
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    • pp.628-634
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    • 2005
  • Zirconia-alumina polymer precursor was prepared from zirconium acetylacetonate (ZA). paluminium nitrate (AN), polyethylene glycol (PEG), and ethyl alcohol via an organic-inorganic solution technique. The thermal properties and viscosity of the polymer precursor were measured by differential scanning calorimetry (DSC), thermograbimetric analyzer (TGA), and dynamic viscometer. The vigorous exothermic reaction with volume expansion occurred at $140^{\circ}C$. The volume expansion was caused by abrupt decomposition of the organic group in metal compounds and the metal ions-PEG reaction. The evidences for these reactions were confirmed by FT-IR and $^{13}C$ solid NMR results. The peak intensity at N-O, O-H and C=C decreased with increasing temperature. This indicated that the decomposition of metal compounds and the metal ions-PEG reaction occurred during the vigorous exothermic reaction. At $800^{\circ}C$ for 2 h, the porous powders transformed to the crystalline $ZrO_2-Al_2O_3$ composites.

Rheological properties and crystallization kinetics of polypropylene block copolymer with repeated extrusion

  • Sung Yu-taek;Seo Won Jin;Kim Jong Sung;Kim Woo Nyon;Kwak Dong-Hwan;Hwang Tae-Won
    • Korea-Australia Rheology Journal
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    • v.17 no.1
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    • pp.21-25
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    • 2005
  • Rheological properties and crystallization kinetics of the polypropylene (PP) block copolymer and recycled PP block copolymer were studied by advanced rheometric expansion system (ARES), differential scanning calorimetry (DSC), and optical microscopy. In the study of the dynamic rheology, it is observed that the storage modulus and loss modulus for the PP block copolymer and recycled PP block copolymer did not change with frequency. In the study of the effect of the repeated extrusion on the crystallization rate, half crystallization time of the PP samples was increased with the number of repeated extrusion in isothermal crystallization temperature ($T_c$). From the isothermal crystallization kinetics study, the crystallization rate was decreased with the increase of the number of repeated extrusion. Also, from the result of Avrami plot, the overall crystallization rate constant (K) was decreased with the increase of the number of the repeated extrusion. From the study of the optical microscopy, the size of the spherulite of the PP samples did not change significantly with the number of repeated extrusion. However, it was clearly observed that the number of the spherulite growth sites was decreased with the number of repeated extrusion. From the results of the crystallization rate, isothermal crystallization kinetics, Avrami plots, and optical microscopy, it is suggested that the crystallization rate of the PP block copolymer is decreased with the increase of the number of repeated extrusion.

Effects of Hardeners on the Low-Temperature Snap Cure Behaviors of Epoxy Adhesives for Flip Chip Bonding (플립칩용 에폭시 접착제의 저온 속경화 거동에 미치는 경화제의 영향)

  • Choi, Won-Jung;Yoo, Se-Hoon;Lee, Hyo-Soo;Kim, Mok-Soon;Kim, Jun-Ki
    • Korean Journal of Materials Research
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    • v.22 no.9
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    • pp.454-458
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    • 2012
  • Various adhesive materials are used in flip chip packaging for electrical interconnection and structural reinforcement. In cases of COF(chip on film) packages, low temperature bonding adhesive is currently needed for the utilization of low thermal resistance substrate films, such as PEN(polyethylene naphthalate) and PET(polyethylene terephthalate). In this study, the effects of anhydride and dihydrazide hardeners on the low-temperature snap cure behavior of epoxy based non-conductive pastes(NCPs) were investigated to reduce flip chip bonding temperature. Dynamic DSC(differential scanning calorimetry) and isothermal DEA(dielectric analysis) results showed that the curing rate of MHHPA(hexahydro-4-methylphthalic anhydride) at $160^{\circ}C$ was faster than that of ADH(adipic dihydrazide) when considering the onset and peak curing temperatures. In a die shear test performed after flip chip bonding, however, ADH-containing formulations indicated faster trends in reaching saturated bond strength values due to the post curing effect. More enhanced HAST(highly accelerated stress test) reliability could be achieved in an assembly having a higher initial bond strength and, thus, MHHPA is considered to be a more effective hardener than ADH for low temperature snap cure NCPs.

Synthesis and Application of Reactive Polymer Modifiers for Asphalt: 2. Application (아스팔트용 반응성 고분자 개질제 합성 및 적용: 2. 적용)

  • Hwang, Ki-Seob;Lee, Jong-Cheol;Jang, Suck-Soo;Lee, Seung-Han;Ha, Ki-Ryong
    • Polymer(Korea)
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    • v.31 no.6
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    • pp.538-542
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    • 2007
  • This study is on the performance analysis of modified asphalts which were prepared by mixing the asphalt with polymer modifiers of varying compositions which were synthesized by the emulsion polymerization method. Thermal properties of mired asphalt were investigated by DSC (differential scanning calorimetry), and dispersion of modifiers in asphalt was investigated by the fluorescence microscope. Dynamic stability and permanent deformation velocities of mixed asphalt were investigated by wheel tracking measurements. Modifier 6 showed the best results in both penetration test and wheel tracking measurement among investigated modifiers, which supports MMA(methyl methacrylate) moiety in modifiers plays better contribution for the enhancement of asphalt performance than styrene moiety does.